Dark-field imaging based on post-processed electron backscatter diffraction patterns of bulk crystalline materials in a scanning electron microscope.

PubMed

Brodusch, Nicolas; Demers, Hendrix; Gauvin, Raynald

2015-01-01

Dark-field (DF) images were acquired in the scanning electron microscope with an offline procedure based on electron backscatter diffraction (EBSD) patterns (EBSPs). These EBSD-DF images were generated by selecting a particular reflection on the electron backscatter diffraction pattern and by reporting the intensity of one or several pixels around this point at each pixel of the EBSD-DF image. Unlike previous studies, the diffraction information of the sample is the basis of the final image contrast with a pixel scale resolution at the EBSP providing DF imaging in the scanning electron microscope. The offline facility of this technique permits the selection of any diffraction condition available in the diffraction pattern and displaying the corresponding image. The high number of diffraction-based images available allows a better monitoring of deformation structures compared to electron channeling contrast imaging (ECCI) which is generally limited to a few images of the same area. This technique was applied to steel and iron specimens and showed its high capability in describing more rigorously the deformation structures around micro-hardness indents. Due to the offline relation between the reference EBSP and the EBSD-DF images, this new technique will undoubtedly greatly improve our knowledge of deformation mechanism and help to improve our understanding of the ECCI contrast mechanisms. Copyright © 2014 Elsevier B.V. All rights reserved.

Tiny twists in time; exploring angular resolution of in situ EBSD orientation microstructures in solar system zircon

NASA Astrophysics Data System (ADS)

Moser, D. E.

2012-12-01

Kikuchi discovered electron diffraction in samples of calcite in the 1920's, and orientation of lattice planes by Electron Backscatter Diffraction (EBSD) is now routinely measured by automated camera systems at a spatial resolution of tens of nanometers using Field Emission Gun SEM. The current methodology is proving particularly powerful when measuring lattice orientation microstructure in U-Pb geochronology minerals such as zircon and baddeleyite that have experienced high temperature deformation or shock metamorphism. These are among the oldest preserved mineral phases in inner solar system materials, and we have been applying EBSD to rare samples of the Early Earth and grains from extraterrestrial environments such as the Moon and Mars. In these cases the EBSD orientation data are useful for identifying high diffusivity pathways that may have afforded isotopic and trace element disturbance, microstructural proxies for shock metamorphic pressures, as well as resolving glide plane systems in ductile zircon and shear twin mechanisms. Blanket estimates of angular resolution for automated EBSD misorientation measurements are often in the range of 0.5 degrees. In some cases strain giving rise to only a few degrees of lattice misorientation has facilitated 100% Pb-loss. In some cases, however, there is a spatial correlation between trace element or cathodoluminescence zoning in zircon and what appears to be low magnitudes misorientation close to the limits of resolution. Given the proven value of performing EBSD analysis on geochronology minerals, a more thorough exploration of the precision and accuracy of EBSD lattice misorientation measurements is warranted. In this talk the relative weighting of the factors that limit EBSD angular resolution will be investigated, focusing on U-Pb dating minerals such as zircon. These factors include; sample surface preparation, phase symmetry, pseudo-symmetry effects, degree of crystallinity, Kikuchi band contrast and indexing, solid solution effects on unit cell, dimension camera calibration and camera-sample distance, beam conditions and focussing, and general microscope operating conditions (e.g. high vacuum vs. variable pressure). An assessment of potential zircon EBSD reference materials and sample preparation protocols will be presented, along with case studies of zircon orientation microstructures from meteorites and terrestrial craters representative of different strain and thermal environments in the inner solar system.BSD lattice misorientation maps of a) crystal-plastically deformed and partly recrystallized zircon, after Rayner et al. (in prep.), and b) shock-metamorphosed lunar zircon (Darling et al., in prep.).

Identifying deformation mechanisms in the NEEM ice core using EBSD measurements

NASA Astrophysics Data System (ADS)

Kuiper, Ernst-Jan; Weikusat, Ilka; Drury, Martyn R.; Pennock, Gill M.; de Winter, Matthijs D. A.

2015-04-01

Deformation of ice in continental sized ice sheets determines the flow behavior of ice towards the sea. Basal dislocation glide is assumed to be the dominant deformation mechanism in the creep deformation of natural ice, but non-basal glide is active as well. Knowledge of what types of deformation mechanisms are active in polar ice is critical in predicting the response of ice sheets in future warmer climates and its contribution to sea level rise, because the activity of deformation mechanisms depends critically on deformation conditions (such as temperature) as well as on the material properties (such as grain size). One of the methods to study the deformation mechanisms in natural materials is Electron Backscattered Diffraction (EBSD). We obtained ca. 50 EBSD maps of five different depths from a Greenlandic ice core (NEEM). The step size varied between 8 and 25 micron depending on the size of the deformation features. The size of the maps varied from 2000 to 10000 grid point. Indexing rates were up to 95%, partially by saving and reanalyzing the EBSP patterns. With this method we can characterize subgrain boundaries and determine the lattice rotation configurations of each individual subgrain. Combining these observations with arrangement/geometry of subgrain boundaries the dislocation types can be determined, which form these boundaries. Three main types of subgrain boundaries have been recognized in Antarctic (EDML) ice core¹². Here, we present the first results obtained from EBSD measurements performed on the NEEM ice core samples from the last glacial period, focusing on the relevance of dislocation activity of the possible slip systems. Preliminary results show that all three subgrain types, recognized in the EDML core, occur in the NEEM samples. In addition to the classical boundaries made up of basal dislocations, subgrain boundaries made of non-basal dislocations are also common. ¹Weikusat, I.; de Winter, D. A. M.; Pennock, G. M.; Hayles, M.; Schneijdenberg, C. T. W. M. Drury, M. R. Cryogenic EBSD on ice: preserving a stable surface in a low pressure SEM. J. Microsc., 2010, doi: 10.1111/j.1365-2818.2010.03471.x ²Weikusat, I.; Miyamoto, A.; Faria, S. H.; Kipfstuhl, S.; Azuma, N.; Hondoh. T. Subgrain boundaries in Antarctic ice quantified by X-ray Laue diffraction. J. of Glaciol., 2011, 57, 85-94

Polycrystal-Plasticity Simulation of Roping in AA 6xxx Automotive Sheet Alloys

NASA Astrophysics Data System (ADS)

Engler, O.; Schäfer, C.; Brinkman, H.-J.

The occurrence of roping in AA 6xxx series sheet for car body applications is caused by the collective deformation of band-like clusters of grains with similar crystallographic orientation. In this study large-scale orientation maps obtained by electron back-scattered diffraction (EBSD) are input into a visco-plastic self-consistent polycrystal-plasticity model to analyze the strain anisotropy caused by the topographic arrangement of the recrystallization texture orientations and, in turn, the occurrence of roping. At variance to earlier studies, the measurements were carried out in the short transverse section of the sheets so as to get information on distribution and morphology of orientation clusters through the sheet thickness. Then, narrow bands in the EBSD maps aligned parallel to the ridges on the sheet surface are considered, and the variation in macroscopic strain response from band to band is determined. For a given deformation of the sample these simulations yield quantitative information on the level of roping of Al-alloy sheet for car body applications.

Delafossite structure of heterogenite polytypes (HCoO2) by Raman and infrared micro-spectroscopy

NASA Astrophysics Data System (ADS)

Burlet, C.; Goethals, H.; Vanbrabant, Y.

2016-04-01

Heterogenite is commonly referred in mineralogy literature as a cobalt oxy-hydroxide CoO(OH). However, detailed analysis of Raman and infrared spectra acquired on particularly well-crystallized natural samples of heterogenite suggests that the mineral can be characterized by a delafossite-type structure, with a general chemical formula ABO2. Indeed, the Raman spectrum of heterogenite, along the one with grimaldiite (HCrO2), lacks visible free OH-group vibrational modes, while the infrared spectrum shows strong hydrogen bond absorption bands. HCoO2 is thus a better formulation of heterogenite that describes more clearly its vibrational behavior and avoids the confusion in literature. Electronic backscattered diffraction (EBSD) is then used to distinguish and map the 2H and 3R heterogenite natural polytypes for the first time. The comparison of EBSD and Raman mappings clearly indicates that the 2H polytype is characterized by an additional peak at 1220 cm- 1. The presence/absence is therefore an efficient tool to distinguish both polytypes.

Understanding deformation with high angular resolution electron backscatter diffraction (HR-EBSD)

NASA Astrophysics Data System (ADS)

Britton, T. B.; Hickey, J. L. R.

2018-01-01

High angular resolution electron backscatter diffraction (HR-EBSD) affords an increase in angular resolution, as compared to ‘conventional’ Hough transform based EBSD, of two orders of magnitude, enabling measurements of relative misorientations of 1 x 10-4 rads (~ 0.006°) and changes in (deviatoric) lattice strain with a precision of 1 x 10-4. This is achieved through direct comparison of two or more diffraction patterns using sophisticated cross-correlation based image analysis routines. Image shifts between zone axes in the two-correlated diffraction pattern are measured with sub-pixel precision and this realises the ability to measure changes in interplanar angles and lattice orientation with a high degree of sensitivity. These shifts are linked to strains and lattice rotations through simple geometry. In this manuscript, we outline the basis of the technique and two case studies that highlight its potential to tackle real materials science challenges, such as deformation patterning in polycrystalline alloys.

Mechanistic Study of Delamination Fracture in Al-Li Alloy C458 (2099)

NASA Technical Reports Server (NTRS)

Tayon, W. A.; Crooks, R. E.; Domack, M. S.; Wagner, J. A.; Beaudoin, A. J.; McDonald, R. J.

2009-01-01

Delamination fracture has limited the use of lightweight Al-Li alloys. In the present study, electron backscattered diffraction (EBSD) methods were used to characterize crack paths in Al-Li alloy C458 (2099). Secondary delamination cracks in fracture toughness samples showed a pronounced tendency for fracture between grain variants of the same deformation texture component. These results were analyzed by EBSD mapping methods and simulated with finite element analyses. Simulation procedures include a description of material anisotropy, local grain orientations, and fracture utilizing crystal plasticity and cohesive zone elements. Taylor factors computed for each grain orientation subjected to normal and shear stresses indicated that grain pairs with the largest Taylor factor differences were adjacent to boundaries that failed by delamination. Examination of matching delamination fracture surface pairs revealed pronounced slip bands in only one of the grains bordering the delamination. These results, along with EBSD studies, plasticity simulations, and Auger electron spectroscopy observations support a hypothesis that delamination fracture occurs due to poor slip accommodation along boundaries between grains with greatly differing plastic response.

Exploring transmission Kikuchi diffraction using a Timepix detector

NASA Astrophysics Data System (ADS)

Vespucci, S.; Winkelmann, A.; Mingard, K.; Maneuski, D.; O'Shea, V.; Trager-Cowan, C.

2017-02-01

Electron backscatter diffraction (EBSD) is a well-established scanning electron microscope (SEM)-based technique [1]. It allows the non-destructive mapping of the crystal structure, texture, crystal phase and strain with a spatial resolution of tens of nanometers. Conventionally this is performed by placing an electron sensitive screen, typically consisting of a phosphor screen combined with a charge coupled device (CCD) camera, in front of a specimen, usually tilted 70° to the normal of the exciting electron beam. Recently, a number of authors have shown that a significant increase in spatial resolution is achievable when Kikuchi diffraction patterns are acquired in transmission geometry; that is when diffraction patterns are generated by electrons transmitted through an electron-transparent, usually thinned, specimen. The resolution of this technique, called transmission Kikuchi diffraction (TKD), has been demonstrated to be better than 10 nm [2,3]. We have recently demonstrated the advantages of a direct electron detector, Timepix [4,5], for the acquisition of standard EBSD patterns [5]. In this article we will discuss the advantages of Timepix to perform TKD and for acquiring spot diffraction patterns and more generally for acquiring scanning transmission electron microscopy micrographs in the SEM. Particularly relevant for TKD, is its very compact size, which allows much more flexibility in the positioning of the detector in the SEM chamber. We will furthermore show recent results using Timepix as a virtual forward scatter detector, and will illustrate the information derivable on producing images through processing of data acquired from different areas of the detector. We will show results from samples ranging from gold nanoparticles to nitride semiconductor nanorods.

Determination of dislocation density by electron backscatter diffraction and X-ray line profile analysis in ferrous lath martensite

DOE Office of Scientific and Technical Information (OSTI.GOV)

Berecz, Tibor, E-mail: berecz@eik.bme.hu; Jenei, Péter, E-mail: jenei@metal.elte.hu; Csóré, András, E-mail: csorean@gmail.com

2016-03-15

The microstructure and the dislocation density in as-quenched ferrous lath martensite were studied by different methods. The blocks, packets and variants formed due to martensitic transformation were identified and their sizes were determined by electron backscatter diffraction (EBSD). Concomitant transmission electron microscopy (TEM) investigation revealed that the laths contain subgrains with the size between 50 and 100 nm. A novel evaluation procedure of EBSD images was elaborated for the determination of the density and the space distribution of geometrically necessary dislocations from the misorientation distribution. The total dislocation density obtained by X-ray diffraction line profile analysis was in good agreementmore » with the value determined by EBSD, indicating that the majority of dislocations formed due to martensitic transformation during quenching are geometrically necessary dislocations.« less

Comparison of quartz crystallographic preferred orientations identified with optical fabric analysis, electron backscatter and neutron diffraction techniques.

PubMed

Hunter, N J R; Wilson, C J L; Luzin, V

2017-02-01

Three techniques are used to measure crystallographic preferred orientations (CPO) in a naturally deformed quartz mylonite: transmitted light cross-polarized microscopy using an automated fabric analyser, electron backscatter diffraction (EBSD) and neutron diffraction. Pole figure densities attributable to crystal-plastic deformation are variably recognizable across the techniques, particularly between fabric analyser and diffraction instruments. Although fabric analyser techniques offer rapid acquisition with minimal sample preparation, difficulties may exist when gathering orientation data parallel with the incident beam. Overall, we have found that EBSD and fabric analyser techniques are best suited for studying CPO distributions at the grain scale, where individual orientations can be linked to their source grain or nearest neighbours. Neutron diffraction serves as the best qualitative and quantitative means of estimating the bulk CPO, due to its three-dimensional data acquisition, greater sample area coverage, and larger sample size. However, a number of sampling methods can be applied to FA and EBSD data to make similar approximations. © 2016 The Authors Journal of Microscopy © 2016 Royal Microscopical Society.

Mechanical Twinning and Microstructures in Experimentally Stressed Quartzite

NASA Astrophysics Data System (ADS)

Minor, A.; Sintubin, M.; Wenk, H. R.; Rybacki, E.

2015-12-01

Since Dauphiné twins in quartz have been identified as a stress-related intracrystalline microstructure, several electron backscatter diffraction (EBSD) studies revealed that Dauphiné twins are present in naturally deformed quartz-bearing rocks in a wide range of tectono-metamorphic conditions. EBSD studies on experimentally stressed quartzite showed that crystals with particular crystallographic orientations contain many Dauphiné twin boundaries, while neighboring crystals with different orientations are largely free of twin boundaries. To understand the relationship between stress direction and orientation of Dauphiné twinned quartz crystals, a detailed EBSD study was performed on experimentally stressed quartzite samples and compared with an undeformed reference sample. We stressed 4 cylindrical samples in triaxial compression in a Paterson type gas deformation apparatus at GFZ Potsdam. Experimental conditions were 300MPa confining pressure, 500°C temperature and axial stresses of 145MPa, 250MPa and 460MPa for about 30 hours, resulting in a minor strain <0.04%. EBSD scans were obtained with a Zeiss Evo scanning electron microscope and TSL software at UC Berkeley. The EBSD maps show that Dauphiné twinning is present in the starting material as well as in experimentally stressed samples. Pole figures of the bulk orientation of the reference sample compared with stressed samples show a significant difference regarding the distribution for the r and z directions. The reference sample shows an indistinct maximum for r and z, whereas the stressed samples show a maximum for r poles and a minimum for z poles in the axial stress direction. EBSD scans of the reference and stressed samples were further analyzed manually to identify the orientations of single grains, which are free of twin boundaries and those, which contain twin boundaries. This analysis aims to quantify the relationship of crystal orientation and stress magnitude to initiate mechanical twinning.

On the use of SEM correlative tools for in situ mechanical tests.

PubMed

Shi, Qiwei; Roux, Stéphane; Latourte, Félix; Hild, François; Loisnard, Dominique; Brynaert, Nicolas

2018-01-01

In situ SEM mechanical tests are key to study crystal plasticity. In particular, imaging and diffraction (EBSD) allow microstructure and surface kinematics to be monitored all along the test. However, to get a full benefit from different modalities, it is necessary to register all images and crystallographic orientation maps from EBSD into the same frame. Different correlative approaches tracking either Pt surface markings, crystal orientations or grain boundaries, allow such registrations to be performed and displacement as well as rotation fields to be measured, a primary information for crystal plasticity identification. However, the different contrasts that are captured in different modalities and unavoidable stage motions also give rise to artifacts that are to be corrected to register the different information onto the same material points. The same image correlation tools reveal very powerful to correct such artifacts. Illustrated by an in situ uniaxial tensile test performed on a bainitic-ferritic steel sample, recent advances in image correlation techniques are reviewed and shown to provide a comprehensive picture of local strain and rotation maps. Copyright © 2017 Elsevier B.V. All rights reserved.

Structural and crystal orientation analysis of Al-Si coating on Ni-based superalloy by means of EBSD technique

NASA Astrophysics Data System (ADS)

Muslimin, A. N.; Sugiarti, E.; Aritonang, T.; Purawiardi, R. I.; Desiati, R. D.

2018-03-01

Ni-based superalloy is widely used for high performance components in power generation turbine due to its excellent mechanical properties. However, Ni-based superalloy has low oxidation resistantance. Therefore, surface coating is required to improve oxidation resistance at high temperatures. Al-Si as a coting material was successfully co-deposited on Ni-based substrate by pack cementation method at 900 °C for about 4 hours. The oxidation test was carried out at high temperature of 1000 °C for 100 hours. Micro structural characterization and analysis on crystal orientation were perfomed by using Field Emission Scanning Electron Microscope (FE-SEM) and Electron Back Scatter Diffraction (EBSD) technique, respectively. The results showed that the coating layer with a homogenous layer and had a thickness of 53 μm consisting of β-NiAl with cubic structure and Ni2Al3 with hexagonal structure. TGO layer was developed after oxidation and had a thickness of about 5 μm consisting of α-Al2O3 and spinel NiCr2O4. The phase composition map and crystal orientation acquired by EBSD technique was also discussed both in TGO and coating layers.

Strain Evolution in Cold-Warm Forged Steel Components Studied by Means of EBSD Technique

PubMed Central

Bonollo, Franco; Bassan, Fabio; Berto, Filippo

2017-01-01

Electron BackScatter Diffraction (EBSD) in conjunction with Field-Emission Environmental Scanning Electron Microscopy (FEG-ESEM) has been used to evaluate the microstructural and local plastic strain evolution in different alloys (AISI 1005, AISI 304L and Duplex 2205) deformed by a single-stage cold and warm forging process. The present work is aimed to describe the different behavior of the austenite and ferrite during plastic deformation as a function of different forging temperatures. Several topological EBSD maps have been measured on the deformed and undeformed states. Then, image quality factor, distributions of the grain size and misorientation have been analyzed in detail. In the austenitic stainless steel, the γ-phase has been found to harden more easily, then α-phase and γ-phase in AISI 1005 and in duplex stainless steel, sequentially. Compared to the high fraction of continuous dynamic recrystallized austenitic zones observed in stainless steels samples forged at low temperatures, the austenitic microstructure of samples forged at higher temperatures, 600–700 °C, has been found to be mainly characterized by large and elongated grains with some colonies of fine nearly-equiaxed grains attributed to discontinuous dynamic recrystallization. PMID:29258249

Three-dimensional full-field X-ray orientation microscopy

PubMed Central

Viganò, Nicola; Tanguy, Alexandre; Hallais, Simon; Dimanov, Alexandre; Bornert, Michel; Batenburg, Kees Joost; Ludwig, Wolfgang

2016-01-01

A previously introduced mathematical framework for full-field X-ray orientation microscopy is for the first time applied to experimental near-field diffraction data acquired from a polycrystalline sample. Grain by grain tomographic reconstructions using convex optimization and prior knowledge are carried out in a six-dimensional representation of position-orientation space, used for modelling the inverse problem of X-ray orientation imaging. From the 6D reconstruction output we derive 3D orientation maps, which are then assembled into a common sample volume. The obtained 3D orientation map is compared to an EBSD surface map and local misorientations, as well as remaining discrepancies in grain boundary positions are quantified. The new approach replaces the single orientation reconstruction scheme behind X-ray diffraction contrast tomography and extends the applicability of this diffraction imaging technique to material micro-structures exhibiting sub-grains and/or intra-granular orientation spreads of up to a few degrees. As demonstrated on textured sub-regions of the sample, the new framework can be extended to operate on experimental raw data, thereby bypassing the concept of orientation indexation based on diffraction spot peak positions. This new method enables fast, three-dimensional characterization with isotropic spatial resolution, suitable for time-lapse observations of grain microstructures evolving as a function of applied strain or temperature. PMID:26868303

DOE Office of Scientific and Technical Information (OSTI.GOV)

Tumurugoti, P.; Clark, B.M.; Edwards, D.J.

Hollandite-rich multiphase waste form compositions processed by melt-solidification and spark plasma sintering (SPS) were characterized, compared, and validated for nuclear waste incorporation. Phase identification by x-ray diffraction (XRD) and electron back-scattered diffraction (EBSD) confirmed hollandite as the major phase present in these samples along with perovskite, pyrochlore and zirconolite. Distribution of selected elements observed by wavelength dispersive spectroscopy (WDS) maps indicated that Cs formed a secondary phase during SPS processing, which was considered undesirable. On the other hand, Cs partitioned into the hollandite phase in melt-processed samples. Further analysis of hollandite structure in melt-processed composition by selected area electron diffractionmore » (SAED) revealed ordered arrangement of tunnel ions (Ba/Cs) and vacancies, suggesting efficient Cs incorporation into the lattice.« less

Microstructural investigations of 0.2% carbon content steel

NASA Astrophysics Data System (ADS)

Tollabimazraehno, Sajjad; Hingerl, Kurt

2011-10-01

The effect of thermal annealing to get different phases on low carbon steel was investigated. Steel sheets (0.2 wt. % C) of 900 μm thickness were heat treated to produce different structures. All the samples have the same starting point, transformation to coarse austenite at 900 degree Celsius. The nano indentation results revealed that samples have different hadness. By making conventional SEM micrographs, focus ion beam maps, and Electron backscatter diffraction (EBSD) the microstructural development and grain boundary variation of transformed phases martensite, biainte, tempered martensite and different combination of these phases were studied.

In-depth quantitative analysis of the microstructures produced by Surface Mechanical Attrition Treatment (SMAT)

DOE Office of Scientific and Technical Information (OSTI.GOV)

Samih, Y., E-mail: youssef.samih@univ-lorraine.fr; Université de Lorraine, Laboratory of Excellence on Design of Alloy Metals for low-mAss Structures; Beausir, B.

2013-09-15

Electron BackScattered Diffraction (EBSD) maps are used to characterize quantitatively the graded microstructure formed by Surface Mechanical Attrition Treatment (SMAT) and applied here to the 316L stainless steel. In particular, the analysis of GNDs – coupled with relevant and reliable criteria – was used to depict the thickness of each zone identified in the SMAT-affected layers: (i) the “ultrafine grain” (UFG) zone present at the extreme top surface, (ii), the “transition zone” where grains were fragmented under the heavy plastic deformation and, finally, (iii) the “deformed zone” where initial grains are simply deformed. The interest of this procedure is illustratedmore » through the comparative analysis of the effect of some SMAT processing parameters (amplitude of vibration and treatment duration). The UFG and transition zones are more significantly modified than the overall affected thickness under our tested conditions. - Highlights: • EBSD maps are used to characterize quantitatively the microstructure of SMAT treated samples. • Calculation of the GND density to quantify strain gradients • A new method to depict the different zone thicknesses in the SMAT affected layer • Effects of SMAT processing parameters on the surface microstructure evolution.« less

Evolution of weld metal microstructure in shielded metal arc welding of X70 HSLA steel with cellulosic electrodes: A case study

DOE Office of Scientific and Technical Information (OSTI.GOV)

Ghomashchi, Reza, E-mail: reza.ghomashchi@adelaide.edu.au; Costin, Walter; Kurji, Rahim

2015-09-15

The microstructure of weld joint in X70 line pipe steel resulted from shielded metal arc welding with E6010 cellulosic electrodes is characterized using optical and electron microscopy. A range of ferritic morphologies have been identified ranging from polygonal inter- and intra-prior austenite grains allotriomorphic, idiomorphic ferrites to Widmanstätten, acicular and bainitic ferrites. Electron Backscatter Diffraction (EBSD) analysis using Image Quality (IQ) and Inverse Pole Figure (IPF) maps through superimposition of IQ and IPF maps and measurement of percentages of high and low angle grain boundaries was identified to assist in differentiation of acicular ferrite from Widmanstätten and bainitic ferrite morphologies.more » In addition two types of pearlitic structures were identified. There was no martensite detected in this weld structure. The morphology, size and chemistry of non-metallic inclusions are also discussed briefly. - Highlights: • Application of EBSD reveals orientation relationships in a range of phases for shielded metal arc welding of HSLA steel. • Nucleation sites of various ferrite morphologies identified • Formation of upper and lower bainite and their morphologies.« less

Large Area Stress Distribution in Crystalline Materials Calculated from Lattice Deformation Identified by Electron Backscatter Diffraction

NASA Astrophysics Data System (ADS)

Shao, Yongliang; Zhang, Lei; Hao, Xiaopeng; Wu, Yongzhong; Dai, Yuanbin; Tian, Yuan; Huo, Qin

2014-08-01

We report a method to obtain the stress of crystalline materials directly from lattice deformation by Hooke's law. The lattice deformation was calculated using the crystallographic orientations obtained from electron backscatter diffraction (EBSD) technology. The stress distribution over a large area was obtained efficiently and accurately using this method. Wurtzite structure gallium nitride (GaN) crystal was used as the example of a hexagonal crystal system. With this method, the stress distribution of a GaN crystal was obtained. Raman spectroscopy was used to verify the stress distribution. The cause of the stress distribution found in the GaN crystal was discussed from theoretical analysis and EBSD data. Other properties related to lattice deformation, such as piezoelectricity, can also be analyzed by this novel approach based on EBSD data.

Large area stress distribution in crystalline materials calculated from lattice deformation identified by electron backscatter diffraction.

PubMed

Shao, Yongliang; Zhang, Lei; Hao, Xiaopeng; Wu, Yongzhong; Dai, Yuanbin; Tian, Yuan; Huo, Qin

2014-08-05

We report a method to obtain the stress of crystalline materials directly from lattice deformation by Hooke's law. The lattice deformation was calculated using the crystallographic orientations obtained from electron backscatter diffraction (EBSD) technology. The stress distribution over a large area was obtained efficiently and accurately using this method. Wurtzite structure gallium nitride (GaN) crystal was used as the example of a hexagonal crystal system. With this method, the stress distribution of a GaN crystal was obtained. Raman spectroscopy was used to verify the stress distribution. The cause of the stress distribution found in the GaN crystal was discussed from theoretical analysis and EBSD data. Other properties related to lattice deformation, such as piezoelectricity, can also be analyzed by this novel approach based on EBSD data.

Large Area Stress Distribution in Crystalline Materials Calculated from Lattice Deformation Identified by Electron Backscatter Diffraction

PubMed Central

Shao, Yongliang; Zhang, Lei; Hao, Xiaopeng; Wu, Yongzhong; Dai, Yuanbin; Tian, Yuan; Huo, Qin

2014-01-01

We report a method to obtain the stress of crystalline materials directly from lattice deformation by Hooke's law. The lattice deformation was calculated using the crystallographic orientations obtained from electron backscatter diffraction (EBSD) technology. The stress distribution over a large area was obtained efficiently and accurately using this method. Wurtzite structure gallium nitride (GaN) crystal was used as the example of a hexagonal crystal system. With this method, the stress distribution of a GaN crystal was obtained. Raman spectroscopy was used to verify the stress distribution. The cause of the stress distribution found in the GaN crystal was discussed from theoretical analysis and EBSD data. Other properties related to lattice deformation, such as piezoelectricity, can also be analyzed by this novel approach based on EBSD data. PMID:25091314

User-independent EBSD parameters to study the progress of recovery and recrystallization in Cu-Zn alloy during in situ heating.

PubMed

Sharma, N K; Shekhar, S

2016-12-01

Microstructural evolution of cold-rolled Cu-5%Zn alloy during in situ heating inside field-emission scanning electron microscope was utilized to obtain user-independent parameters in order to trace the progress of static recovery and recrystallization. Electron back-scattered diffraction (EBSD)-based orientation imaging microscopy was used to obtain micrographs at various stages of in situ heating. It is shown that unlike the pre-existing methods, additional EBSD-based parameter can be used to trace the progress of recovery and recrystallization, which is not dependent on user input and hence less prone to error. True strain of 0.3 was imposed during cold rolling of alloy sample. Rolled sample was subjected to in situ heating from room temperature to 500°C (∼0.58 Tm) with soaking time of 10 min, at each of the intermediate temperatures viz. 100, 200, 300, 400 and 450°C. After reaching 500°C, the sample was kept at this temperature for a maximum duration of around 15 h. The sample showed clear signs of recovery for temperature up to 450°C, and at 500°C, recrystallization started to take place. Recrystallization kinetics was moderate, and full recrystallization was achieved in approximately 120 min. We found that EBSD parameter, namely, band contrast intensity can be used as an extra handle to map out the progress of recrystallization occurring in the sample. By contrast, mean angular deviation can be used to understand the evolution of recovery in samples. The parameters mentioned in the current study, unlike other pre-existing methods, can also be used for mapping local microstructural transformations due to recovery and recrystallization. We discuss the benefits and limitations in using these additional handles in understanding the changes taking place in the material during in situ heating. © 2016 The Authors Journal of Microscopy © 2016 Royal Microscopical Society.

Detail Extraction from Electron Backscatter Diffraction Patterns

NASA Astrophysics Data System (ADS)

Basinger, Jay

Cross-correlation based analysis of electron backscatter diffraction (EBSD) patterns and the use of simulated reference patterns has opened up entirely new avenues of insight into local lattice properties within EBSD scans. The benefits of accessing new levels of orientation resolution and multiple types of previously inaccessible data measures are accompanied with new challenges in characterizing microscope geometry and other error previously ignored in EBSD systems. The foremost of these challenges, when using simulated patterns in high resolution EBSD (HR-EBSD), is the determination of pattern center (the location on the sample from which the EBSD pattern originated) with sufficient accuracy to avoid the introduction of phantom lattice rotations and elastic strain into these highly sensitive measures. This dissertation demonstrates how to greatly improve pattern center determination. It also presents a method for the extraction of grain boundary plane information from single two-dimensional surface scans. These are accomplished through the use of previously un-accessed detail within EBSD images, coupled with physical models of the backscattering phenomena. A software algorithm is detailed and applied for the determination of pattern center with an accuracy of ˜0.03% of the phosphor screen width, or ˜10μm. This resolution makes it possible to apply a simulated pattern method (developed at BYU) in HR-EBSD, with several important benefits over the original HR-EBSD approach developed by Angus Wilkinson. Experimental work is done on epitaxially-grown silicon and germanium in order to gauge the precision of HR-EBSD with simulated reference patterns using the new pattern center calibration approach. It is found that strain resolution with a calibrated pattern center and simulated reference patterns can be as low as 7x10-4. Finally, Monte Carlo-based models of the electron interaction volume are used in conjunction with pattern-mixing-strength curves of line scans crossing grain boundaries in order to recover 3D grain boundary plane information. Validation of the approach is done using 3D serial scan data and coherent twin boundaries in tantalum and copper. The proposed method for recovery of grain boundary plane orientation exhibits an average error of 3 degrees.

Skeletal growth phases of the cold-water coral Lophelia pertusa shown by scanning electron microscope and electron backscatter diffraction

NASA Astrophysics Data System (ADS)

Mouchi, Vincent; Vonlanthen, Pierre; Verrecchia, Eric P.; Crowley, Quentin G.

2016-04-01

Lophelia pertusa is a cold-water coral, which may form reefs by the association of multiple coralites within which a polyp lives. Each individual polyp builds an aragonite skeleton by an initial phase of early mineralization (traditionally referred to as centres of calcification) from which aragonite fibres grow in thickening deposits. The skeleton wall features successive optically opaque and translucent bands previously attributed to different regimes of growth as either uniform in crystal orientation (translucent bands) or with a chaotic organization (opaque bands). The processes involved in any organizational changes are still unknown. Microlayers in the coral wall, which represent separate periods of skeletal growth, have been recently identified and described. These growth patterns are readily visible under scanning electron microscope (SEM) after etching in dilute formic acid, but they do not necessarily form continuously visible structures. Here we present high quality SEM images and electron backscatter diffraction (EBSD) maps to study aragonite fibre orientation across the wall of L. pertusa. Both microlayers and opaque and translucent bands are compared to the crystallographic orientation of the aragonite fibres. EBSD maps and SEM images indicate that aragonite fibres do not exhibit a chaotic orientation, even in opaque bands. The absence of continuity of microlayers is partially explained by an association of multiple crystallographic preferred orientations of aragonite fibres. In the case of L. pertusa, careful textural characterisation is necessary prior to elemental or isotope analysis in order to select a skeletal transect representing a linear and continuous time period.

Damage Assessment of Heat Resistant Steels through Electron BackScatter Diffraction Strain Analysis under Creep and Creep-Fatigue Conditions

NASA Astrophysics Data System (ADS)

Fujiyama, Kazunari; Kimachi, Hirohisa; Tsuboi, Toshiki; Hagiwara, Hiroyuki; Ogino, Shotaro; Mizutani, Yoshiki

EBSD(Electron BackScatter Diffraction) analyses were conducted for studying the quantitative microstructural metrics of creep and creep-fatigue damage for austenitic SUS304HTB boiler tube steel and ferritic Mod.9Cr piping steel. KAM(Kernel Average Misorientation) maps and GOS(Grain Orientation Spread) maps were obtained for these samples and the area averaged values KAMave and GOSave were obtained. While the increasing trends of these misorientation metrics were observed for SUS304HTB steel, the decreasing trends were observed for damaged Mod.9Cr steel with extensive recovery of subgrain structure. To establish more universal parameter representing the accumulation of damage to compensate these opposite trends, the EBSD strain parameters were introduced for converting the misorientation changes into the quantities representing accumulated permanent strains during creep and creep-fatigue damage process. As KAM values were dependent on the pixel size (inversely proportional to the observation magnification) and the permanent strain could be expressed as the shear strain which was the product of dislocation density, Burgers vector and dislocation movement distance, two KAM strain parameters MεKAMnet and MεδKAMave were introduced as the sum of product of the noise subtracted KAMnet and the absolute change from initial value δKAMave with dislocation movement distance divided by pixel size. MεδKAMave parameter showed better relationship both with creep strain in creep tests and accumulated creep strain range in creep-fatigue tests. This parameter can be used as the strain-based damage evaluation and detector of final failure.

Tutorial: Crystal orientations and EBSD — Or which way is up?

DOE Office of Scientific and Technical Information (OSTI.GOV)

Britton, T.B., E-mail: b.britton@imperial.ac.uk; Jiang, J.; Guo, Y.

2016-07-15

Electron backscatter diffraction (EBSD) is an automated technique that can measure the orientation of crystals in a sample very rapidly. There are many sophisticated software packages that present measured data. Unfortunately, due to crystal symmetry and differences in the set-up of microscope and EBSD software, there may be accuracy issues when linking the crystal orientation to a particular microstructural feature. In this paper we outline a series of conventions used to describe crystal orientations and coordinate systems. These conventions have been used to successfully demonstrate that a consistent frame of reference is used in the sample, unit cell, pole figuremore » and diffraction pattern frames of reference. We establish a coordinate system rooted in measurement of the diffraction pattern and subsequently link this to all other coordinate systems. A fundamental outcome of this analysis is to note that the beamshift coordinate system needs to be precisely defined for consistent 3D microstructure analysis. This is supported through a series of case studies examining particular features of the microscope settings and/or unambiguous crystallographic features. These case studies can be generated easily in most laboratories and represent an opportunity to demonstrate confidence in use of recorded orientation data. Finally, we include a simple software tool, written in both MATLAB® and Python, which the reader can use to compare consistency with their own microscope set-up and which may act as a springboard for further offline analysis. - Highlights: • Presentation of conventions used to describe crystal orientations • Three case studies that outline how conventions are consistent • Demonstrates a pathway for calibration and validation of EBSD based orientation measurements • EBSD computer code supplied for validation by the reader.« less

Application of Electron Backscatter Diffraction to evaluate the ASR risk of concrete aggregates

DOE Office of Scientific and Technical Information (OSTI.GOV)

Rößler, C., E-mail: christiane.roessler@uni-weimar.de; Möser, B.; Giebson, C.

Alkali-Silica Reaction (ASR) is a frequent cause of reduced concrete durability. Eliminating the application of alkali reactive aggregates would reduce the quantity of ASR concrete deterioration in the field. This study introduces an Electron Backscatter Diffraction (EBSD) technique to distinguish the ASR risk of slow-late reacting aggregates by measuring microstructural properties of quartz. Quantifying the amount of quartz grain boundaries and the associated misorientation of grains can thereby be used to differentiate microstructures bearing an ASR risk. It is also shown that dissolution of quartz in high pH environments occurs along quartz grain and subgrain boundaries. Results of EBSD analysismore » are compared with ASR performance testing on concrete prisms and optical light microscopy characterization of quartz microstructure. EBSD opens new possibilities to quantitatively characterize microstructure of quartz in concrete aggregates with respect to ASR. This leads to a better understanding on the actual cause of ASR.« less

Evolution of the substructure of a novel 12% Cr steel under creep conditions

DOE Office of Scientific and Technical Information (OSTI.GOV)

Yadav, Surya Deo, E-mail: surya.yadav@tugraz.at; Kalácska, Szilvia, E-mail: kalacska@metal.elte.hu; Dománková, Mária, E-mail: maria.domankova@stuba.sk

2016-05-15

In this work we study the microstruture evolution of a newly developed 12% Cr martensitic/ferritic steel in as-received condition and after creep at 650 °C under 130 MPa and 80 MPa. The microstructure is described as consisting of mobile dislocations, dipole dislocations, boundary dislocations, precipitates, lath boundaries, block boundaries, packet boundaries and prior austenitic grain boundaries. The material is characterized employing light optical microscopy (LOM), scanning electron microscopy (SEM), transmission electron microscopy (TEM), X-ray diffraction (XRD) and electron backscatter diffraction (EBSD). TEM is used to characterize the dislocations (mobile + dipole) inside the subgrains and XRD measurements are used tomore » the characterize mobile dislocations. Based on the subgrain boundary misorientations obtained from EBSD measurements, the boundary dislocation density is estimated. The total dislocation density is estimated for the as-received and crept conditions adding the mobile, boundary and dipole dislocation densities. Additionally, the subgrain size is estimated from the EBSD measurements. In this publication we propose the use of three characterization techniques TEM, XRD and EBSD as necessary to characterize all type of dislocations and quantify the total dislocation densty in martensitic/ferritic steels. - Highlights: • Creep properties of a novel 12% Cr steel alloyed with Ta • Experimental characterization of different types of dislocations: mobile, dipole and boundary • Characterization and interpretation of the substructure evolution using unique combination of TEM, XRD and EBSD.« less

Anelasticity of olivine single crystals investigated by stress-reduction tests and high-angular resolution electron backscatter diffraction

NASA Astrophysics Data System (ADS)

Wallis, D.; Hansen, L. N.; Kempton, I.; Wilkinson, A. J.

2017-12-01

Geodynamic phenomena, including glacial isostatic adjustment and postseismic deformation, can involve transient deformation in response to changes in differential stress acting on mantle rocks. As such, rheological models of transient deformation are incorporated in predictions of associated processes, including sea-level rise and stress redistribution after earthquakes. However, experimental constraints on rheological models for transient deformation of mantle materials are sparse. In particular, experiments involving stress reductions have been lacking. Moreover, a material's response to a reduction in stress can provide clues to the microphysical processes controlling deformation. To constrain models of transient deformation of mantle rocks we performed stress-reduction tests on single crystals of olivine at 1250-1300°C. Mechanical and piezoelectric actuators controlled constant initial stress during creep. At various strain intervals stress was reduced near-instantaneously using the piezoelectric actuator, inducing both elastic and anelastic (time-dependent) lengthening of the samples. A range of magnitudes of stress reduction were applied, typically unloading 10-90% of the initial stress. High-angular resolution electron backscatter diffraction (HR-EBSD), based on cross-correlation of diffraction patterns, was used to map dislocation density and elastic strain distributions in the recovered samples. Magnitudes of anelastic back-strain increase with increasing magnitudes of stress reduction and show a marked increase when stress reductions exceed 50% of the initial stress, consistent with previous observations in metals and alloys. This observation is inconsistent with the Burgers rheological model commonly used to describe transient behaviour and suggests that the style of rheological behaviour depends on the magnitude of stress change. HR-EBSD maps reveal that the crystal lattices are smoothly curved and generally lack subgrain boundaries and elastic strain heterogeneities. The dependence of the anelastic behaviour on the initial stress, combined with the lack of subgrain boundaries, suggest that the anelastic behaviour is controlled by local interactions between dislocations, rather than resistance imposed by the lattice or subgrain boundaries.

Energy-weighted dynamical scattering simulations of electron diffraction modalities in the scanning electron microscope.

PubMed

Pascal, Elena; Singh, Saransh; Callahan, Patrick G; Hourahine, Ben; Trager-Cowan, Carol; Graef, Marc De

2018-04-01

Transmission Kikuchi diffraction (TKD) has been gaining momentum as a high resolution alternative to electron back-scattered diffraction (EBSD), adding to the existing electron diffraction modalities in the scanning electron microscope (SEM). The image simulation of any of these measurement techniques requires an energy dependent diffraction model for which, in turn, knowledge of electron energies and diffraction distances distributions is required. We identify the sample-detector geometry and the effect of inelastic events on the diffracting electron beam as the important factors to be considered when predicting these distributions. However, tractable models taking into account inelastic scattering explicitly are lacking. In this study, we expand the Monte Carlo (MC) energy-weighting dynamical simulations models used for EBSD [1] and ECP [2] to the TKD case. We show that the foil thickness in TKD can be used as a means of energy filtering and compare band sharpness in the different modalities. The current model is shown to correctly predict TKD patterns and, through the dictionary indexing approach, to produce higher quality indexed TKD maps than conventional Hough transform approach, especially close to grain boundaries. Copyright © 2018 The Authors. Published by Elsevier B.V. All rights reserved.

Lattice-Preferred Orientation in Deformed Novaculite - Comparison of in-situ Results Using BEARTEX and Post-Mortem EBSD Analyses

NASA Astrophysics Data System (ADS)

Willenweber, A.; Thomas, S.; Burnley, P. C.

2012-12-01

The Berkeley Texture Package BEARTEX is a Windows-based computer software that combines various algorithms to analyze lattice-preferred orientation in polycrystalline materials. BEARTEX was initially designed to interpret diffraction intensity data from pole figure goniometers. Recently it has been successfully used to process synthetic forsterite powder diffraction data from in-situ synchrotron X-ray diffraction taken during deformation (Bollinger et al. 2012). Our study aims to test the practicability of using BEARTEX to analyze the evolution of lattice-preferred orientation in natural polycrystalline quartz (novaculite) during deformation. In-situ X-ray diffraction data was collected during the deformation of novaculite at 2.5 GPa and up to 1000 °C in a D-DIA apparatus using the ten-element energy-dispersive detector at the NSLS beamline X17B2. Diffraction intensities are a function of crystal orientation, expressed in azimuth angle η and pole distance ψ. The latter is the angle between the normal of a given diffraction plane and the vertical direction of the D-DIA apparatus - our principal stress direction during compression. Orientation-dependent diffraction intensities were corrected for different responses of the single detectors and x-ray absorption effects of the anvils. Orientation distributions (ODs) and inverse pole figures were calculated using BEARTEX. In addition, electron backscatter diffraction (EBSD) analyses were carried out on the deformed novaculite samples. Generated pole figures were compared with those derived from BEARTEX. Textural properties of our novaculite starting material complicated the BEARTEX analyses. The relatively strong variation of grain sizes in our natural specimens caused non-random diffraction intensity distributions. Those lead to non-random distributions of crystal orientations when analyzed with BEARTEX, although pole figures from EBSD data clearly show random crystal orientations. In an attempt to solve this problem, we employed a scanning routine when recording in-situ synchrotron X-ray diffraction and so collected diffraction from multiple sample volumes rather than from one single spot. Here, we will present a comparison of pole figures derived from independent BEARTEX and EBSD analyses for a series of novaculite experiments and discuss the practicability of BEARTEX to analyze the evolution of lattice-preferred orientation in natural polycrystalline quartz. REFERENCES C. BOLLINGER, S. MERKEL AND P. RATERRON (2012): In situ quantitative analysis of stress and texture development in forsterite aggregates deformed at 6 GPa and 1373 K. J. Appl. Cryst., 45, 263-271.

Chromium Grain-boundary Segregation and Effect of Ion Beam Cleaning on Fe-Ni-Cr Alloys

DOE Office of Scientific and Technical Information (OSTI.GOV)

Saraf, Laxmikant V.

2011-04-01

The grain boundaries play important role to control the mechanical strength of ternary alloys. From spacecrafts to naval vessels to nuclear reactors, stress corrosion cracking, brittleness, oxidation mostly originates at the grain boundaries and cause long term structural stability problems in most of the metallic structures [1]. Fe-Ni-Cr based ternary metal alloys have been widely studied for more than fifty years [2, 3]. Despite of vast amount of research, chromium diffusion in stainless steel or other Ni-Fe-Cr based ternary alloys is still an open scientific problem with challenges in structural stability and corrosion resistance [4]. Particularly, austenite Fe-Ni-Cr is lookedmore » upon favorably in space and jet engine industry for their improved resistance to stress corrosion cracking [5]. In solid oxide fuel cells (SOFC), Ni-alloys are frequently used as interconnects and seals [6]. In this communication, simultaneous energy dispersive spectroscopy (EDS) and electron backscatter diffraction (EBSD) mapping is utilized to study chemical and structural aspects of chromium segregation in Fe-Ni-Cr alloy. A focused Ga-ion beam is also utilized to study the effect of ion beam cleaning on EBSD image quality (IQ) and inverse pole figure (IPF) maps of Fe-Ni-Cr alloy.« less

DOE Office of Scientific and Technical Information (OSTI.GOV)

Wang, Yiyu; Kannan, Rangasayee; Li, Leijun, E-mail

Non-equilibrium microstructure of the heat-affected zone (HAZ) in the as-welded modified 9Cr–1Mo–V–Nb pipe steel (P91) weldment deposited by gas tungsten arc welding (GTAW) and flux core arc welding (FCAW) has been characterized by field-emission scanning electron microscope (FESEM) and electron backscatter diffraction (EBSD). The heterogeneous structures in the sub-layers of the as-welded HAZ are attributable to phase transformations caused by the welding thermal cycles and the local structure variations in the as-received base metal. Coarse-grained heat-affected zone (CGHAZ) has a prior austenite grain (PAG) size of 20 μm. Fine uniformly-distributed precipitates and a higher fraction of MX carbonitrides are observedmore » in the CGHAZ. Fine-grained heat-affected zone (FGHAZ) consists of the finest grains (1.22 μm measured by EBSD, 5 μm PAG size), coarse undissolved M{sub 23}C{sub 6} carbides within the PAG boundaries and fine nucleated M{sub 23}C{sub 6} particles within the martensite laths. Inter-critical heat-affected zone (ICHAZ) consists of partially austenitized grains and over-tempered martensite laths. EBSD kernel average misorientation (KAM) map in the FGHAZ close to the ICHAZ illustrates the greatest local strain variations with a moderate normalized KAM value of 0.92°. The majority (88.1%) of the matrix grains in the CGHAZ are classified as deformed grains by EBSD grain average misorientation (GAM) evaluation. The FGHAZ close to the ICHAZ has the most recrystallized grains with an area fraction of 14.4%. The highest density variation of precipitates within grains in the FGHAZ originates from the inhomogeneous chemistry in the base metal. - Highlights: •A comprehensive characterization of the as-welded HAZ of P91 weldment is conducted. •Structural features in the each layer of the HAZ are quantified by EBSD. •Structural heterogenities in HAZ are due to welding cycle and base metal structure. •FGHAZ contains the finest grain structure and largest precipitate density variation.« less

Microstructure, crystallography and diagenetic alteration in fossil ostrich eggshells from Upper Palaeolithic sites of Indian peninsular region.

PubMed

Jain, Sonal; Bajpai, Sunil; Kumar, Giriraj; Pruthi, Vikas

2016-05-01

Biominerals studies are of importance as they provide an understanding of natural evolutionary processes. In this study we have investigated the fossil ostrich eggshells using Scanning Electron Microscopy (SEM), X-ray Diffraction (XRD) and Electron Backscatter Diffraction (EBSD). SEM studies demonstrated the ultrastructure of fossil eggshells and formation of calcified cuticular layer. The presence of calcified cuticle layer in eggshell is the basis for ancient DNA studies as it contains preserved biomolecules. EBSD accentuates the crystallographic structure of the ostrich eggshells with sub-micrometer resolution. It is a non-destructive tool for evaluating the extent of diagenesis in a biomineral. EBSD analysis revealed the presence of dolomite in the eggshells. This research resulted in the complete recognition of the structure of ostrich eggshells as well as the nature and extent of diagenesis in these eggshells which is vital for genetic and paleoenvironmental studies. Copyright © 2016 Elsevier Ltd. All rights reserved.

Combined application of electron backscatter diffraction and stereo-photogrammetry in fractography studies.

PubMed

Davies, P A; Randle, V

2001-10-01

The main aim of this paper is to report on recent experimental developments that have succeeded in combining electron back-scatter diffraction (EBSD) with stereo-photogrammetry, compared with two other methods for study of fracture surfaces, namely visual fractography analysis in the scanning electron microscope (SEM) and EBSD directly from facets. These approaches will be illustrated with data relating to the cleavage plane orientation analysis in a ferritic and C-Mn steel. It is demonstrated that the combined use of EBSD and stereo-photogrammetry represents a significant advance in the methodology for facet crystallography analysis. The results of point counting from fractograph characterization determined that the proportions of intergranular fracture in C-Mn and ferritic steels were 10.4% and 9.4%, respectively. The crystallographic orientation was determined directly from the fracture surface of a ferritic steel sample and produced an orientation distribution with a clear trend towards the [001] plane. A stereo-photogrammetry technique was validated using the known geometry of a Vickers hardness indent. The technique was then successfully employed to measure the macroscopic orientation of individual cleavage facets in the same reference frame as the EBSD measurements. Correlating the results of these measurements indicated that the actual crystallographic orientation of every cleavage facet identified in the steel specimens is [001].

Study of Etching Pits in a Large-grain Single Cell Bulk Niobium Cavity

DOE Office of Scientific and Technical Information (OSTI.GOV)

Zhao, Xin; Ciovati, Gianluigi; Reece, Charles E.

2009-11-01

Performance of SRF cavities are limited by non-linear localized effects. The variation of local material characters between "hot" and "cold" spots is thus of intense interest. Such locations were identified in a BCP-etched large-grain single-cell cavity and removed for examination by high resolution electron microscopy (SEM), electron-back scattering diffraction microscopy (EBSD), optical microscopy, and 3D profilometry. Pits with clearly discernable crystal facets were observed in both "hotspot" and "coldspot" specimens. The pits were found in-grain, at bi-crystal boundaries, and on tri-crystal junctions. They are interpreted as etch pits induced by surface crystal defects (e.g. dislocations). All "coldspots" examined had qualitativelymore » low density of etching pits or very shallow tri-crystal boundary junction. EBSD revealed crystal structure surrounding the pits via crystal phase orientation mapping, while 3D profilometry gave information on the depth and size of the pits. In addition, a survey of the samples by energy dispersive X-ray analysis (EDX) did not show any significant contamination of the samples surface.« less

Electron Backscatter Diffraction (EBSD) Analysis and U-Pb Geochronology of the Oldest Lunar Zircon: Constraining Early Lunar Differentiation and Dating Impact-Related Deformation

NASA Technical Reports Server (NTRS)

Timms, Nick; Nemchin, Alexander; Grange, Marion; Reddy, Steve; Pidgeon, Bob; Geisler, Thorsten; Meyer, Chuck

2009-01-01

The evolution of the early moon was dominated by two processes (i) crystallization of the Lunar Magma Ocean (LMO) and differentiation of potassium-rare earth element-phosphorous-rich residual magma reservoir referred to as KREEP, and (ii) an intense meteorite bombardment referred to as lunar cataclysm . The exact timing of these processes is disputed, and resolution relies on collection and interpretation of precise age data. This study examines the microstructure and geochronology of zircon from lunar impact breccias collected during the Apollo 17 mission. A large zircon clast within lunar breccia 72215,195 shows sector zoning in optical microscopy, cathodoluminescence (CL) imaging and Raman mapping, and indicates that it was a relict fragment of a much larger magmatic grain. Sensitive high resolution ion microprobe (SHRIMP) U-Pb analysis of the zircon shows that U and Th concentration correlate with sector zoning, with darkest CL domains corresponding with high-U and Th (approx.150 and approx.100 ppm respectively), and the brightest-CL sectors containing approx.30-50 ppm U and approx.10-20 ppm Th. This indicates that variations in optical CL and Raman properties correspond to differential accumulation of alpha-radiation damage in each sector. Electron backscatter diffraction (EBSD) mapping shows that the quality of electron backscatter patterns (band contrast) varies with sector zoning, with the poorest quality patterns obtained from high-U and Th, dark-CL zones. EBSD mapping also reveals a deformation microstructure that is cryptic in optical, CL and Raman imaging. Two orthogonal sets of straight discrete and gradational low-angle boundaries accommodate approx.12 misorientation across the grain. The deformation bands are parallel to the crystallographic {a}-planes of the zircon, have misorientation axes parallel to the c-axis, and are geometrically consistent with formation by dislocation creep associated with <100>{010} slip. The deformation bands are unlike curved morphology of crystal-plastic microstructures in tectonically deformed terrestrial zircon, and geometrically similar to dislocation microstructures reported in experimentally shocked zircon. We interpret these crystal-plastic deformation microstructures to have resulted from a significant impact, either directly from impact shock, or during ductile flow directly following the impact. The deformation bands appear to continue undeflected through the non-indexed, radiation-damaged areas of the grain, which suggests that the orientation variation predates any significant mechanical weakening from radiation damage in the grain, and therefore occurred early in its history.

EBSD as a tool to identify and quantify bainite and ferrite in low-alloyed Al-TRIP steels.

PubMed

Zaefferer, S; Romano, P; Friedel, F

2008-06-01

Bainite is thought to play an important role for the chemical and mechanical stabilization of metastable austenite in low-alloyed TRIP steels. Therefore, in order to understand and improve the material properties, it is important to locate and quantify the bainitic phase. To this aim, electron backscatter diffraction-based orientation microscopy has been employed. The main difficulty herewith is to distinguish bainitic ferrite from ferrite because both have bcc crystal structure. The most important difference between them is the occurrence of transformation induced geometrically necessary dislocations in the bainitic phase. To determine the areas with larger geometrically necessary dislocation density, the following orientation microscopy maps were explored: pattern quality maps, grain reference orientation deviation maps and kernel average misorientation maps. We show that only the latter allow a reliable separation of the bainitic and ferritic phase. The kernel average misorientation threshold value that separates both constituents is determined by an algorithm that searches for the smoothness of the boundaries between them.

Characterization of Ultra-fine Grained and Nanocrystalline Materials Using Transmission Kikuchi Diffraction

PubMed Central

Proust, Gwénaëlle; Trimby, Patrick; Piazolo, Sandra; Retraint, Delphine

2017-01-01

One of the challenges in microstructure analysis nowadays resides in the reliable and accurate characterization of ultra-fine grained (UFG) and nanocrystalline materials. The traditional techniques associated with scanning electron microscopy (SEM), such as electron backscatter diffraction (EBSD), do not possess the required spatial resolution due to the large interaction volume between the electrons from the beam and the atoms of the material. Transmission electron microscopy (TEM) has the required spatial resolution. However, due to a lack of automation in the analysis system, the rate of data acquisition is slow which limits the area of the specimen that can be characterized. This paper presents a new characterization technique, Transmission Kikuchi Diffraction (TKD), which enables the analysis of the microstructure of UFG and nanocrystalline materials using an SEM equipped with a standard EBSD system. The spatial resolution of this technique can reach 2 nm. This technique can be applied to a large range of materials that would be difficult to analyze using traditional EBSD. After presenting the experimental set up and describing the different steps necessary to realize a TKD analysis, examples of its use on metal alloys and minerals are shown to illustrate the resolution of the technique and its flexibility in term of material to be characterized. PMID:28447998

Characterization of Ultra-fine Grained and Nanocrystalline Materials Using Transmission Kikuchi Diffraction.

PubMed

Proust, Gwénaëlle; Trimby, Patrick; Piazolo, Sandra; Retraint, Delphine

2017-04-01

One of the challenges in microstructure analysis nowadays resides in the reliable and accurate characterization of ultra-fine grained (UFG) and nanocrystalline materials. The traditional techniques associated with scanning electron microscopy (SEM), such as electron backscatter diffraction (EBSD), do not possess the required spatial resolution due to the large interaction volume between the electrons from the beam and the atoms of the material. Transmission electron microscopy (TEM) has the required spatial resolution. However, due to a lack of automation in the analysis system, the rate of data acquisition is slow which limits the area of the specimen that can be characterized. This paper presents a new characterization technique, Transmission Kikuchi Diffraction (TKD), which enables the analysis of the microstructure of UFG and nanocrystalline materials using an SEM equipped with a standard EBSD system. The spatial resolution of this technique can reach 2 nm. This technique can be applied to a large range of materials that would be difficult to analyze using traditional EBSD. After presenting the experimental set up and describing the different steps necessary to realize a TKD analysis, examples of its use on metal alloys and minerals are shown to illustrate the resolution of the technique and its flexibility in term of material to be characterized.

Observations on the Role of Hydrogen in Facet Formation in Near-alpha Titanium (Preprint)

DTIC Science & Technology

2011-05-01

using quantitative tilt fractography and electron backscatter diffraction while facet topography was examined using ultra high resolution scanning...quantitative tilt fractography and electron backscatter diffraction while facet topography was examined using ultra high resolution scanning electron...tilt fractography / electron backscatter diffraction (EBSD) technique in which both the crystallographic orientation of the fractured grain and the

Deformation and spallation of a magnesium alloy under high strain rate loading

DOE Office of Scientific and Technical Information (OSTI.GOV)

Wang, M.; Lu, L.; Li, C.

2016-04-01

We investigate deformation and damage of a magnesium alloy, AZ91, under high strain rate (similar to 10(5) s(-1)) loading via planar impact. The soft-recovered specimens are examined with electron back-scatter diffraction (EBSD). EBSD analysis reveals three types of twinning: {1012} extension, {10 (1) over bar1} contraction, and {10 (1) over bar1}-{10 (1) over bar2) double twinning, and their number density increases with increasing impact velocity. The extension twins dominate contraction and double twins in size and number. Dislocation densities of the recovered specimens are evaluated with x-ray diffraction, and increase with increasing impact velocity. X-ray tomography is used to resolvemore » three-dimensional microstructure of shock-recovered samples. The EBSD and tomography results demonstrate that the second phase, Mg17Al12, plays an important role in both deformation twinning and tensile cracking. Deformation twinning appears to be a common mechanism in deformation of magnesium alloys at low, medium and high strain rates, in addition to dislocation motion. (C) 2016 Elsevier B.V. All rights reserved.« less

An automated method of quantifying ferrite microstructures using electron backscatter diffraction (EBSD) data.

PubMed

Shrestha, Sachin L; Breen, Andrew J; Trimby, Patrick; Proust, Gwénaëlle; Ringer, Simon P; Cairney, Julie M

2014-02-01

The identification and quantification of the different ferrite microconstituents in steels has long been a major challenge for metallurgists. Manual point counting from images obtained by optical and scanning electron microscopy (SEM) is commonly used for this purpose. While classification systems exist, the complexity of steel microstructures means that identifying and quantifying these phases is still a great challenge. Moreover, point counting is extremely tedious, time consuming, and subject to operator bias. This paper presents a new automated identification and quantification technique for the characterisation of complex ferrite microstructures by electron backscatter diffraction (EBSD). This technique takes advantage of the fact that different classes of ferrite exhibit preferential grain boundary misorientations, aspect ratios and mean misorientation, all of which can be detected using current EBSD software. These characteristics are set as criteria for identification and linked to grain size to determine the area fractions. The results of this method were evaluated by comparing the new automated technique with point counting results. The technique could easily be applied to a range of other steel microstructures. © 2013 Published by Elsevier B.V.

Microstructural and microtextural characterization of oxide scale on steel using electron backscatter diffraction.

PubMed

Birosca, S; Dingley, D; Higginson, R L

2004-03-01

High-temperature oxidation of steel has been extensively studied. The microstructure of iron oxides is, however, not well understood because of the difficulty in imaging it using conventional methods, such as optical or electron microscopy. A knowledge of the oxide microstructure and texture is critical in understanding how the oxide film behaves during high-temperature deformation of steels and more importantly how it can be removed following processing. Recently, electron back-scatter diffraction (EBSD) has proved to be a powerful technique for distinguishing the different phases in scales. This technique gives valuable information both on the microstructure and on the orientation relationships between the steel and the scale layers. In the current study EBSD has been used to investigate the microstructure and microtexture of iron oxide layers grown on interstitial free steel at different times and temperatures. Heat treatments have been carried out under normal oxidation conditions in order to relate the results to real steel manufacturing in industry. The composition, morphologies, microstructure and microtexture of selected conditions have been studied using EBSD.

Phase structures and morphologies of tempered CA6NM stainless steel welded by hybrid laser-arc process

DOE Office of Scientific and Technical Information (OSTI.GOV)

Mirakhorli, F., E-mail: Fatemeh.mirakhorli.1@ens.e

The post-weld tempered microstructure of hybrid laser-arc welded CA6NM, a cast low carbon martensitic stainless steel, was investigated. The microstructural evolutions from the fusion zone to the base metal were characterized in detail using optical microscopy, scanning electron microscopy (SEM), electron backscatter diffraction (EBSD), X-ray diffraction (XRD) and microhardness techniques. The fusion zone, in its post-weld tempered condition, consisted of tempered lath martensite, residual delta-ferrite with various morphologies, reversed austenite and chromium carbides. The reversed austenite, which can be detected through both EBSD and XRD techniques, was found to be finely dispersed along the martensite lath boundaries, particularly at triplemore » junctions. Based on the EBSD analysis, the orientation relationship between the reversed austenite and the adjacent martensite laths seemed to follow the Kurdjumov-Sachs (K-S) model. The results also revealed the presence of the reversed austenite in the different regions of the heat affected zone after post-weld tempering. The microindentation hardness distribution was measured, and correlated to the evolution of the corresponding microstructure across the welds. - Highlights: •The EBSD analysis was performed on hybrid laser-arc welded CA6NM. •The FZ consisted of tempered lath martensite, reversed austenite, carbides and δ ferrite after tempering. •The reversed γ was formed along the α′ lath boundaries, particularly at triple junctions.« less

DOE Office of Scientific and Technical Information (OSTI.GOV)

Chang, Y.L.; Chen, P.Y.; Tsai, Y.T.

The crystallography of lenticular martensite, which formed in coarse austenite grains (size about 80 μm) after subzero treatment at − 196 °C (liquid nitrogen) for different holding times, was investigated using electron backscatter diffraction (EBSD). For the sample treated with 15 min of isothermal holding, more than 50 martensite plates (with a thickness of larger than 1 μm) that formed within a coarse austenite grain were employed to obtain the pole figures. The pole figures clearly indicated that the individual plate of lenticular martensite approximately adopted the Kurdjumov–Sachs (K–S) orientation relationship with respect to the austenite matrix. For the samplemore » treated with 30 s of isothermal holding, a few martensite plates that formed in variant pairings in a coarse austenite grain were analyzed. The results showed that zigzag couplings (including spear couplings), the major product of plate martensite, had an absolute dominance of a specific variant pair (V1/V17). The orientation gradient within a lenticular martensite plate was also measured using convergent beam electron diffraction (CBED). The evidence strongly suggests that the spread in diffracted intensity within pole figures is related to the misorientation gradient within the lenticular martensite plate. - Highlights: • The orientation relationship between lenticular martensite and austenite was investigated by pole figures via Electron Backscatter Diffraction (EBSD). • The initial stage of lenticular martensite formation was investigated, excluding interference from hard impingement. • In addition to EBSD, convergent beam electron diffraction (CBED) was used to measure the misorientation angle from the midrib to the untwinned region in lenticular martensite plate. • Zigzag couplings (including spear couplings), the major product of plate martensite, had an absolute dominance of a specific variant pair (V1/V17).« less

Backscattered Diffraction | Materials Science | NREL

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crystalline orientation (left) and grain distribution (right). EBSD images showing properties of crystalline investigate misorientation between grain boundaries, texture, grain distribution, deformation, strain, and

The Weighted Burgers Vector: a new quantity for constraining dislocation densities and types using electron backscatter diffraction on 2D sections through crystalline materials.

PubMed

Wheeler, J; Mariani, E; Piazolo, S; Prior, D J; Trimby, P; Drury, M R

2009-03-01

The Weighted Burgers Vector (WBV) is defined here as the sum, over all types of dislocations, of [(density of intersections of dislocation lines with a map) x (Burgers vector)]. Here we show that it can be calculated, for any crystal system, solely from orientation gradients in a map view, unlike the full dislocation density tensor, which requires gradients in the third dimension. No assumption is made about gradients in the third dimension and they may be non-zero. The only assumption involved is that elastic strains are small so the lattice distortion is entirely due to dislocations. Orientation gradients can be estimated from gridded orientation measurements obtained by EBSD mapping, so the WBV can be calculated as a vector field on an EBSD map. The magnitude of the WBV gives a lower bound on the magnitude of the dislocation density tensor when that magnitude is defined in a coordinate invariant way. The direction of the WBV can constrain the types of Burgers vectors of geometrically necessary dislocations present in the microstructure, most clearly when it is broken down in terms of lattice vectors. The WBV has three advantages over other measures of local lattice distortion: it is a vector and hence carries more information than a scalar quantity, it has an explicit mathematical link to the individual Burgers vectors of dislocations and, since it is derived via tensor calculus, it is not dependent on the map coordinate system. If a sub-grain wall is included in the WBV calculation, the magnitude of the WBV becomes dependent on the step size but its direction still carries information on the Burgers vectors in the wall. The net Burgers vector content of dislocations intersecting an area of a map can be simply calculated by an integration round the edge of that area, a method which is fast and complements point-by-point WBV calculations.

Influence of Heat Treatments on Microstructure and Magnetic Domains in Duplex Stainless Steel S31803

NASA Astrophysics Data System (ADS)

Dille, Jean; Pacheco, Clara Johanna; Camerini, Cesar Giron; Malet, Loic Charles; Nysten, Bernard; Pereira, Gabriela Ribeiro; De Almeida, Luiz Henrique; Alcoforado Rebello, João Marcos

2018-06-01

The influence of heat treatments on microstructure and magnetic domains in duplex stainless steel S31803 is studied using an innovative structural characterization protocol. Electron backscatter diffraction (EBSD) maps as well as magnetic force microscopy (MFM) images acquired on the same region of the sample, before and after heat treatment, are compared. The influence of heat treatments on the phase volumetric fractions is studied, and several structural modifications after heat treatment are highlighted. Three different mechanisms for the decomposition of ferrite into sigma phase and secondary austenite are observed during annealing at 800 °C. MFM analysis reveals that a variety of magnetic domain patterns can exist in one ferrite grain.

HR-EBSD as a new tool for quantifying geometrically necessary dislocations in quartz: Application to chessboard subgrain boundaries

NASA Astrophysics Data System (ADS)

Wallis, D.; Parsons, A. J.; Hansen, L. N.

2017-12-01

Chessboard subgrains in quartz, with boundaries composed of {m}[c] edge dislocations, are widely used as evidence for high-temperature deformation and have been suggested to form only in β-quartz. However, the origins and dislocation structure of chessboard subgrains remain poorly constrained and, without precise constraints on axes of misorientations across subgrain boundaries, other subgrain types formed at lower temperatures can be misidentified as chessboard subgrains. The technique most commonly employed to investigate subgrain structures, electron backscatter diffraction, can only resolve misorientation angles and axes for a portion of the substructure. This limitation hinders detailed interpretation of the dislocation types, densities, and processes that generate characteristic subgrain structures. We overcome these limitations by employing high-angular resolution electron backscatter diffraction (HR-EBSD), which employs cross-correlation of diffraction patterns to achieve angular resolution on the order of 0.01° with well-constrained misorientation axes. We analyse chessboard subgrains in samples from the Greater Himalayan Sequence, Nepal, which were deformed along well constrained pressure-temperature paths confined to the stability field of α-quartz. HR-EBSD analysis demonstrates that the subgrain boundaries consist of two sets. One set consists primarily of {m}[c] edge dislocations and the other consists of dislocations primarily with Burgers vectors. Apparent densities of geometrically necessary dislocations vary from > 1013 m-2 within some subgrain boundaries to < 1012 m-2 within subgrain interiors. This analysis provides new insight into the structure of chessboard subgrain boundaries, and a new tool to distinguish them from superficially similar deformation microstructures formed by other dislocation types at lower temperatures. Application of HR-EBSD to quartz from the Greater Himalayan Sequence confirms the activity of {m}[c] slip in the α-quartz stability field and demonstrates that formation of chessboard subgrains is not restricted to the stability field of β-quartz. Most importantly, this study demonstrates the potential of HR-EBSD as an improved method for analysis of quartz microstructures used as indicators of deformation conditions.

In-Depth View of the Structure and Growth of SnO2 Nanowires and Nanobrushes.

PubMed

Stuckert, Erin P; Geiss, Roy H; Miller, Christopher J; Fisher, Ellen R

2016-08-31

Strategic application of an array of complementary imaging and diffraction techniques is critical to determine accurate structural information on nanomaterials, especially when also seeking to elucidate structure-property relationships and their effects on gas sensors. In this work, SnO2 nanowires and nanobrushes grown via chemical vapor deposition (CVD) displayed the same tetragonal SnO2 structure as revealed via powder X-ray diffraction bulk crystallinity data. Additional characterization using a range of electron microscopy imaging and diffraction techniques, however, revealed important structure and morphology distinctions between the nanomaterials. Tailoring scanning transmission electron microscopy (STEM) modes combined with transmission electron backscatter diffraction (t-EBSD) techniques afforded a more detailed view of the SnO2 nanostructures. Indeed, upon deeper analysis of individual wires and brushes, we discovered that, despite a similar bulk structure, wires and brushes grew with different crystal faces and lattice spacings. Had we not utilized multiple STEM diffraction modes in conjunction with t-EBSD, differences in orientation related to bristle density would have been overlooked. Thus, it is only through a methodical combination of several structural analysis techniques that precise structural information can be reliably obtained.

Textural and chemical evolution of pyroxene during hydration and deformation: A consequence of retrograde metamorphism

NASA Astrophysics Data System (ADS)

Centrella, Stephen; Putnis, Andrew; Lanari, Pierre; Austrheim, Håkon

2018-01-01

Centimetre-sized grains of Al-rich clinopyroxene within the granulitic anorthosites of the Bergen Arcs, W-Norway undergo deformation by faults and micro-shear zones (kinks) along which fluid has been introduced. The clinopyroxene (11 wt% Al2O3) reacts to the deformation and hydration in two different ways: reaction to garnet (Alm41Prp32Grs21) plus a less aluminous pyroxene (3 wt% Al2O3) along kinks and the replacement of the Al-rich clinopyroxene by chlorite along cleavage planes. These reactions only take place in the hydrated part of a hand specimen that is separated from dry, unreacted granulite by a sharp interface that defines the limit of hydration. We use electron probe microanalysis (EPMA) and X-Ray mapping together with electron backscatter diffraction (EBSD) mapping to investigate the spatial and possible temporal relationships between these two parageneses. Gresens' analysis (Gresens, 1967) has been used to determine the mass balance and the local volume changes associated with the two reactions. The reaction to garnet + low-Al clinopyroxene induces a loss in volume of the solid phases whereas the chlorite formation gains volume. Strain variations result in local variation in undulose extinction in the parent clinopyroxene. EBSD results suggest that the density-increasing reaction to garnet + low-Al clinopyroxene takes place where the strain is highest whereas the density-decreasing reaction to chlorite forms away from shear zones where EBSD shows no significant strain. Modelling of phase equilibria suggest that the thermodynamic pressure of the assemblage within the shear zones is > 6 kbar higher than the pressure conditions for the whole rock for the same range of temperature ( 650 °C). This result suggests that the stress redistribution within a rock may play a role in determining the reactions that take place during retrograde metamorphism.

Microshear in the deep EDML ice core analyzed using cryogenic EBSD

NASA Astrophysics Data System (ADS)

Kuiper, Ernst-Jan; Pennock, Gill; Drury, Martyn; Kipfstuhl, Sepp; Faria, Sérgio; Weikusat, Ilka

2017-04-01

Ice sheets play an important role in sea level evolution by storing large amounts of fresh water on land. The ice in an ice sheet flows from the interior of the ice sheet to the edges where it either melts or calves into the ocean. This flow of ice results from internal deformation of the ice aggregate. Dislocation creep is assumed to be the dominant deformation mechanism for polar ice and is grain size insensitive. Recently, a different deformation mechanism was identified in the deeper part of the EDML ice core (Antarctica) where, at a depth of 2385 meters, the grain size strongly decreases, the grain aspect ratio increase and, the inclination of the grain elongation changes (Faria et al., 2006; Weikusat et al., 2017). At this depth the borehole displacement increases strongly (Weikusat et al., 2017), which indicates a relatively high strain rate. Part of this EDML ice core section was studied using cryogenic electron backscattered diffraction (cryo-EBSD) (Weikusat et al, 2011). EBSD produces high resolution, full crystallographic (a-axis and c-axis) maps of the ice core samples. EBSD samples were taken from an ice core section at 2392.2 meter depth. This section was chosen for its very small grain size and the strongly aligned grain boundaries. The EBSD maps show a very low orientation gradient of <0.3° per millimetre inside the grains, which is 5-10 times lower than the orientation gradients found in other parts of the ice core. Furthermore, close to some grain boundaries, a relatively strong orientation gradient of 1°-2° per millimetre was found. The subgrain boundaries developed such that they elongate the sliding boundaries in order to accommodate the incompatibilities and maintain the strongly aligned grain boundary network. We identify the dominant deformation mechanism in this part of the ice core as grain boundary sliding accommodated by localized dislocation creep, which is a process similar to microshear (Drury and Humpreys, 1988). The existence of layers of soft ice has serious implications for ice core dating, related paleoclimate studies and ice flow modelling with respect to ice sheet mass balance and sea level predictions. References: - Drury and Humphreys, 1988. Microstructural shear criteria associated with grain boundary sliding during ductile deformation. J. of Struc. Geol. 10, 1, 83-89. - Faria et al., 2006. Is Antarctica like a birthday cake?, Max Planck Institute of Mathematics and the Sciences - Weikusat et al., 2011. Cryogenic EBSD on ice: preserving a stable surface in a low pressure SEM. J. Micros. 242, 3, 295-310. (doi: 10.1111/j.1365-2818.2010.03471.x) - Weikusat et al., 2017. Physical analysis of an Antarctic ice core-towards an integration of micro- and macrodynamics of polar ice. Phil. Trans. R. Soc. A 375, 2015347. (doi:10.1098/rsta.2015.0347)

Identifying Planar Deformation Features Using EBSD and FIB

NASA Astrophysics Data System (ADS)

Pickersgill, A. E.; Lee, M. R.

2015-09-01

Planar deformation features in quartz grains from the Gow Lake impact structure have been successfully identified and indexed using electron backscatter diffraction in combination with focused ion beam milling.

A novel EBSD-based finite-element wave propagation model for investigating seismic anisotropy: Application to Finero Peridotite, Ivrea-Verbano Zone, Northern Italy

NASA Astrophysics Data System (ADS)

Zhong, Xin; Frehner, Marcel; Kunze, Karsten; Zappone, Alba

2014-10-01

A novel electron backscatter diffraction (EBSD) -based finite-element (FE) wave propagation simulation is presented and applied to investigate seismic anisotropy of peridotite samples. The FE model simulates the dynamic propagation of seismic waves along any chosen direction through representative 2D EBSD sections. The numerical model allows separation of the effects of crystallographic preferred orientation (CPO) and shape preferred orientation (SPO). The obtained seismic velocities with respect to specimen orientation are compared with Voigt-Reuss-Hill estimates and with laboratory measurements. The results of these three independent methods testify that CPO is the dominant factor controlling seismic anisotropy. Fracture fillings and minor minerals like hornblende only influence the seismic anisotropy if their volume proportion is sufficiently large (up to 23%). The SPO influence is minor compared to the other factors. The presented FE model is discussed with regard to its potential in simulating seismic wave propagation using EBSD data representing natural rock petrofabrics.

Hyperspectral Imaging at the Micro- and Nanoscale using Energy-dispersive Spectroscopy (EDS) with Silicon Drift Detector (SDD) and EBSD Analysis

NASA Astrophysics Data System (ADS)

Salge, T.; Goran, D.

2010-12-01

SDD systems have become state of the art technology in the field of EDS. The main characteristic of the SDDs is their extremely high pulse load capacity of up to 750,000 counts per second at good energy resolution (<123 eV Mn-Kα, <46 eV C-Kα at 100,000 counts per seconds). These properties in conjunction with electron backscatter diffraction (EBSD) technique and modern data processing allows not only high speed mapping but also hyperspectral analysis. Here, a database is created that contains an EDS spectrum and/or EBSD pattern for each pixel of the SEM image setting the stage for innovative analysis options: The Maximum Pixel Spectrum function [1] synthesizes a spectrum out of the EDS database, consisting of the highest count level found in each spectrum channel. Here, (trace) elements which occur in only one pixel can be detected qualitatively. Areas of similar EDS composition can be made visible with Autophase, a spectroscopic phase detection system. In cases where the crystallographic phase assessment by EBSD is problematic due to pattern similarity, the EDS signal can be used as additional information for phase separation. This paper presents geoscience applications with the QUANTAX system with EDS SDD and EBSD detector using the options described above: (1) Drill core analysis of a Chicxulub impact ejecta sequence from the K/Pg boundary at ODP leg 207 [2] using fast, high resolution element maps. (2) Detection of monazite in granite by the Maximum Pixel Spectrum function. (3) Distribution of elements with overlapping peaks by deconvolution at the example of rare earth elements in zoned monazite. (4) Spectroscopic phase analysis of a sulfate-carbonate-dominated impact matrix at borehole UNAM-7 from the Chicxulub impact crater [3]. (5) EBSD studies with examples of iron meteorites and impact-induced, recrystallized carbonate melts [4]. In addition, continuing technological advances require the elemental analysis of increasingly smaller structures in many fields, including geosciences. It will be demonstrated that using low accelerating voltages, the element distribution of structures at the nanoscale in bulk samples can be displayed in a short time due to optimized signal processing and solid angle. Peaks composed of contributions from several overlapping elements e.g. N-K (392 eV) and Ti-Ll (395 eV) can be deconvolved [6] using an improved atomic database with 250 additional L, M and N lines below 4 keV. Improved light element quantification allows the standardless quantification of features at the nanoscale such as rutile grains 200-500 nm in size. References: [1] Bright D S. & Newbury D. E. (2004) Journal of Microscopy 216:186-193. [2] Schulte P. et al. (2010) Science 327: 1214-1218. [3] Salge T. (2007) PhD thesis: 130p. http://edoc.huberlin.de/docviews/abstract.php?lang=ger&id=27753. [4] Deutsch A. et al. MAPS 45: A45. [6] Tunckan O. (2010) Joining ceramics using capacitor discharge technique and determination of metal ceramic interface reactions, PhD thesis, Anadolu University, Eskisehir, Turkey. Acknowledgements: We thank P. Schulte, A. Deutsch, ODP, L. Hecht, A. Kearsley, J. Urrutria-Fucugauchi, O. Tunckan and S. Turan for generously providing the samples.

Crystallography of Magnetite Plaquettes and their Significance as Asymmetric Catalysts for the Synthesis of Chiral Organics in Carbonaceous Chondrites

NASA Technical Reports Server (NTRS)

Chan, Q. H. S.; Zolensky, M. E.

2015-01-01

We have previously observed the magnetite plaquettes in carbonaceous chondrites using scanning electron microscope (SEM) imaging, examined the crystal orientation of the polished surfaces of magnetite plaquettes in CI Orgueil using electron backscattered diffraction (EBSD) analysis, and concluded that these magnetite plaquettes are likely naturally asymmetric materials. In this study, we expanded our EBSD observation to other magnetite plaquettes in Orgueil, and further examined the internal structure of these remarkable crystals with the use of X-ray computed microtomography.

Coarsening behaviour of M23C6 carbides in creep-resistant steel exposed to high temperatures

NASA Astrophysics Data System (ADS)

Godec, M.; Skobir Balantič, D. A.

2016-07-01

High operating temperatures can have very deleterious effects on the long-term performance of high-Cr, creep-resistant steels used, for example, in the structural components of power plants. For the popular creep-resistant steel X20CrMoV12.1 we analysed the processes of carbide growth using a variety of analytical techniques: transmission electron microscopy (TEM) and diffraction (TED), scanning electron microscopy (SEM), and electron backscatter diffraction (EBSD). The evolution of the microstructure after different aging times was the basis for a much better understanding of the boundary-migration processes and the growth of the carbides. We present an explanation as to why some locations are preferential for this growth, and using EBSD we were able to define the proper orientational relationship between the carbides and the matrix.

Tackling pseudosymmetry problems in electron backscatter diffraction (EBSD) analyses of perovskite structures

NASA Astrophysics Data System (ADS)

Mariani, Elisabetta; Kaercher, Pamela; Mecklenburgh, Julian; Wheeler, John

2016-04-01

Perovskite minerals form an important mineral group that has applications in Earth science and emerging alternative energy technologies, however crystallographic quantification of these minerals with electron backscatter diffraction (EBSD) is not accurate due to pseudosymmetry problems. The silicate perovskite Bridgmanite, (Mg,Fe)SiO3, is understood to be the dominant phase in the Earth's lower mantle. Gaining insight into its physical and rheological properties is therefore vital to understand the dynamics of the Earth's deep interior. Rock deformation experiments on analogue perovskite phases, for example (Ca,Sr)TiO3, combined with quantitative microstructural analyses of the recovered samples by EBSD, yield datasets that can reveal what deformation mechanisms may dominate the flow of perovskite in the lower mantle. Additionally, perovskite structures have important technological applications as new, suitable cathodes for the operation of more efficient and environmentally-friendly solid oxide fuel cells (SOFC). In recent years they have also been recognised as a potential substitute for silicon in the next generation of photovoltaic cells for the construction of economic and energy efficient solar panels. EBSD has the potential to be a valuable tool for the study of crystal orientations achieved in perovskite substrates as crystal alignment has a direct control on the properties of these materials. However, perovskite structures currently present us with challenges during the automated indexing of Kikuchi bands in electron backscatter diffraction patterns (EBSPs). Such challenges are represented by the pseudosymmetric character of perovskites, where atoms are subtly displaced (0.005 nm to 0.05 nm) from their higher symmetry positions. In orthorhombic Pbnm perovskites, for example, pseudosymmetry may be evaluated from the c/a unit cell parameter ratio, which is very close to 1. Two main types of distortions from the higher symmetry structure are recognised: a tilt and a deformation of the anion octahedron. These distortions may occur together. Common misidentifications observed in EBSD data are [100] and [001] seen as equivalent solutions, whereby these dyad symmetry axes are misidentified as tetrad axes of the cubic symmetry. In this study we investigate methods that could be applied to the EBSP automated indexing algorithm to solve the pseudosymmetry problem in perovskite structures. Attention is given to subtle angular deviations between bands and to differences in pseudosymmetric Kikuchi patterns.

Experimental Characterization and Simulation of Slip Transfer at Grain Boundaries and Microstructurally-Sensitive Crack Propagation

NASA Technical Reports Server (NTRS)

Gupta, Vipul; Hochhalter, Jacob; Yamakov, Vesselin; Scott, Willard; Spear, Ashley; Smith, Stephen; Glaessgen, Edward

2013-01-01

A systematic study of crack tip interaction with grain boundaries is critical for improvement of multiscale modeling of microstructurally-sensitive fatigue crack propagation and for the computationally-assisted design of more durable materials. In this study, single, bi- and large-grain multi-crystal specimens of an aluminum-copper alloy are fabricated, characterized using electron backscattered diffraction (EBSD), and deformed under tensile loading and nano-indentation. 2D image correlation (IC) in an environmental scanning electron microscope (ESEM) is used to measure displacements near crack tips, grain boundaries and within grain interiors. The role of grain boundaries on slip transfer is examined using nano-indentation in combination with high-resolution EBSD. The use of detailed IC and EBSD-based experiments are discussed as they relate to crystal-plasticity finite element (CPFE) model calibration and validation.

Advances in 6d diffraction contrast tomography

NASA Astrophysics Data System (ADS)

Viganò, N.; Ludwig, W.

2018-04-01

The ability to measure 3D orientation fields and to determine grain boundary character plays a key role in understanding many material science processes, including: crack formation and propagation, grain coarsening, and corrosion processes. X-ray diffraction imaging techniques offer the ability to retrieve such information in a non-destructive manner. Among them, Diffraction Contrast Tomography (DCT) is a monochromatic beam, near-field technique, that uses an extended beam and offers fast mapping of 3D sample volumes. It was previously shown that the six-dimensional extension of DCT can be applied to moderately deformed samples (<= 5% total strain), made from materials that exhibit low levels of elastic deformation of the unit cell (<= 1%). In this article, we improved over the previously proposed 6D-DCT reconstruction method, through the introduction of both a more advanced forward model and reconstruction algorithm. The results obtained with the proposed improvements are compared against the reconstructions previously published in [1], using Electron Backscatter Diffraction (EBSD) measurements as a reference. The result was a noticeably higher quality reconstruction of the grain boundary positions and local orientation fields. The achieved reconstruction quality, together with the low acquisition times, render DCT a valuable tool for the stop-motion study of polycrystalline microstructures, evolving as a function of applied strain or thermal annealing treatments, for selected materials.

A Microstructure Study on an AZ31 Magnesium Alloy Tube after Hot Metal Gas Forming Process

NASA Astrophysics Data System (ADS)

Liu, Yi; Wu, Xin

2007-06-01

An AZ31 magnesium alloy tube has been deformed by the hot metal gas forming (HMGF) technique. Microstructures before and after deformation have been investigated by using Electron Backscattered Diffraction (EBSD) and Electron Microscopy. Due to the inhomogeneous distribution by induction heating, there is a temperature gradient distribution along the tube axis. Accordingly, the deformation mechanism is also different. In the middle area of deformation zone where the temperature is ˜410 °C, almost no twinning has been found, whereas at the edge areas of deformation zone where the temperature is ˜200 °C, a high density of twins has been found. EBSD experiments show a weak (0001) fiber texture along the radial direction of the tube before and after deformation in the high-temperature zone. EBSD experiments on the low temperature deformation region were not successful due to the high stored energy. Schmid factor analysis on the EBSD data shows that, despite the (0001) fiber texture, there are still many grains favoring basal slip along both the axis direction and hoop direction.

Electron imaging with an EBSD detector.

PubMed

Wright, Stuart I; Nowell, Matthew M; de Kloe, René; Camus, Patrick; Rampton, Travis

2015-01-01

Electron Backscatter Diffraction (EBSD) has proven to be a useful tool for characterizing the crystallographic orientation aspects of microstructures at length scales ranging from tens of nanometers to millimeters in the scanning electron microscope (SEM). With the advent of high-speed digital cameras for EBSD use, it has become practical to use the EBSD detector as an imaging device similar to a backscatter (or forward-scatter) detector. Using the EBSD detector in this manner enables images exhibiting topographic, atomic density and orientation contrast to be obtained at rates similar to slow scanning in the conventional SEM manner. The high-speed acquisition is achieved through extreme binning of the camera-enough to result in a 5 × 5 pixel pattern. At such high binning, the captured patterns are not suitable for indexing. However, no indexing is required for using the detector as an imaging device. Rather, a 5 × 5 array of images is formed by essentially using each pixel in the 5 × 5 pixel pattern as an individual scattered electron detector. The images can also be formed at traditional EBSD scanning rates by recording the image data during a scan or can also be formed through post-processing of patterns recorded at each point in the scan. Such images lend themselves to correlative analysis of image data with the usual orientation data provided by and with chemical data obtained simultaneously via X-Ray Energy Dispersive Spectroscopy (XEDS). Copyright © 2014 The Authors. Published by Elsevier B.V. All rights reserved.

An EBSD Evaluation of the Microstructure of Crept Nimonic 101 for the Validation of a Polycrystal-Plasticity Model

NASA Astrophysics Data System (ADS)

Reschka, S.; Munk, L.; Wriggers, P.; Maier, H. J.

2017-12-01

Nimonic 101 is one of the early nickel-based superalloys developed for the use in gas turbines. In such environments, the material is exposed to a combination of both high temperatures and mechanical loads for a long duration. Hence, thermal creep is of the utmost concern as it often limits service life. This study focuses on creep tests, carried out on Nimonic 101 at different temperatures under a constant tensile load of 735 MPa. To characterize the microstructural evolution, electron backscatter diffraction (EBSD) measurements were employed before and after loading. At higher temperatures, a significant change of the microstructure was observed. The grains elongated and aligned their orientation along the load axis. In parallel, a crystal plasticity material model has been set up in the classical large deformation framework. Modeling results are compared to the acquired EBSD data.

Testing the Crystalline Integrity of Baddeleyite: A Systematic EBSD and Confocal Laser-Raman Spectroscopy Study

NASA Astrophysics Data System (ADS)

DesOrmeau, J. W.; Ibanez-Mejia, M.; Lafuente Valverde, B.; Eddy, M. P.; Trail, D.; Wang, Y.

2017-12-01

The accessory mineral baddeleyite (monoclinic ZrO2) has great potential as a high-precision U-Pb geochronometer in silica-undersaturated rocks. However, due to a lack of understanding of alpha-recoil damage to the crystal structure and the influences on chemical diffusion properties and closed-system behavior, limitations still exist. Studies have shown phase transformations in baddeleyite (monoclinic to tetragonal) resulting from radiation damage due to ion bombardment [e.g., 1], but the effects of self-irradiation on the baddeleyite crystal structure over geologic timescales remain poorly understood. A recent study reported confocal laser-Raman spectra suggesting the presence of a tetragonal phase in a Phalaborwa baddeleyite [2], which has crucial implications for Pb mobility and high-precision U-Pb results. To better understand the physical effects of self-irradiation in baddeleyite over geologic timescales, samples of various ages (ca. 2060-32 Ma) and calculated alpha-doses (0.001-0.901 x 1016 α/mg) were imaged by cathodoluminescence (CL) and subsequently analyzed via electron backscatter diffraction (EBSD) and confocal laser-Raman spectroscopy. Synthetic baddeleyite grown in a one-atmosphere furnace was also analyzed to allow a comparison of EBSD and Raman results of the pure monoclinic phase and the natural unknown samples. Whole grain EBSD maps (n=75) of baddeleyite from the Phalabowra and Kovdor carbonatites, the Ammänpelto sill, and the Duluth, Ogden and Yinmawanshan gabbros show complex twinning that is loosely correlated to CL zoning and identification of the monoclinic phase only, suggesting no evidence for phase transformations within grains of contrasting age and amounts of alpha-doses. Preliminary Raman results show evidence of systematic shifts in the vibrational modes of Phalabowra baddeleyite with respect to the younger crystals, which may be the result of radiation-induced damage accumulation rather than phase transformation. These results aim to better characterize the poorly known effects of radiation damage in natural baddeleyite and assist in improving methods for high-precision U-Pb dating of mafic systems on Earth and other planetary bodies. [1] Valdez et al. (2008), J. Nucl. Mater. 381, pp. 259-266. [2[ Schaltegger and Davies (2017), RIMG 83, pp.297-328.

A new barometer from stress fields around inclusions

NASA Astrophysics Data System (ADS)

Avadanii, Diana; Hansen, Lars; Wallis, David; Waters, David

2017-04-01

A key step in understanding geological and geodynamic processes is modelling the pressure-temperature paths of metamorphic rocks. Traditional thermobarometry relies on mineral assemblage equilibria and thermodynamic modelling to infer the pressures and temperatures of chemical equilibration. This approach requires the presence of specific mineral assemblages and compositions, which narrows its applicability. In this study we aim to develop a geobarometer based on mechanical interactions between inclusions and their host grains. Exhumation of minerals with inclusions causes heterogeneous residual stress fields due to the different, and often anisotropic, elastic properties of the inclusion and host. Recent studies measure residual mean stresses within inclusions using Raman spectroscopy and use those stresses as a barometer. In contrast, we map each component of the stress tensor around inclusions using high angular-resolution electron backscatter diffraction (HR-EBSD). This technique provides both higher spatial resolution and increased sensitivity to elastic strains relative to Raman spectroscopy. We focus on quartz inclusions in garnet, a common feature in metamorphic rocks. This assemblage also provides an opportunity to test our results with compositional thermobarometry. We analyse samples metamorphosed at pressures ranging from ˜ 300 MPa to ˜ 1600 MPa, as recorded by independent geobarometers. HR-EBSD reveals symmetric and lobate signals around inclusions, with elastic strains and residual stresses of the order 10-3 and ±102 -103 MPa, respectively. We solve Eshelby's problem for the 'inhomogeneous inclusion' case to simulate the elastic strain/stress field around an anisotropic ellipsoidal inclusion surrounded by an isotropic, homogeneous, infinite matrix. This model calculates the stress disturbances caused by differential expansion of an inclusion and host subjected to decompression. We additionally account for differential expansion related to cooling by imposing an eigenstrain in the inclusion, according to the thermal expansivity of quartz. Thermal contraction in the host garnet is accounted for by modifying the macroscopic pressure. The simulations reproduce the general pattern of the elastic fields that we observe from HR-EBSD and account for different geometries of the inclusion. The simulations provide the basis for quantitatively relating the stress fields measured by HR-EBSD to the entrapment pressures of inclusions.

Investigation of Parent Austenite Grains from Martensite Structure Using EBSD in a Wear Resistant Steel

PubMed Central

Gyhlesten Back, Jessica; Engberg, Göran

2017-01-01

Crystallographic reconstruction of parent austenite grain boundaries from the martensitic microstructure in a wear resistant steel was carried out using electron backscattered diffraction (EBSD). The present study mainly aims to investigate the parent austenite grains from the martensitic structure in an as-rolled (reference) steel sample and samples obtained by quenching at different cooling rates with corresponding dilatometry. Subsequently, this study is to correlate the nearest cooling rate by the dilatometer which yields a similar orientation relationship and substructure as the reference sample. The Kurdjumov-Sachs orientation relationship was used to reconstruct the parent austenite grain boundaries from the martensite boundaries in both reference and dilatometric samples using EBSD crystallographic data. The parent austenite grain boundaries were successfully evaluated from the EBSD data and the corresponding grain sizes were measured. The parent austenite grain boundaries of the reference sample match the sample quenched at 100 °C/s (CR100). Also the martensite substructures and crystallographic textures are similar in these two samples. The results from hardness measurements show that the reference sample exhibits higher hardness than the CR100 sample due to the presence of carbides in the reference sample. PMID:28772813

Investigation of Parent Austenite Grains from Martensite Structure Using EBSD in a Wear Resistant Steel.

PubMed

Gyhlesten Back, Jessica; Engberg, Göran

2017-04-26

Crystallographic reconstruction of parent austenite grain boundaries from the martensitic microstructure in a wear resistant steel was carried out using electron backscattered diffraction (EBSD). The present study mainly aims to investigate the parent austenite grains from the martensitic structure in an as-rolled (reference) steel sample and samples obtained by quenching at different cooling rates with corresponding dilatometry. Subsequently, this study is to correlate the nearest cooling rate by the dilatometer which yields a similar orientation relationship and substructure as the reference sample. The Kurdjumov-Sachs orientation relationship was used to reconstruct the parent austenite grain boundaries from the martensite boundaries in both reference and dilatometric samples using EBSD crystallographic data. The parent austenite grain boundaries were successfully evaluated from the EBSD data and the corresponding grain sizes were measured. The parent austenite grain boundaries of the reference sample match the sample quenched at 100 °C/s (CR100). Also the martensite substructures and crystallographic textures are similar in these two samples. The results from hardness measurements show that the reference sample exhibits higher hardness than the CR100 sample due to the presence of carbides in the reference sample.

Raman spectroscopy as a tool to characterize heterogenite (CoO·OH) (Katanga Province, Democratic Republic of Congo)

NASA Astrophysics Data System (ADS)

Burlet, C.; Vanbrabant, Y.; Goethals, H.; Thys, T.; Dupin, L.

2011-10-01

Natural heterogenite (CoO·OH) samples were studied by Raman microspectroscopy, electronic microprobe and Electronic BackScattered Diffraction (EBSD). Raw samples and polished sections were made from 10 mines covering the Katanga copperbelt (Katanga Province, Democratic Republic of Congo). Four typical Raman responses have been obtained leading to investigate the laser-induced dehydroxylation of heterogenite into a Co-spinel structure. The results are also compared with EBSD patterns from oven heated heterogenite samples. A close relationship was established between the chemical substitutions of Co by mainly Cu, Ni, Mn and Al and their impact on the mineral Raman response.

EBSD and Nanoindentation-Correlated Study of Delamination Fracture in Al-Li Alloy 2090

NASA Technical Reports Server (NTRS)

Tayon, Wesley A.; Crooks, Roy E.; Domack, Marcia S.; Wagner, John A.; Elmustafa, A. A.

2008-01-01

Al-Li alloys offer attractive combinations of high strength and low density. However, a tendency for delamination fracture has limited their use. A better understanding of the delamination mechanisms may identify methods to control delaminations through processing modifications. A combination of new techniques has been used to evaluate delamination fracture in Al-Li alloys. Both high quality electron backscattered diffraction (EBSD) information and valid nanoindentation measurements were obtained from fractured test specimens. Correlations were drawn between nano-scale hardness variations and local texture along delaminating boundaries. Intriguing findings were observed for delamination fracture through the combined analysis of grain orientation, Taylor factor, and kernel average misorientation.

Stress Corrosion Cracking Facet Crystallography of Ti-8Al-1Mo-1V (Preprint)

DTIC Science & Technology

2011-05-01

fractography and electron backscatter diffraction. The results indicate that most facets are formed nearly perpendicular to the loading direction on...of Ti-8Al- 1Mo-1V have been characterized using quantitative fractography and electron backscatter diffraction. The results indicate that most facets...EBSD and quantitative tilt fractography [27;29] allow for determination of the crystallographic fracture plane to an accuracy between 1o [29] and

Ion-damage-free planarization or shallow angle sectioning of solar cells for mapping grain orientation and nanoscale photovoltaic properties

DOE PAGES

Kutes, Yasemin; Luria, Justin; Sun, Yu; ...

2017-04-11

Ion beam milling is the most common modern method for preparing specific features for microscopic analysis, even though concomitant ion implantation and amorphization remain persistent challenges, particularly as they often modify materials properties of interest. Atomic force microscopy (AFM), on the other hand, can mechanically mill specific nanoscale regions in plan-view without chemical or high energy ion damage, due to its resolution, directionality, and fine load control. As an example, AFM-nanomilling (AFM-NM) is implemented for top-down planarization of polycrystalline CdTe thin film solar cells, with a resulting decrease in the root mean square (RMS) roughness by an order of magnitude,more » even better than for a low incidence FIB polished surface. Subsequently AFM-based property maps reveal a substantially stronger contrast, in this case of the short-circuit current or open circuit voltage during light exposure. Furthermore, electron back scattering diffraction (EBSD) imaging also becomes possible upon AFM-NM, enabling direct correlations between the local materials properties and the polycrystalline microstructure. Smooth shallow-angle cross-sections are demonstrated as well, based on targeted oblique milling. As expected, this reveals a gradual decrease in the average short-circuit current and maximum power as the underlying CdS and electrode layers are approached, but a relatively consistent open-circuit voltage through the diminishing thickness of the CdTe absorber. AFM-based nanomilling is therefore a powerful tool for material characterization, uniquely providing ion-damage free, selective area, planar smoothing or low-angle sectioning of specimens while preserving their functionality. This then enables novel, co-located advanced AFM measurements, EBSD analysis, and investigations by related techniques that are otherwise hindered by surface morphology or surface damage.« less

Deformation microstructures and magnetite texture development in synthetic shear zones

NASA Astrophysics Data System (ADS)

Till, Jessica L.; Moskowitz, Bruce M.

2014-08-01

We present observations of deformation features in magnetite from synthetic magnetite-bearing silicate aggregates deformed between 1000 °C and 1200 °C in transpressional shear experiments with strains of up to 300%. Anisotropy of magnetic susceptibility and shape preferred orientation (SPO) analysis were combined with electron backscatter diffraction (EBSD) to characterize the magnetite deformation fabrics and intragrain microstructures. Crystallographic preferred orientation (CPO) in magnetite is very weak in all deformed samples and does not vary as a function of either temperature or shear strain. Magnetic anisotropy and SPO increase strongly with both strain and deformation temperature and indicate that strain partitioning between magnetite and the plagioclase matrix decreases at higher temperatures. EBSD orientation mapping of individual magnetite particles revealed substantial dispersions in intragrain orientation, analogous to undulose extinction, after deformation at 1000 and 1100 °C, indicating that dislocation creep processes were active in magnetite despite the lack of a well-developed CPO. Geometrical analysis of crystallographic orientation dispersions from grain map data indicates that low-angle grain boundary formation in magnetite could have been accommodated by slip on {110} or {100} planes, but no evidence for dominant slip on the expected {111} planes was found. Evidence for activation of multiple slip systems was seen in some magnetite grains and could be partially responsible for the lack of CPO in magnetite. These results suggest that, at least in polyphase rocks, crystallographic textures in magnetite may be inherently weak or slow to develop and CPO alone is not an adequate indicator of magnetite deformation mechanisms. These results may aid in the interpretation of deformation textures in other spinel-structured phases such as chromite and ringwoodite.

Ion-damage-free planarization or shallow angle sectioning of solar cells for mapping grain orientation and nanoscale photovoltaic properties

NASA Astrophysics Data System (ADS)

Kutes, Yasemin; Luria, Justin; Sun, Yu; Moore, Andrew; Aguirre, Brandon A.; Cruz-Campa, Jose L.; Aindow, Mark; Zubia, David; Huey, Bryan D.

2017-05-01

Ion beam milling is the most common modern method for preparing specific features for microscopic analysis, even though concomitant ion implantation and amorphization remain persistent challenges, particularly as they often modify materials properties of interest. Atomic force microscopy (AFM), on the other hand, can mechanically mill specific nanoscale regions in plan-view without chemical or high energy ion damage, due to its resolution, directionality, and fine load control. As an example, AFM-nanomilling (AFM-NM) is implemented for top-down planarization of polycrystalline CdTe thin film solar cells, with a resulting decrease in the root mean square (RMS) roughness by an order of magnitude, even better than for a low incidence FIB polished surface. Subsequent AFM-based property maps reveal a substantially stronger contrast, in this case of the short-circuit current or open circuit voltage during light exposure. Electron back scattering diffraction (EBSD) imaging also becomes possible upon AFM-NM, enabling direct correlations between the local materials properties and the polycrystalline microstructure. Smooth shallow-angle cross-sections are demonstrated as well, based on targeted oblique milling. As expected, this reveals a gradual decrease in the average short-circuit current and maximum power as the underlying CdS and electrode layers are approached, but a relatively consistent open-circuit voltage through the diminishing thickness of the CdTe absorber. AFM-based nanomilling is therefore a powerful tool for material characterization, uniquely providing ion-damage free, selective area, planar smoothing or low-angle sectioning of specimens while preserving their functionality. This enables novel, co-located advanced AFM measurements, EBSD analysis, and investigations by related techniques that are otherwise hindered by surface morphology or surface damage.

Microstructural evolution during thermal annealing of ice-Ih

NASA Astrophysics Data System (ADS)

Hidas, Károly; Tommasi, Andréa; Mainprice, David; Chauve, Thomas; Barou, Fabrice; Montagnat, Maurine

2017-06-01

We studied the evolution of the microstructure of ice-Ih during static recrystallization by stepwise annealing experiments. We alternated thermal annealing and electron backscatter diffraction (EBSD) analyses on polycrystalline columnar ice pre-deformed in uniaxial compression at temperature of -7 °C to macroscopic strains of 3.0-5.2. Annealing experiments were carried out at -5 °C and -2 °C up to a maximum of 3.25 days, typically in 5-6 steps. EBSD crystal orientation maps obtained after each annealing step permit the description of microstructural changes. Decrease in average intragranular misorientation at the sample scale and modification of the misorientation across subgrain boundaries provide evidence for recovery from the earliest stages of annealing. This initial evolution is similar for all studied samples irrespective of their initial strain or annealing temperature. After an incubation period ≥1.5 h, recovery is accompanied by recrystallization (nucleation and grain boundary migration). Grain growth proceeds at the expense of domains with high intragranular misorientations, consuming first the most misorientated parts of primary grains. Grain growth kinetics fits the parabolic growth law with grain growth exponents in the range of 2.4-4.0. Deformation-induced tilt boundaries and kink bands may slow down grain boundary migration. They are stable features during early stages of static recrystallization, only erased by normal growth, which starts after >24 h of annealing.

3-D microstructure of olivine in complex geological materials reconstructed by correlative X-ray μ-CT and EBSD analyses.

PubMed

Kahl, W-A; Dilissen, N; Hidas, K; Garrido, C J; López-Sánchez-Vizcaíno, V; Román-Alpiste, M J

2017-11-01

We reconstruct the 3-D microstructure of centimetre-sized olivine crystals in rocks from the Almirez ultramafic massif (SE Spain) using combined X-ray micro computed tomography (μ-CT) and electron backscatter diffraction (EBSD). The semidestructive sample treatment involves geographically oriented drill pressing of rocks and preparation of oriented thin sections for EBSD from the μ-CT scanned cores. The μ-CT results show that the mean intercept length (MIL) analyses provide reliable information on the shape preferred orientation (SPO) of texturally different olivine groups. We show that statistical interpretation of crystal preferred orientation (CPO) and SPO of olivine becomes feasible because the highest densities of the distribution of main olivine crystal axes from EBSD are aligned with the three axes of the 3-D ellipsoid calculated from the MIL analyses from μ-CT. From EBSD data we distinguish multiple CPO groups and by locating the thin sections within the μ-CT volume, we assign SPO to the corresponding olivine crystal aggregates, which confirm the results of statistical comparison. We demonstrate that the limitations of both methods (i.e. no crystal orientation data in μ-CT and no spatial information in EBSD) can be overcome, and the 3-D orientation of the crystallographic axes of olivines from different orientation groups can be successfully correlated with the crystal shapes of representative olivine grains. Through this approach one can establish the link among geological structures, macrostructure, fabric and 3-D SPO-CPO relationship at the hand specimen scale even in complex, coarse-grained geomaterials. © 2017 The Authors Journal of Microscopy © 2017 Royal Microscopical Society.

Deformation compatibility in a single crystalline Ni superalloy

PubMed Central

Zhang, Tiantian; Dunne, Fionn P. E.

2016-01-01

Deformation in materials is often complex and requires rigorous understanding to predict engineering component lifetime. Experimental understanding of deformation requires utilization of advanced characterization techniques, such as high spatial resolution digital image correlation (HR-DIC) and high angular resolution electron backscatter diffraction (HR-EBSD), combined with clear interpretation of their results to understand how a material has deformed. In this study, we use HR-DIC and HR-EBSD to explore the mechanical behaviour of a single-crystal nickel alloy and to highlight opportunities to understand the complete deformations state in materials. Coupling of HR-DIC and HR-EBSD enables us to precisely focus on the extent which we can access the deformation gradient, F, in its entirety and uncouple contributions from elastic deformation gradients, slip and rigid body rotations. Our results show a clear demonstration of the capabilities of these techniques, found within our experimental toolbox, to underpin fundamental mechanistic studies of deformation in polycrystalline materials and the role of microstructure. PMID:26997901

Measuring Shock Stage of ltokawa Regolith Grains by Electron Back-Scattered Diffraction and Synchrotron X-Ray Diffraction

NASA Technical Reports Server (NTRS)

Zolensky, Michael; Mikouchi, Takashi; Hagiya, Kenji; Ohsumi, Kazumasa; Martinez, James; Hagiya, Kenji; Sitzman, Scott; Terada, Yasuko; Yagi, Naoto; Komatsu, Mutsumi;

Modern Material Analysis Instruments Add a New Dimension to Materials Characterization and Failure Analysis

NASA Technical Reports Server (NTRS)

Panda, Binayak

2009-01-01

Modern analytical tools can yield invaluable results during materials characterization and failure analysis. Scanning electron microscopes (SEMs) provide significant analytical capabilities, including angstrom-level resolution. These systems can be equipped with a silicon drift detector (SDD) for very fast yet precise analytical mapping of phases, as well as electron back-scattered diffraction (EBSD) units to map grain orientations, chambers that admit large samples, variable pressure for wet samples, and quantitative analysis software to examine phases. Advanced solid-state electronics have also improved surface and bulk analysis instruments: Secondary ion mass spectroscopy (SIMS) can quantitatively determine and map light elements such as hydrogen, lithium, and boron - with their isotopes. Its high sensitivity detects impurities at parts per billion (ppb) levels. X-ray photo-electron spectroscopy (XPS) can determine oxidation states of elements, as well as identifying polymers and measuring film thicknesses on coated composites. This technique is also known as electron spectroscopy for chemical analysis (ESCA). Scanning Auger electron spectroscopy (SAM) combines surface sensitivity, spatial lateral resolution (10 nm), and depth profiling capabilities to describe elemental compositions of near and below surface regions down to the chemical state of an atom.

Crystallography of refractory metal nuggets in carbonaceous chondrites: A transmission Kikuchi diffraction approach

NASA Astrophysics Data System (ADS)

Daly, Luke; Bland, Phil A.; Dyl, Kathryn A.; Forman, Lucy V.; Saxey, David W.; Reddy, Steven M.; Fougerouse, Denis; Rickard, William D. A.; Trimby, Patrick W.; Moody, Steve; Yang, Limei; Liu, Hongwei; Ringer, Simon P.; Saunders, Martin; Piazolo, Sandra

2017-11-01

Transmission Kikuchi diffraction (TKD) is a relatively new technique that is currently being developed for geological sample analysis. This technique utilises the transmission capabilities of a scanning electron microscope (SEM) to rapidly and accurately map the crystallographic and geochemical features of an electron transparent sample. TKD uses a similar methodology to traditional electron backscatter diffraction (EBSD), but is capable of achieving a much higher spatial resolution (5-10 nm) (Trimby, 2012; Trimby et al., 2014). Here we apply TKD to refractory metal nuggets (RMNs) which are micrometre to sub-micrometre metal alloys composed of highly siderophile elements (HSEs) found in primitive carbonaceous chondrite meteorites. TKD allows us to analyse RMNs in situ, enabling the characterisation of nanometre-scale variations in chemistry and crystallography, whilst preserving their spatial and crystallographic context. This provides a complete representation of each RMN, permitting detailed interpretation of their formation history. We present TKD analysis of five transmission electron microscopy (TEM) lamellae containing RMNs coupled with EBSD and TEM analyses. These analyses revealed textures and relationships not previously observed in RMNs. These textures indicate some RMNs experienced annealing, forming twins. Some RMNs also acted as nucleation centres, and formed immiscible metal-silicate fluids. In fact, each RMN analysed in this study had different crystallographic textures. These RMNs also had heterogeneous compositions, even between RMNs contained within the same inclusion, host phase and even separated by only a few nanometres. Some RMNs are also affected by secondary processes at low temperature causing exsolution of molybdenite. However, most RMNs had crystallographic textures indicating that the RMN formed prior to their host inclusion. TKD analyses reveal most RMNs have been affected by processing in the protoplanetary disk. Despite this alteration, RMNs still preserve primary crystallographic textures and heterogeneous chemical signatures. This heterogeneity in crystallographic relationships, which mostly suggest that RMNs pre-date their host, is consistent with the idea that there is not a dominant RMN forming process. Each RMN has experienced a complex history, supporting the suggestion of Daly et al. (2017), that RMNs may preserve a diverse pre-solar chemical signature inherited from the Giant Molecular Cloud.

High Strength and Ductility of Additively Manufactured 316L Stainless Steel Explained

NASA Astrophysics Data System (ADS)

Shamsujjoha, Md.; Agnew, Sean R.; Fitz-Gerald, James M.; Moore, William R.; Newman, Tabitha A.

2018-04-01

Structure-property relationships of an additively manufactured 316L stainless steel were explored. A scanning electron microscope and electron backscattered diffraction (EBSD) analysis revealed a fine cellular-dendritic (0.5 to 2 μm) substructure inside large irregularly shaped grains ( 100 μm). The cellular structure grows along the <100> crystallographic directions. However, texture analysis revealed that the main <100> texture component is inclined by 15 deg from the building direction. X-ray diffraction line profile analysis indicated a high dislocation density of 1 × 1015 m-2 in the as-built material, which correlates well with the observed EBSD microstructure and high-yield strength, via the traditional Taylor hardening equation. Significant variations in strain hardening behavior and ductility were observed for the horizontal (HB) and vertical (VB) built samples. Ductility of HB and VB samples measured 49 and 77 pct, respectively. The initial growth texture and subsequent texture evolution during tensile deformation are held responsible for the observed anisotropy. Notably, EBSD analysis of deformed samples showed deformation twins, which predominately form in the grains with <111> aligned parallel to the loading direction. The VB samples showed higher twinning activity, higher strain hardening rates at high strain, and therefore, higher ductility. Analysis of annealed samples revealed that the observed microstructures and properties are thermally stable, with only a moderate decrease in strength and very similar levels of ductility and anisotropy, compared with the as-built condition.

High Strength and Ductility of Additively Manufactured 316L Stainless Steel Explained

NASA Astrophysics Data System (ADS)

Shamsujjoha, Md.; Agnew, Sean R.; Fitz-Gerald, James M.; Moore, William R.; Newman, Tabitha A.

2018-07-01

Structure-property relationships of an additively manufactured 316L stainless steel were explored. A scanning electron microscope and electron backscattered diffraction (EBSD) analysis revealed a fine cellular-dendritic (0.5 to 2 μm) substructure inside large irregularly shaped grains ( 100 μm). The cellular structure grows along the <100> crystallographic directions. However, texture analysis revealed that the main <100> texture component is inclined by 15 deg from the building direction. X-ray diffraction line profile analysis indicated a high dislocation density of 1 × 1015 m-2 in the as-built material, which correlates well with the observed EBSD microstructure and high-yield strength, via the traditional Taylor hardening equation. Significant variations in strain hardening behavior and ductility were observed for the horizontal (HB) and vertical (VB) built samples. Ductility of HB and VB samples measured 49 and 77 pct, respectively. The initial growth texture and subsequent texture evolution during tensile deformation are held responsible for the observed anisotropy. Notably, EBSD analysis of deformed samples showed deformation twins, which predominately form in the grains with <111> aligned parallel to the loading direction. The VB samples showed higher twinning activity, higher strain hardening rates at high strain, and therefore, higher ductility. Analysis of annealed samples revealed that the observed microstructures and properties are thermally stable, with only a moderate decrease in strength and very similar levels of ductility and anisotropy, compared with the as-built condition.

Microstructure heterogeneity after the ECAP process and its influence on recrystallization in aluminium

DOE Office of Scientific and Technical Information (OSTI.GOV)

Wronski, S., E-mail: wronski@fis.agh.edu.pl; Tarasiuk, J., E-mail: tarasiuk@ftj.agh.edu.pl; Bacroix, B., E-mail: brigitte.bacroix@univ-paris13.fr

The main purpose of the present work is to describe the qualitative and quantitative behaviours of aluminium during high strain plastic deformation and the effect of deformation on the subsequent recrystallization process. An Electron Backscatter Diffraction analysis of aluminium after the Equal channel angular pressing (ECAP) and recrystallization process is presented. In order to do this, several topological maps are measured for samples processed by 4 and 8 passes and recrystallized. The processing was conducted with route C. For all samples, distributions of grain size, misorientation, image quality factor (IQ) and texture were preceded and then analysed in some detail.more » - Highlights: ► Describe the microstructure fragmentation in aluminum. ► High strain plastic deformation and effect of deformation on recrystallization. ► The microstructure fragmentation and its influence on recrystallization. ► Image quality factor and misorientation characteristics are examined using EBSD.« less

Measurements of stress fields near a grain boundary: Exploring blocked arrays of dislocations in 3D

DOE PAGES

Guo, Y.; Collins, D. M.; Tarleton, E.; ...

2015-06-24

The interaction between dislocation pile-ups and grain boundaries gives rise to heterogeneous stress distributions when a structural metal is subjected to mechanical loading. Such stress heterogeneity leads to preferential sites for damage nucleation and therefore is intrinsically linked to the strength and ductility of polycrystalline metals. To date the majority of conclusions have been drawn from 2D experimental investigations at the sample surface, allowing only incomplete observations. Our purpose here is to significantly advance the understanding of such problems by providing quantitative measurements of the effects of dislocation pile up and grain boundary interactions in 3D. This is accomplished throughmore » the application of differential aperture X-ray Laue micro-diffraction (DAXM) and high angular resolution electron backscatter diffraction (HR-EBSD) techniques. Our analysis demonstrates a similar strain characterization capability between DAXM and HR-EBSD and the variation of stress intensity in 3D reveals that different parts of the same grain boundary may have different strengths in resisting slip transfer, likely due to the local grain boundary curvature.« less

DOE Office of Scientific and Technical Information (OSTI.GOV)

Overman, Nicole R.; Toloczko, Mychailo B.; Olszta, Matthew J.

High chromium, nickel-base Alloy 690 exhibits an increased resistance to stress corrosion cracking (SCC) in pressurized water reactor (PWR) primary water environments over lower chromium alloy 600. As a result, Alloy 690 has been used to replace Alloy 600 for steam generator tubing, reactor pressure vessel nozzles and other pressure boundary components. However, recent laboratory crack-growth testing has revealed that heavily cold-worked Alloy 690 materials can become susceptible to SCC. To evaluate reasons for this increased SCC susceptibility, detailed characterizations have been performed on as-received and cold-worked Alloy 690 materials using electron backscatter diffraction (EBSD) and Vickers hardness measurements. Examinationsmore » were performed on cross sections of compact tension specimens that were used for SCC crack growth rate testing in simulated PWR primary water. Hardness and the EBSD integrated misorientation density could both be related to the degree of cold work for materials of similar grain size. However, a microstructural dependence was observed for strain correlations using EBSD and hardness which should be considered if this technique is to be used for gaining insight on SCC growth rates« less

Testing and Comparison of Imaging Detectors for Electrons in the Energy Range 10-20 keV

NASA Astrophysics Data System (ADS)

Matheson, J.; Moldovan, G.; Kirkland, A.; Allinson, N.; Abrahams, J. P.

2017-11-01

Interest in direct detectors for low-energy electrons has increased markedly in recent years. Detection of electrons in the energy range up to low tens of keV is important in techniques such as photoelectron emission microscopy (PEEM) and electron backscatter diffraction (EBSD) on scanning electron microscopes (SEMs). The PEEM technique is used both in the laboratory and on synchrotron light sources worldwide. The ubiquity of SEMs means that there is a very large market for EBSD detectors for materials studies. Currently, the most widely used detectors in these applications are based on indirect detection of incident electrons. Examples include scintillators or microchannel plates (MCPs), coupled to CCD cameras. Such approaches result in blurring in scintillators/phosphors, distortions in optical systems, and inefficiencies due the limited active area of MCPs. In principle, these difficulties can be overcome using direct detection in a semiconductor device. Growing out of a feasibility study into the use of a direct detector for use on an XPEEM, we have built at Rutherford Appleton Laboratory a system to illuminate detectors with an electron beam of energy up to 20 keV . We describe this system in detail. It has been used to measure the performance of a custom back-thinned monolithic active pixel sensor (MAPS), a detector based on the Medipix2 chip, and a commercial detector based on MCPs. We present a selection of the results from these measurements and compare and contrast different detector types.

Characterization of etch pits found on a large-grain bulk niobium superconducting radio-frequency resonant cavity

DOE PAGES

Zhao, Xin; Ciovati, G.; Bieler, T. R.

2010-12-15

The performance of superconducting radio-frequency (SRF) resonant cavities made of bulk niobium is limited by nonlinear localized effects. Surface analysis of regions of higher power dissipation is thus of intense interest. Such areas (referred to as “hotspots”) were identified in a large-grain single-cell cavity that had been buffered-chemical polished and dissected for examination by high resolution electron microscopy, electron backscattered diffraction microscopy (EBSD), and optical microscopy. Pits with clearly discernible crystal facets were observed in both “hotspot” and “coldspot” specimens. The pits were found in-grain, at bicrystal boundaries, and on tricrystal junctions. They are interpreted as etch pits induced bymore » crystal defects (e.g. dislocations). All coldspots examined had a qualitatively lower density of etch pits or relatively smooth tricrystal boundary junctions. EBSD mapping revealed the crystal orientation surrounding the pits. Locations with high pit density are correlated with higher mean values of the local average misorientation angle distributions, indicating a higher geometrically necessary dislocation content. In addition, a survey of the samples by energy dispersive x-ray analysis did not show any significant contamination of the samples’ surface. In conclusion, the local magnetic field enhancement produced by the sharp-edge features observed on the samples is not sufficient to explain the observed degradation of the cavity quality factor, which starts at peak surface magnetic field as low as 20 mT.« less

Statistical analysis of dislocations and dislocation boundaries from EBSD data.

PubMed

Moussa, C; Bernacki, M; Besnard, R; Bozzolo, N

2017-08-01

Electron BackScatter Diffraction (EBSD) is often used for semi-quantitative analysis of dislocations in metals. In general, disorientation is used to assess Geometrically Necessary Dislocations (GNDs) densities. In the present paper, we demonstrate that the use of disorientation can lead to inaccurate results. For example, using the disorientation leads to different GND density in recrystallized grains which cannot be physically justified. The use of disorientation gradients allows accounting for measurement noise and leads to more accurate results. Misorientation gradient is then used to analyze dislocations boundaries following the same principle applied on TEM data before. In previous papers, dislocations boundaries were defined as Geometrically Necessary Boundaries (GNBs) and Incidental Dislocation Boundaries (IDBs). It has been demonstrated in the past, through transmission electron microscopy data, that the probability density distribution of the disorientation of IDBs and GNBs can be described with a linear combination of two Rayleigh functions. Such function can also describe the probability density of disorientation gradient obtained through EBSD data as reported in this paper. This opens the route for determining IDBs and GNBs probability density distribution functions separately from EBSD data, with an increased statistical relevance as compared to TEM data. The method is applied on deformed Tantalum where grains exhibit dislocation boundaries, as observed using electron channeling contrast imaging. Copyright © 2017 Elsevier B.V. All rights reserved.

Evaluation of macrozone dimensions by ultrasound and EBSD techniques

DOE Office of Scientific and Technical Information (OSTI.GOV)

Moreau, Andre, E-mail: Andre.Moreau@cnrc-nrc.gc.ca; Toubal, Lotfi; Ecole de technologie superieure, 1100, rue Notre-Dame Ouest, Montreal, QC, Canada H3C 1K3

2013-01-15

Titanium alloys are known to have texture heterogeneities, i.e. regions much larger than the grain dimensions, where the local orientation distribution of the grains differs from one region to the next. The electron backscattering diffraction (EBSD) technique is the method of choice to characterize these macro regions, which are called macrozones. Qualitatively, the images obtained by EBSD show that these macrozones may be larger or smaller, elongated or equiaxed. However, often no well-defined boundaries are observed between the macrozones and it is very hard to obtain objective and quantitative estimates of the macrozone dimensions from these data. In the presentmore » work, we present a novel, non-destructive ultrasonic technique that provides objective and quantitative characteristic dimensions of the macrozones. The obtained dimensions are based on the spatial autocorrelation function of fluctuations in the sound velocity. Thus, a pragmatic definition of macrozone dimensions naturally arises from the ultrasonic measurement. This paper has three objectives: 1) to disclose the novel, non-destructive ultrasonic technique to measure macrozone dimensions, 2) to propose a quantitative and objective definition of macrozone dimensions adapted to and arising from the ultrasonic measurement, and which is also applicable to the orientation data obtained by EBSD, and 3) to compare the macrozone dimensions obtained using the two techniques on two samples of the near-alpha titanium alloy IMI834. In addition, it was observed that macrozones may present a semi-periodical arrangement. - Highlights: Black-Right-Pointing-Pointer Discloses a novel, ultrasonic NDT technique to measure macrozone dimensions Black-Right-Pointing-Pointer Proposes a quantitative and objective definition of macrozone dimensions Black-Right-Pointing-Pointer Compares macrozone dimensions obtained using EBSD and ultrasonics on 2 Ti samples Black-Right-Pointing-Pointer Observes that macrozones may have a semi-periodical arrangement.« less

Oriented Nucleation of both Ge-Fresnoite and Benitoite/BaGe4O9 during the Surface Crystallisation of Glass Studied by Electron Backscatter Diffraction

PubMed Central

Wisniewski, Wolfgang; Patschger, Marek; Murdzheva, Steliana; Thieme, Christian; Rüssel, Christian

2016-01-01

Two glasses of the compositions 2 BaO - TiO2 - 2.75 GeO2 and 2 BaO – TiO2 –3.67 GeO2 (also known as BTG55) are annealed at temperatures from 680 to 970 °C to induce surface crystallization. The resulting samples are analyzed by X-ray diffraction (XRD) and scanning electron microscopy (SEM) including electron backscatter diffraction (EBSD). Ge-Fresnoite (Ba2TiGe2O8, BTG) is observed at the immediate surface of all samples and oriented nucleation is proven in both compositions. After a very fast kinetic selection, the crystal growth of BTG into the bulk occurs via highly oriented dendrites where the c-axes are oriented perpendicular to the surface. The growth of this oriented layer is finally blocked by dendritc BTG originating from bulk nucleation. The secondary phases BaTiGe3O9 (benitoite) and BaGe4O9 are also identified near the surface by XRD and localized by EBSD which additionally indicates orientation preferences for these phases. This behaviour is in contrast with previous reports from the Ba2TiSi2O8 as well as the Sr2TiSi2O8 systems. PMID:26853738

Mapping of elasticity and damping in an α + β titanium alloy through atomic force acoustic microscopy

PubMed Central

Phani, M Kalyan; Kumar, Anish; Jayakumar, T; Samwer, Konrad

2015-01-01

Summary The distribution of elastic stiffness and damping of individual phases in an α + β titanium alloy (Ti-6Al-4V) measured by using atomic force acoustic microscopy (AFAM) is reported in the present study. The real and imaginary parts of the contact stiffness k * are obtained from the contact-resonance spectra and by using these two quantities, the maps of local elastic stiffness and the damping factor are derived. The evaluation of the data is based on the mass distribution of the cantilever with damped flexural modes. The cantilever dynamics model considering damping, which was proposed recently, has been used for mapping of indentation modulus and damping of different phases in a metallic structural material. The study indicated that in a Ti-6Al-4V alloy the metastable β phase has the minimum modulus and the maximum damping followed by α′- and α-phases. Volume fractions of the individual phases were determined by using a commercial material property evaluation software and were validated by using X-ray diffraction (XRD) and electron back-scatter diffraction (EBSD) studies on one of the heat-treated samples. The volume fractions of the phases and the modulus measured through AFAM are used to derive average modulus of the bulk sample which is correlated with the bulk elastic properties obtained by ultrasonic velocity measurements. The average modulus of the specimens estimated by AFAM technique is found to be within 5% of that obtained by ultrasonic velocity measurements. The effect of heat treatments on the ultrasonic attenuation in the bulk sample could also be understood based on the damping measurements on individual phases using AFAM. PMID:25977847

Mapping of elasticity and damping in an α + β titanium alloy through atomic force acoustic microscopy.

PubMed

Phani, M Kalyan; Kumar, Anish; Jayakumar, T; Arnold, Walter; Samwer, Konrad

2015-01-01

The distribution of elastic stiffness and damping of individual phases in an α + β titanium alloy (Ti-6Al-4V) measured by using atomic force acoustic microscopy (AFAM) is reported in the present study. The real and imaginary parts of the contact stiffness k (*) are obtained from the contact-resonance spectra and by using these two quantities, the maps of local elastic stiffness and the damping factor are derived. The evaluation of the data is based on the mass distribution of the cantilever with damped flexural modes. The cantilever dynamics model considering damping, which was proposed recently, has been used for mapping of indentation modulus and damping of different phases in a metallic structural material. The study indicated that in a Ti-6Al-4V alloy the metastable β phase has the minimum modulus and the maximum damping followed by α'- and α-phases. Volume fractions of the individual phases were determined by using a commercial material property evaluation software and were validated by using X-ray diffraction (XRD) and electron back-scatter diffraction (EBSD) studies on one of the heat-treated samples. The volume fractions of the phases and the modulus measured through AFAM are used to derive average modulus of the bulk sample which is correlated with the bulk elastic properties obtained by ultrasonic velocity measurements. The average modulus of the specimens estimated by AFAM technique is found to be within 5% of that obtained by ultrasonic velocity measurements. The effect of heat treatments on the ultrasonic attenuation in the bulk sample could also be understood based on the damping measurements on individual phases using AFAM.

Grain Boundary Evolution of Cold-Rolled FePd Alloy during Recrystallization at Disordering Temperature

PubMed Central

Lin, Hung-Pin; Chen, Delphic; Kuo, Jui-Chao

2015-01-01

In this study, the grain boundary character and texture of 50% and 90% cold-rolled FePd alloy was investigated during recrystallization at 700 °C. Electron backscatter diffraction (EBSD) measurements were performed on the rolling direction to normal direction section. Kernel average misorientation (KAM) calculated from EBSD measurements was employed to determine the recrystallization fraction. The Avrami exponent n of recrystallization is 1.9 and 4.9 for 50% and 90% cold rolling, respectively. The new formation of texture reveals random texture during the recrystallization process. As annealing time increased, the number of high angle boundary (HAGB) and coincidence site lattice (CSL) increased with consumption of low angle boundary (LAGB). In addition, possible transformations between different grain boundaries are observed here.

A numerical and experimental investigation on seismic anisotropy of Finero Peridotite, Ivrea-Verbano Zone, northern Italy

NASA Astrophysics Data System (ADS)

Zhong, Xin; Frehner, Marcel; Zappone, Alba; Kunze, Karsten

2014-05-01

We present a combined experimental and numerical study on Finero Peridotite to investigate the major factors creating its seismic anisotropy. We extrapolate the ultrasonic seismic wave velocity measured in a hydrostatic pressure vessel to 0 MPa and 250 MPa confining pressure to compare with numerical simulations at atmospheric pressure and to restore the velocity at in-situ lower crustal conditions, respectively. A linear relation between confining pressure and seismic velocity above 80 MPa reveals the intrinsic mechanical property of the bulk rock without the interference of cracks. To visualize the crystallographic preferred orientation (CPO) we use the electron backscatter diffraction (EBSD) method and create crystallographic orientation maps and pole figures. The first also reveals the shape preferred orientation (SPO). We found that very weak CPO but significant SPO exist in most of the peridotite. The Voigt and Reuss bounds as well as the Hill average (VRH) are calculated from EBSD data to visualize seismic velocity and to calculate anisotropy in the form of velocity pole figures. We perform finite element (FE) simulations of wave propagation on the EBSD crystallographic orientation maps to calculate the effective wave velocity at different propagation angles, hence estimate the anisotropy numerically. In fracture-free models the FE simulation results agree well with the Hill average. In one case of a sample containing fractures the FE simulation yields similar minimal velocity as the laboratory measurement, which lies outside the VR bounds. This is a warning that care has to be taken when using VRH averages in fractured rocks. All three velocity estimates (hydrostatic pressure vessel, VRH average, and FE simulation) result in equally weak seismic anisotropy. This is mainly the consequence of weak CPO. Although SPO is significantly stronger it has minor influence on anisotropy. Hydrous minerals influence the seismic anisotropy only when their modal composition is large enough to allow waves to propagate preferentially through them. Unlike hornblende, phlogopite is not proven to be a major source for the seismic anisotropy due to its small modal composition. Seismic velocity is also influenced by the source frequency distribution. A lower-frequency source in the FE simulations results in lower effective velocity regardless of sample orientation. The frequency spectrum of the propagating wave is modified from source to receiver due to scattering at the mineral grains, thus leading to effective negative attenuation factors peaked at around 1-3 MHz depending on the source spectrum. However, compared with other factors, such as CPO, SPO, fractures, or hydrous mineral phases, the effect of the source frequency distribution is minor, but may be influential when extrapolated to seismic frequencies (Hz-kHz). This study provides a comprehensive method combining laboratory measurements, EBSD data, and numerical simulations to estimate seismic anisotropy. Future work may focus on modeling the influence of different pore fluids or more complex fracture geometries on seismic velocity and anisotropy. Acknowledgements This work was supported by the Swiss National Science Foundation (project UPseis, 200021_143319).

EBSD analysis of subgrain boundaries and dislocation slip systems in Antarctic and Greenland ice

NASA Astrophysics Data System (ADS)

Weikusat, Ilka; Kuiper, Ernst-Jan N.; Pennock, Gill M.; Kipfstuhl, Sepp; Drury, Martyn R.

2017-09-01

Ice has a very high plastic anisotropy with easy dislocation glide on basal planes, while glide on non-basal planes is much harder. Basal glide involves dislocations with the Burgers vector b = 〈a〉, while glide on non-basal planes can involve dislocations with b = 〈a〉, b = [c], and b = 〈c + a〉. During the natural ductile flow of polar ice sheets, most of the deformation is expected to occur by basal slip accommodated by other processes, including non-basal slip and grain boundary processes. However, the importance of different accommodating processes is controversial. The recent application of micro-diffraction analysis methods to ice, such as X-ray Laue diffraction and electron backscattered diffraction (EBSD), has demonstrated that subgrain boundaries indicative of non-basal slip are present in naturally deformed ice, although so far the available data sets are limited. In this study we present an analysis of a large number of subgrain boundaries in ice core samples from one depth level from two deep ice cores from Antarctica (EPICA-DML deep ice core at 656 m of depth) and Greenland (NEEM deep ice core at 719 m of depth). EBSD provides information for the characterization of subgrain boundary types and on the dislocations that are likely to be present along the boundary. EBSD analyses, in combination with light microscopy measurements, are presented and interpreted in terms of the dislocation slip systems. The most common subgrain boundaries are indicative of basal 〈a〉 slip with an almost equal occurrence of subgrain boundaries indicative of prism [c] or 〈c + a〉 slip on prism and/or pyramidal planes. A few subgrain boundaries are indicative of prism 〈a〉 slip or slip of 〈a〉 screw dislocations on the basal plane. In addition to these classical polygonization processes that involve the recovery of dislocations into boundaries, alternative mechanisms are discussed for the formation of subgrain boundaries that are not related to the crystallography of the host grain.The finding that subgrain boundaries indicative of non-basal slip are as frequent as those indicating basal slip is surprising. Our evidence of frequent non-basal slip in naturally deformed polar ice core samples has important implications for discussions on ice about plasticity descriptions, rate-controlling processes which accommodate basal glide, and anisotropic ice flow descriptions of large ice masses with the wider perspective of sea level evolution.

Stress and Microstructure Evolution during Transient Creep of Olivine at 1000 and 1200 °C

NASA Astrophysics Data System (ADS)

Thieme, M.; Demouchy, S. A.; Mainprice, D.; Barou, F.; Cordier, P.

2017-12-01

As the major constituent of Earth's upper mantle, olivine largely determines its physical properties. In the past, deformation experiments were usually run until steady state or to a common value of finite strain. Additionally, few studies were performed on polycrystalline aggregates at low to intermediate temperatures (<1100 °C). For the first time, we study the mechanical response and correlated microstructure as a function of incremental finite strains. Deformation experiments were conducted in uniaxial compression in an internally heated gas-medium deformation apparatus at temperatures of 1000 and 1200 °C, at strain rates of 10-5s-1 and under 300 MPa of confining pressure. Sample volumes are large with > 1.2 cm3. Finite strains range from 0.1 to 8.6 % and corresponding differential stresses range from 71 to 1073 MPa. Deformed samples were characterized by high resolution electron backscatter diffraction (EBSD) and transmission electron microscopy (TEM). EBSD maps with step sizes as low as 0.05 µm were aquired for the first time without introducing artifacts. The grain size ranges from 1.8 to 2.3 µm, with no significant change in between samples. Likewise, the texture and texture strength (J- and BA-index), grain shape and aspect ratio, density of geometrically necessary dislocations, grain orientation spread, subgrain boundary spacing and misorientation do not change significantly as a function of finite strain or temperature. The dislocation distribution is highly heterogeneous, with some grains remaining dislocation free. TEM shows grain boundaries acting as low activity sites for dislocation nucleation. Even during early mechanical steady state, plasticity seems not to affect grains in unfavorable orientations. We find no confirmation of dislocation entanglements or increasing dislocation densities being the reason for strain hardening during transient creep. This suggests other, yet not understood, mechanisms affecting the strength of deformed olivine. Futhermore, we will map disclinations (rotational topological defects) to estimate their contribution to the transient deformation regime.

Electron backscatter diffraction applied to lithium sheets prepared by broad ion beam milling.

PubMed

Brodusch, Nicolas; Zaghib, Karim; Gauvin, Raynald

2015-01-01

Due to its very low hardness and atomic number, pure lithium cannot be prepared by conventional methods prior to scanning electron microscopy analysis. Here, we report on the characterization of pure lithium metallic sheets used as base electrodes in the lithium-ion battery technology using electron backscatter diffraction (EBSD) and X-ray microanalysis using energy dispersive spectroscopy (EDS) after the sheet surface was polished by broad argon ion milling (IM). No grinding and polishing were necessary to achieve the sufficiently damage free necessary for surface analysis. Based on EDS results the impurities could be characterized and EBSD revealed the microsctructure and microtexture of this material with accuracy. The beam damage and oxidation/hydration resulting from the intensive use of IM and the transfer of the sample into the microscope chamber was estimated to be <50 nm. Despite the fact that the IM process generates an increase of temperature at the specimen surface, it was assumed that the milling parameters were sufficient to minimize the heating effect on the surface temperature. However, a cryo-stage should be used if available during milling to guaranty a heating artefact free surface after the milling process. © 2014 Wiley Periodicals, Inc.

Surface modification of hydroturbine steel using friction stir processing

NASA Astrophysics Data System (ADS)

Grewal, H. S.; Arora, H. S.; Singh, H.; Agrawal, A.

2013-03-01

Friction stir processing (FSP) has proved to be a viable tool for enhancing the mechanical properties of materials, however, the major focus has been upon improving the bulk properties of light metals and their alloys. Hydroturbines are susceptible to damage owing to slurry and cavitation erosion. In this study, FSP of a commonly employed hydroturbine steel, 13Cr4Ni was undertaken. Microstructural characterization of the processed steel was conducted using optical microscopy (OM), scanning electron microscopy (SEM) equipped with energy dispersive spectroscopy (EDS), X-ray diffraction (XRD) and electron back scatter diffraction (EBSD) techniques. Mechanical characterization of the steel was undertaken in terms of microhardness and resistance to cavitation erosion (CE). FSP resulted in the refinement of the microstructure with reduction in grain size by a factor of 10. EBSD results confirmed the existence of submicron and ultrafine grained microstructure. The microhardness of the steel was found to enhance by 2.6 times after processing. The processed steel also showed 2.4 times higher resistance against cavitation erosion in comparison to unprocessed steel. The primary erosion mechanism for both the steels was identical in nature, with plastic deformation responsible for the loss of material.

Electron back-scattered diffraction and nanoindentation analysis of nanostructured Al tubes processed by multipass tubular-channel angular pressing

NASA Astrophysics Data System (ADS)

Mesbah, Mohsen; Faraji, Ghader; Bushroa, A. R.

2016-03-01

Microstructural evolution and mechanical properties of nanostructured 1060 aluminum alloy tubes processed by tubular-channel angular pressing (TCAP) process were investigated using electron back-scattered diffraction (EBSD), transmission electron microscopy (TEM) and nanoindentation analyzes. EBSD scans revealed a homogeneous ultrafine grained microstructure after the third passes of the TCAP process. Apart from that the mean grain sizes of the TCAP processed tubes were refined to 566 nm, 500 nm and 480 nm respectively after the first, second and third passes. The results showed that after the three TCAP passes, the grain boundaries with a high angle comprised 78% of all the boundaries. This is in comparison to the first pass processed sample that includes approximately 20% HAGBs. The TEM inspection afforded an appreciation of the role of very low-angle misorientation boundaries in the process of refining microstructure. Nanoindentation results showed that hardness was the smallest form of an unprocessed sample while the largest form of the processed sample after the three passes of TCAP indicated the highest resistant of the material. In addition, the module of elasticity of the TCAP processed samples was greater from that of the unprocessed sample.

Comparison of the microstructure and phase stability of as-cast, CAD/CAM and powder metallurgy manufactured Co-Cr dental alloys.

PubMed

Li, Kai Chun; Prior, David J; Waddell, J Neil; Swain, Michael V

2015-12-01

The objective of this study was to identify the different microstructures produced by CC, PM and as-cast techniques for Co-Cr alloys and their phase stability following porcelain firings. Three bi-layer porcelain veneered Co-Cr specimens and one monolithic Co-Cr specimen of each alloy group [cast, powder metallurgy (PM), CAD/CAM (CC)] were manufactured and analyzed using electron backscatter diffraction (EBSD), energy dispersive spectrometry (EDS) and X-ray diffraction (XRD). Specimens were treated to incremental numbers of porcelain firings (control 0, 5, 15) with crystallographic data, grain size and chemical composition subsequently obtained and analyzed. EBSD datasets of the cast alloy indicated large grains >200 μm whereas PM and CC alloy consisted of mean arithmetic grain sizes of 29.6 μm and 19.2 μm respectively. XRD and EBSD results both indicated the highest increase in hcp content (>13vol%) for cast Co-Cr alloy after treatment with porcelain firing while PM and CC indicated <2vol% hcp content. A fine grain interfacial layer developed on all surfaces of the alloy after porcelain firing. The depth of this layer increased with porcelain firings for as-cast and PM but no significant increase (p>.05) was observed in CC. EDS line scans indicated an increase in Cr content at the alloy surface after porcelain firing treatment for all three alloys. PM and CC produced alloy had superior fcc phase stability after porcelain firings compared to a traditional cast alloy. It is recommended that PM and CC alloys be used for porcelain-fused-to-metal restorations. Copyright © 2015 Academy of Dental Materials. Published by Elsevier Ltd. All rights reserved.

Reinforcement of the Cube texture during recrystallization of a 1050 aluminum alloy partially recrystallized and 10% cold-rolled

DOE Office of Scientific and Technical Information (OSTI.GOV)

Wang Wei; Helbert, Anne-Laure, E-mail: anne-laure.helbert@u-psud.fr; Baudin, Thierry

In high purity Aluminum, very strong {l_brace}100{r_brace}<001> recrystallization texture is developed after 98% cold rolling and annealing at 500 Degree-Sign C. On the contrary, in Aluminum alloys of commercial purity, the Cube component hardly exceeds 30% after complete recrystallization. Parameters controlling Cube orientation development are mainly the solute dragging due to impurities in solid solution and the stored deformation energy. In the present study, besides the 85% cold rolling, two extra annealings and a slight cold rolling are introduced in the processing route to increase the Cube volume fraction. The Cube development was analyzed by X-ray diffraction and Electron BackScatteredmore » Diffraction (EBSD). The nucleation and growth mechanisms responsible for the large Cube growth were investigated using FEG/EBSD in-situ heating experiments. Continuous recrystallization was observed in Cube oriented grains and competed with SIBM (Strain Induced Boundary Migration) mechanism. This latter was favored by the stored energy gap introduced during the additional cold-rolling between the Cube grains and their neighbors. Finally, a Cube volume fraction of 65% was reached after final recrystallization. - Highlights: Black-Right-Pointing-Pointer EBSD in-situ heating experiments of aluminum alloy of commercial purity. Black-Right-Pointing-Pointer A 10% cold-rolling after a partial recrystallization improved Cube nucleation and growth. Black-Right-Pointing-Pointer Annealing before cold-rolling limited the solute drag effect and permitted a large Cube growth. Black-Right-Pointing-Pointer Cube development is enhanced by continuous recrystallization of Cube sub-grains. Black-Right-Pointing-Pointer The preferential Cube growth occurs by SIBM of small Cube grains.« less

Analysis of soft magnetic materials by electron backscatter diffraction as a powerful tool

NASA Astrophysics Data System (ADS)

Schuller, David; Hohs, Dominic; Loeffler, Ralf; Bernthaler, Timo; Goll, Dagmar; Schneider, Gerhard

2018-04-01

The current work demonstrates that electron backscatter diffraction (EBSD) is a powerful and versatile characterization technique for investigating soft magnetic materials. The properties of soft magnets, e.g., magnetic losses strongly depend on the materials chemical composition and microstructure, including grain size and shape, texture, degree of plastic deformation and elastic strain. In electrical sheet stacks for e-motor applications, the quality of the machined edges/surfaces of each individual sheet is of special interest. Using EBSD, the influence of the punching process on the microstructure at the cutting edge is quantitatively assessed by evaluating the crystallographic misorientation distribution of the deformed grains. Using an industrial punching process, the maximum affected deformation depth is determined to be 200 - 300 μm. In the case of laser cutting, the affected deformation depth is determined to be approximately zero. Reliability and detection limits of the developed EBSD approach are evaluated on non-affected sample regions and model samples containing different indentation test bodies. A second application case is the investigation of the recrystallization process during the annealing step of soft magnetic composites (SMC) toroids produced by powder metallurgy as a function of compaction pressure, annealing parameters and powder particle size. With increasing pressure and temperature, the recrystallized area fraction (e.g., grains with crystallographic misorientations < 3°) increases from 71 % (200 MPa, 800°C) to 90% (800 MPa, 800°C). Recrystallization of the compacted powder material starts at the particle boundaries or areas with existing plastic deformation. The progress of recrystallization is visualized as a function of time and of different particle to grain size distributions. Here, large particles with coarse internal grain structures show a favorable recrystallization behavior which results in large bulk permeability of up to 600 - 700 and lower amount of residual misorientations (>3°).

EBSD and TEM characterization of high burn-up mixed oxide fuel

NASA Astrophysics Data System (ADS)

Teague, Melissa; Gorman, Brian; Miller, Brandon; King, Jeffrey

2014-01-01

Understanding and studying the irradiation behavior of high burn-up oxide fuel is critical to licensing of future fast breeder reactors. Advancements in experimental techniques and equipment are allowing for new insights into previously irradiated samples. In this work dual column focused ion beam (FIB)/scanning electron microscope (SEM) was utilized to prepared transmission electron microscope samples from mixed oxide fuel with a burn-up of 6.7% FIMA. Utilizing the FIB/SEM for preparation resulted in samples with a dose rate of <0.5 mRem/h compared to ∼1.1 R/h for a traditionally prepared TEM sample. The TEM analysis showed that the sample taken from the cooler rim region of the fuel pellet had ∼2.5× higher dislocation density than that of the sample taken from the mid-radius due to the lower irradiation temperature of the rim. The dual column FIB/SEM was additionally used to prepared and serially slice ∼25 μm cubes. High quality electron back scatter diffraction (EBSD) were collected from the face at each step, showing, for the first time, the ability to obtain EBSD data from high activity irradiated fuel.

EBSD Analysis of Relationship Between Microstructural Features and Toughness of a Medium-Carbon Quenching and Partitioning Bainitic Steel

NASA Astrophysics Data System (ADS)

Li, Qiangguo; Huang, Xuefei; Huang, Weigang

2017-12-01

A multiphase microstructure of bainite, martensite and retained austenite in a 0.3C bainitic steel was obtained by a novel bainite isothermal transformation plus quenching and partitioning (B-QP) process. The correlations between microstructural features and toughness were investigated by electron backscatter diffraction (EBSD), and the results showed that the multiphase microstructure containing approximately 50% bainite exhibits higher strength (1617 MPa), greater elongation (18.6%) and greater impact toughness (103 J) than the full martensite. The EBSD analysis indicated that the multiphase microstructure with a smaller average local misorientation (1.22°) has a lower inner stress concentration possibility and that the first formed bainitic ferrite plates in the multiphase microstructure can refine subsequently generated packets and blocks. The corresponding packet and block average size decrease from 11.9 and 2.3 to 8.4 and 1.6 μm, respectively. A boundary misorientation analysis indicated that the multiphase microstructure has a higher percentage of high-angle boundaries (67.1%) than the full martensite (57.9%) because of the larger numbers and smaller sizes of packets and blocks. The packet boundary obstructs crack propagation more effectively than the block boundary.

EBSD and TEM Characterization of High Burn-up Mixed Oxide Fuel

DOE Office of Scientific and Technical Information (OSTI.GOV)

Teague, Melissa C.; Gorman, Brian P.; Miller, Brandon D.

2014-01-01

Understanding and studying the irradiation behavior of high burn-up oxide fuel is critical to licensing of future fast breeder reactors. Advancements in experimental techniques and equipment are allowing for new insights into previously irradiated samples. In this work dual column focused ion beam (FIB)/scanning electron microscope (SEM) was utilized to prepared transmission electron microscope samples from mixed oxide fuel with a burn-up of 6.7% FIMA. Utilizing the FIB/SEM for preparation resulted in samples with a dose rate of <0.5 mRem/h compared to approximately 1.1 R/h for a traditionally prepared TEM sample. The TEM analysis showed that the sample taken frommore » the cooler rim region of the fuel pellet had approximately 2.5x higher dislocation density than that of the sample taken from the mid-radius due to the lower irradiation temperature of the rim. The dual column FIB/SEM was additionally used to prepared and serially slice approximately 25 um cubes. High quality electron back scatter diffraction (EBSD) were collected from the face at each step, showing, for the first time, the ability to obtain EBSD data from high activity irradiated fuel.« less

Microstructural analysis and calcite piezometry on hydrothermal veins: Insights into the deformation history of the Cocos Plate at Site U1414 (IODP Expedition 344)

NASA Astrophysics Data System (ADS)

Brandstätter, Jennifer; Kurz, Walter; Rogowitz, Anna

2017-08-01

In this study we present microstructural data from hydrothermal veins in the sedimentary cover and the igneous basement recovered from Hole U1414A, Integrated Ocean Drilling Program (IODP) Expedition 344 (Costa Rica Seismogenesis Project), to constrain deformation mechanism operating in the subducting Cocos Plate. Cathodoluminescence studies, mechanical e-twin piezometry and electron backscatter diffraction (EBSD) analyses of carbonate veins were used to give insights into the deformation conditions and to help to understand the tectonic deformation history of the Cocos Plate offshore Costa Rica. Analyses of microstructures in the sedimentary rocks and in the basalt of the igneous basement reveal brittle deformation, as well as crystal-plastic deformation of the host rock and the vein material. Cathodoluminescence images showed that in the basalt fluid flow and related precipitation occurred over several episodes. The differential stresses, obtained from two different piezometers using the same parameter (twin density), indicate various mean differential stresses of 49 ± 11 and 69 ± 30 MPa and EBSD mapping of calcite veins reveals low-angle subgrain boundaries. Deformation temperatures are restricted to the range from 170°C to 220°C, due to the characteristics of the existing twins and the lack of high-temperature intracrystalline deformation mechanisms (>220°C). The obtained results suggest that deformation occurred over a period associated with changes of ambient temperatures, occurrence of fluids and hydrofracturing, induced differential stresses due to the bending of the plate at the trench, and related seismic activity.

Microstructural analysis and calcite piezometry on hydrothermal veins: Insights into the deformation history of the Cocos Plate at Site U1414 (IODP Expedition 344).

PubMed

Brandstätter, Jennifer; Kurz, Walter; Rogowitz, Anna

2017-08-01

In this study we present microstructural data from hydrothermal veins in the sedimentary cover and the igneous basement recovered from Hole U1414A, Integrated Ocean Drilling Program (IODP) Expedition 344 (Costa Rica Seismogenesis Project), to constrain deformation mechanism operating in the subducting Cocos Plate. Cathodoluminescence studies, mechanical e-twin piezometry and electron backscatter diffraction (EBSD) analyses of carbonate veins were used to give insights into the deformation conditions and to help to understand the tectonic deformation history of the Cocos Plate offshore Costa Rica. Analyses of microstructures in the sedimentary rocks and in the basalt of the igneous basement reveal brittle deformation, as well as crystal-plastic deformation of the host rock and the vein material. Cathodoluminescence images showed that in the basalt fluid flow and related precipitation occurred over several episodes. The differential stresses, obtained from two different piezometers using the same parameter (twin density), indicate various mean differential stresses of 49 ± 11 and 69 ± 30 MPa and EBSD mapping of calcite veins reveals low-angle subgrain boundaries. Deformation temperatures are restricted to the range from 170°C to 220°C, due to the characteristics of the existing twins and the lack of high-temperature intracrystalline deformation mechanisms (>220°C). The obtained results suggest that deformation occurred over a period associated with changes of ambient temperatures, occurrence of fluids and hydrofracturing, induced differential stresses due to the bending of the plate at the trench, and related seismic activity.

Microstructural analysis and calcite piezometry on hydrothermal veins: Insights into the deformation history of the Cocos Plate at Site U1414 (IODP Expedition 344)

PubMed Central

Kurz, Walter; Rogowitz, Anna

2017-01-01

Abstract In this study we present microstructural data from hydrothermal veins in the sedimentary cover and the igneous basement recovered from Hole U1414A, Integrated Ocean Drilling Program (IODP) Expedition 344 (Costa Rica Seismogenesis Project), to constrain deformation mechanism operating in the subducting Cocos Plate. Cathodoluminescence studies, mechanical e‐twin piezometry and electron backscatter diffraction (EBSD) analyses of carbonate veins were used to give insights into the deformation conditions and to help to understand the tectonic deformation history of the Cocos Plate offshore Costa Rica. Analyses of microstructures in the sedimentary rocks and in the basalt of the igneous basement reveal brittle deformation, as well as crystal‐plastic deformation of the host rock and the vein material. Cathodoluminescence images showed that in the basalt fluid flow and related precipitation occurred over several episodes. The differential stresses, obtained from two different piezometers using the same parameter (twin density), indicate various mean differential stresses of 49 ± 11 and 69 ± 30 MPa and EBSD mapping of calcite veins reveals low‐angle subgrain boundaries. Deformation temperatures are restricted to the range from 170°C to 220°C, due to the characteristics of the existing twins and the lack of high‐temperature intracrystalline deformation mechanisms (>220°C). The obtained results suggest that deformation occurred over a period associated with changes of ambient temperatures, occurrence of fluids and hydrofracturing, induced differential stresses due to the bending of the plate at the trench, and related seismic activity. PMID:29081570

Effects of Retained Austenite Volume Fraction, Morphology, and Carbon Content on Strength and Ductility of Nanostructured TRIP-assisted Steels

DOE Office of Scientific and Technical Information (OSTI.GOV)

Shen, Yongfeng; Qiu, LN; Sun, Xin

2015-06-01

With a suite of multi-modal and multi-scale characterization techniques, the present study unambiguously proves that a substantially-improved combination of ultrahigh strength and good ductility can be achieved by tailoring the volume fraction, morphology, and carbon content of the retained austenite (RA) in a transformation-induced-plasticity (TRIP) steel with the nominal chemical composition of 0.19C-0.30Si-1.76Mn-1.52Al (weight percent, wt.%). After intercritical annealing and bainitic holding, a combination ultimate tensile strength (UTS) of 1,100 MPa and true strain of 50% has been obtained, as a result of the ultrafine RA lamellae, which are alternately arranged in the bainitic ferrite around junction regions of ferritemore » grains. For reference, specimens with a blocky RA, prepared without the bainitic holding, yield a low ductility (35%) and a low UTS (800 MPa). The volume fraction, morphology, and carbon content of RA have been characterized using various techniques, including magnetic probing, scanning electron microscopy (SEM), electron-backscatter-diffraction (EBSD), and transmission electron microscopy (TEM). Interrupted tensile tests, mapped using EBSD in conjunction with the kernel average misorientation (KAM) analysis, reveal that the lamellar RA is the governingmicrostructure component responsible for the higher mechanical stability, compared to the blocky one. By coupling these various techniques, we quantitatively demonstrate that in addition to the RA volume fraction, its morphology and carbon content are equally important in optimizing the strength and ductility of TRIP-assisted steels.« less

Role of microstructure on twin nucleation and growth in HCP titanium: A statistical study

DOE Office of Scientific and Technical Information (OSTI.GOV)

Arul Kumar, M.; Wroński, M.; McCabe, Rodney James

In this study, a detailed statistical analysis is performed using Electron Back Scatter Diffraction (EBSD) to establish the effect of microstructure on twin nucleation and growth in deformed commercial purity hexagonal close packed (HCP) titanium. Rolled titanium samples are compressed along rolling, transverse and normal directions to establish statistical correlations for {10–12}, {11–21}, and {11–22} twins. A recently developed automated EBSD-twinning analysis software is employed for the statistical analysis. Finally, the analysis provides the following key findings: (I) grain size and strain dependence is different for twin nucleation and growth; (II) twinning statistics can be generalized for the HCP metalsmore » magnesium, zirconium and titanium; and (III) complex microstructure, where grain shape and size distribution is heterogeneous, requires multi-point statistical correlations.« less

Role of microstructure on twin nucleation and growth in HCP titanium: A statistical study

DOE PAGES

Arul Kumar, M.; Wroński, M.; McCabe, Rodney James; ...

2018-02-01

In this study, a detailed statistical analysis is performed using Electron Back Scatter Diffraction (EBSD) to establish the effect of microstructure on twin nucleation and growth in deformed commercial purity hexagonal close packed (HCP) titanium. Rolled titanium samples are compressed along rolling, transverse and normal directions to establish statistical correlations for {10–12}, {11–21}, and {11–22} twins. A recently developed automated EBSD-twinning analysis software is employed for the statistical analysis. Finally, the analysis provides the following key findings: (I) grain size and strain dependence is different for twin nucleation and growth; (II) twinning statistics can be generalized for the HCP metalsmore » magnesium, zirconium and titanium; and (III) complex microstructure, where grain shape and size distribution is heterogeneous, requires multi-point statistical correlations.« less

Effect of annealing on Curie temperature and phase transition in La{sub 0.55}Sr{sub 0.08}Mn{sub 0.37}O{sub 3} epitaxial films grown on SrTiO{sub 3} (100) substrates by reactive radio frequency magnetron sputtering

DOE Office of Scientific and Technical Information (OSTI.GOV)

Ichinose, T.

2016-08-15

Mn-poor LaSrMnO{sub 3} (LSMO) epitaxial films were grown on SrTiO{sub 3} (100) substrates by radio frequency magnetron sputtering in an argon and oxygen gas mix, and then the samples were annealed in air at various temperatures (T{sub a}). 2 theta-chi X-ray diffraction mapping, nano-beam diffraction analysis through transmission electron microscopy, and electron back scatter diffraction through scanning electron microscopy revealed that the crystal symmetry of the LSMO films changed from monoclinic/orthorhombic to rhombohedral on annealing in air. Curie temperature (T{sub C}) of the LSMO films was found to increase with increasing T{sub a}, and become higher than the room temperaturemore » at T{sub a} ≥ 861 °C, indicating that the cause of these changes was the filling of oxygen and the transition of the crystal symmetry into rhombohedral. - Highlights: •Mn-poor LSMO changed from monoclinic/orthorhombic to rhombohedral by oxygen supply. •Mn-poor LSMO was increased T{sub C} by changed crystal symmetry, and it showed T{sub C} above RT. •Annealed in air effectively supplied O{sub 2} more than O{sub 2} gas during sputtering •EBSD is useful to evaluate crystal symmetry of complex oxide film from the substrate.« less

Crystallography and Morphology of Niobium Carbide in As-Cast HP-Niobium Reformer Tubes

NASA Astrophysics Data System (ADS)

Buchanan, Karl G.; Kral, Milo V.

2012-06-01

The microstructures of two as-cast heats of niobium-modified HP stainless steels were characterized. Particular attention was paid to the interdendritic niobium-rich carbides formed during solidification of these alloys. At low magnifications, these precipitates are grouped in colonies of similar lamellae. Higher magnifications revealed that the lamellae actually obtain two distinct morphologies. The type I morphology exhibits broad planar interfaces with a smooth platelike shape. Type II lamellae have undulating interfaces and an overall reticulated shape. To provide further insight into the origin of these two different morphologies, the microstructure and crystallography of each have been studied in detail using high resolution scanning electron microscopy, transmission electron microscopy, various electron diffraction methods (electron backscatter diffraction (EBSD), selected area diffraction (SAD), and convergent beam electron diffraction (CBED)), and energy dispersive X-ray spectroscopy.

Three dimensional X-ray Diffraction Contrast Tomography Reconstruction of Polycrystalline Strontium Titanate during Sintering and Electron Backscatter Diffraction Validation

NASA Astrophysics Data System (ADS)

Syha, M.; Rheinheimer, W.; Loedermann, B.; Graff, A.; Trenkle, A.; Baeurer, M.; Weygand, D.; Ludwig, W.; Gumbsch, P.

The microstructural evolution of polycrystalline strontium titanate was investigated in three dimensions (3D) using X-ray diffraction contrast tomography (DCT) before and after ex-situ annealing at 1600°C. Post-annealing, the specimen was additionally subjected to phase contrast tomography (PCT) in order to finely resolve the porosities. The resulting microstructure reconstructions were studied with special emphasis on morphology and interface orientation during microstructure evolution. Subsequently, cross-sections of the specimen were studied using electron backscatter diffraction (EBSD). Corresponding cross-sections through the 3D reconstruction were identified and the quality of the reconstruction is validated with special emphasis on the spatial resolution at the grain boundaries, the size and location of pores contained in the material and the accuracy of the orientation determination.

Acquisition of a High Resolution Field Emission Scanning Electron Microscope for the Analysis of Returned Samples

NASA Technical Reports Server (NTRS)

Nittler, Larry R.

2003-01-01

This grant furnished funds to purchase a state-of-the-art scanning electron microscope (SEM) to support our analytical facilities for extraterrestrial samples. After evaluating several instruments, we purchased a JEOL 6500F thermal field emission SEM with the following analytical accessories: EDAX energy-dispersive x-ray analysis system with fully automated control of instrument and sample stage; EDAX LEXS wavelength-dispersive x-ray spectrometer for high sensitivity light-element analysis; EDAX/TSL electron backscatter diffraction (EBSD) system with software for phase identification and crystal orientation mapping; Robinson backscatter electron detector; and an in situ micro-manipulator (Kleindiek). The total price was $550,000 (with $150,000 of the purchase supported by Carnegie institution matching funds). The microscope was delivered in October 2002, and most of the analytical accessories were installed by January 2003. With the exception of the wavelength spectrometer (which has been undergoing design changes) everything is working well and the SEM is in routine use in our laboratory.

Microstructural evolution and rheology of quartz in a mid-crustal shear zone

NASA Astrophysics Data System (ADS)

Rahl, Jeffrey M.; Skemer, Philip

2016-06-01

We present microstructural and crystallographic preferred orientation (CPO) data on quartz deformed in the middle crust to explore the interaction and feedback between dynamic recrystallization, deformation processes, and CPO evolution. The sample investigated here is a moderately deformed quartz-rich mylonite from the Blue Ridge in Virginia. We have created high-resolution crystallographic orientation maps using electron backscatter diffraction (EBSD) of 51 isolated quartz porphyroclasts with recrystallized grain fractions ranging from 10 to 100%. Recrystallized grains are internally undeformed and display crystallographic orientations dispersed around the orientation of the associated parent porphyroclast. We document a systematic decrease in fabric intensity with recrystallization, suggesting that progressive deformation of the recrystallized domains involves processes that can weaken a pre-existing CPO. Relationships between recrystallization fraction and shear strain suggest that complete microstructural re-equilibration requires strains in excess of γ = 5. Variation in the degree of recrystallization implies that strain was accumulated heterogeneously, and that a steady-state microstructure and rheology were not achieved.

Scaling ice microstructures from the laboratory to nature: cryo-EBSD on large samples.

NASA Astrophysics Data System (ADS)

Prior, David; Craw, Lisa; Kim, Daeyeong; Peyroux, Damian; Qi, Chao; Seidemann, Meike; Tooley, Lauren; Vaughan, Matthew; Wongpan, Pat

2017-04-01

Electron backscatter diffraction (EBSD) has extended significantly our ability to conduct detailed quantitative microstructural investigations of rocks, metals and ceramics. EBSD on ice was first developed in 2004. Techniques have improved significantly in the last decade and EBSD is now becoming more common in the microstructural analysis of ice. This is particularly true for laboratory-deformed ice where, in some cases, the fine grain sizes exclude the possibility of using a thin section of the ice. Having the orientations of all axes (rather than just the c-axis as in an optical method) yields important new information about ice microstructure. It is important to examine natural ice samples in the same way so that we can scale laboratory observations to nature. In the case of ice deformation, higher strain rates are used in the laboratory than those seen in nature. These are achieved by increasing stress and/or temperature and it is important to assess that the microstructures produced in the laboratory are comparable with those observed in nature. Natural ice samples are coarse grained. Glacier and ice sheet ice has a grain size from a few mm up to several cm. Sea and lake ice has grain sizes of a few cm to many metres. Thus extending EBSD analysis to larger sample sizes to include representative microstructures is needed. The chief impediments to working on large ice samples are sample exchange, limitations on stage motion and temperature control. Large ice samples cannot be transferred through a typical commercial cryo-transfer system that limits sample sizes. We transfer through a nitrogen glove box that encloses the main scanning electron microscope (SEM) door. The nitrogen atmosphere prevents the cold stage and the sample from becoming covered in frost. Having a long optimal working distance for EBSD (around 30mm for the Otago cryo-EBSD facility) , by moving the camera away from the pole piece, enables the stage to move without crashing into either the EBSD camera or the SEM pole piece (final lens). In theory a sample up to 100mm perpendicular to the tilt axis by 150mm parallel to the tilt axis can be analysed. In practice, the motion of our stage is restricted to maximum dimensions of 100 by 50mm by a conductive copper braid on our cold stage. Temperature control becomes harder as the samples become larger. If the samples become too warm then they will start to sublime and the quality of EBSD data will reduce. Large samples need to be relatively thin ( 5mm or less) so that conduction of heat to the cold stage is more effective at keeping the surface temperature low. In the Otago facility samples of up to 40mm by 40mm present little problem and can be analysed for several hours without significant sublimation. Larger samples need more care, e.g. fast sample transfer to keep the sample very cold. The largest samples we work on routinely are 40 by 60mm in size. We will show examples of EBSD data from glacial ice and sea ice from Antarctica and from large laboratory ice samples.

XRD and EBSD analysis of anisotropic microstructure development in cold rolled F138 stainless steel

DOE Office of Scientific and Technical Information (OSTI.GOV)

De Vincentis, N.S., E-mail: devincentis@ifir-conic

The microstructural characteristics of deformation-processed materials highly influence their mechanical properties. For a complete characterization of a microstructure both local and global information must be gathered, which requires the combination of different analysis techniques. X-ray and Electron Backscatter Diffraction were used in the present paper to characterize the deformation induced in a cold rolled F138 austenitic stainless steel sample. The results obtained using laboratory and synchrotron X-ray sources were compared and combined with EBSD quantitative results, allowing the global and local characterization and orientation dependence of the deformation microstructure. A particular behavior was observed in the XRD data corresponding tomore » the planes with < 220 >∥ ND, likely due to a smaller amount of defects accumulated in the crystals with that particular orientation. EBSD was used to separate the scans data into partitions and to calculate misorientation variables and parameters, showing that this behavior can be attributed to a combination of larger grain sizes, lower local boundary misorientations and dislocation densities for crystals having < 220 >∥ ND. Several conclusions, of general validity for the evaluation of microstructure anisotropy, can be extracted from the results. - Highlights: •Combined XRD and EBSD for studying microstructure gave a superb insight on anisotropic accumulation of defects. •W-H and CMWP methods were applied for checking consistency of results. •XRD showed that a smaller accumulation of defects occurred in crystals with < 220 >∥ ND. •High brilliance X-ray beam allowed to study the anisotropy of defect accumulation.« less

EBSD characterization of the growth mechanism of SiC synthesized via direct microwave heating

DOE Office of Scientific and Technical Information (OSTI.GOV)

Wang, Jigang, E-mail: wangjigang@seu.edu.cn; Xizang Key Laboratory of Optical Information Processing and Visualization Technology, School of Information Engineering, Xizang Minzu University, Xianyang 712082; Huang, Shan

2016-04-15

Well-crystallized 3C-silicon carbide (SiC) grains/nanowires have been synthesized rapidly and conveniently via direct microwave heating, simply using silicon dioxide powders and artificial graphite as raw materials. The comprehensive characterizations have been employed to investigate the micro-structure of the obtained 3C-SiC products. Results indicated that, different from the classic screw dislocation growth mechanism, the 3C-SiC grains/nanowires synthesized via high-energy vacuum microwave irradiation were achieved through the two-dimension nucleation and laminar growth mechanism. Especially, the electron backscattered diffraction (EBSD) was employed to characterize the crystal planes of the as-grown SiC products. The calculated Euler angles suggested that the fastest-growing crystal planes (211)more » were overlapped gradually. Through the formation of the (421) transformation plane, (211) finally evolved to (220) which existed as the side face of SiC grains. The most stable crystal planes (111) became the regular hexagonal planes in the end, which could be explained by the Bravais rule. The characterization results of EBSD provided important experimental information for the evolution of crystal planes. - Graphical abstract: The formation of 3C-SiC prepared via direct microwave heating follows the mechanism of two-dimension nucleation and laminar growth. - Highlights: • 3C−SiC grains/nanowires were obtained via direct microwave heating. • 3C−SiC followed the mechanism of two-dimension nucleation and laminar growth. • In-situ EBSD analysis provided the experimental evidences of the growth.« less

Applying Transmission Kikuchi Diffraction (TKD) to Understand Nanogranular Fault Rock Materials

NASA Astrophysics Data System (ADS)

Smith, S. A. F.; Demurtas, M.; Prior, D. J.; Di Toro, G.

2017-12-01

Nanoparticles (<< 1 µm) form in the localized slip zones of natural and experimental faults, but their origin (e.g. seismic vs. aseismic slip) and mechanical behaviour is still debated. Understanding the deformation processes that produce nanoparticles in faults requires an understanding of grain sizes, shapes and crystallographic orientations at higher spatial resolution than is currently possible using standard EBSD techniques. Transmission Kikuchi Diffraction (TKD) in the SEM is a technique that allows to overcome this spatial resolution issue by performing orientation mapping in a commercial EBSD system on electron transparent foils with resolutions that can be below 10 nm. Therefore, the potential of TKD to understand deformation processes in nanoparticles is very high. We present results of TKD analysis performed on mixed calcite-dolomite gouges deformed in a rotary-shear apparatus at slip rates ranging from sub-seismic to co-seismic (30 µm/s to 1 m/s). Samples for TKD were prepared by argon ion slicing, a method that yields relatively large (104 µm2) electron transparent areas, as well as standard argon ion milling. Coupled TKD-EDS analysis allows quantification of elemental contents at a scale of tens of nanometers. Preliminary results show that at a slip velocity of 1 m/s, the localized slip zone that forms in the gouges during shearing is composed of recrystallized grains of calcite and Mg-calcite (the latter being a decarbonation product of dolomite) with an average grain size of c. 300 nm. Individual grains are characterized by relatively straight boundaries, and many triple and quadruple grain junctions are present. The nanogranular aggregates show a polygonised texture with absence of clear porosity and shape preferred orientation. Orientation data show a random distribution of the calcite c-axes. Further investigation will help to obtain new insights into the deformation mechanisms active during seismic faulting in carbonate-bearing faults. The integration of grain size, grain shape and crystallographic information into flow laws will help to describe and predict the rheological behaviour of carbonate faults during seismic sliding.

Evaluation of in-situ deformation experiments of TRIP steel

NASA Astrophysics Data System (ADS)

Procházka, J.; Kučerová, L.; Bystrianský, M.

2017-02-01

The paper reports on the behaviour of low alloyed TRIP (transformation induced plasticity) steel with Niobium during tensile test. The structures were analysed using in-situ tensile testing coupled with electron backscattering diffraction (EBSD) analysis carried out in scanning electron microscope (SEM). Steel specimens were of same chemical composition; however three different annealing temperatures, 800 °C, 850 °C and 950 °C, were applied to the material during the heat treatment. The treatment consisted of annealing for 20 minutes in the furnace; cooling in salt bath after the heating and holding at 425 °C for 20 minutes for all the samples. Untreated bar was used as reference material. Flat samples for deformation stage were cut out of the heat-treated bars. In situ documentation of microstructure and crystallography development were carried out during the deformation experiments. High deformation lead to significant degradation of EBSD signal.

Analysis of FIB-induced damage by electron channelling contrast imaging in the SEM.

PubMed

Gutierrez-Urrutia, Ivan

2017-01-01

We have investigated the Ga + ion-damage effect induced by focused ion beam (FIB) milling in a [001] single crystal of a 316 L stainless steel by the electron channelling contrast imaging (ECCI) technique. The influence of FIB milling on the characteristic electron channelling contrast of surface dislocations was analysed. The ECCI approach provides sound estimation of the damage depth produced by FIB milling. For comparison purposes, we have also studied the same milled surface by a conventional electron backscatter diffraction (EBSD) approach. We observe that the ECCI approach provides further insight into the Ga + ion-damage phenomenon than the EBSD technique by direct imaging of FIB artefacts in the scanning electron microscope. We envisage that the ECCI technique may be a convenient tool to optimize the FIB milling settings in applications where the surface crystal defect content is relevant. © 2016 The Authors Journal of Microscopy © 2016 Royal Microscopical Society.

Nano-Scale Structure of Twin Boundaries in Shocked Zircon from the Vredefort Impact Structure.

NASA Astrophysics Data System (ADS)

Sharp, T. G.; Cavosie, A. J.

2017-12-01

Shock deformation of zircon produces distinct microstructures that can be used as evidence of shock in natural samples. These deformation features include {112} twins that have been observed in naturally shocked samples from Vredefort and elsewhere [1-3]. Electron backscatter diffraction (EBSD) has shown that these twins are polysynthetic, generally < 1µm wide and have a 65°/<110> crystallographic relation to the host zircon [2]. The structure and composition of these twin boundaries, and their effects on element mobility have not been explored previously. Here we use high-resolution TEM to investigate the nano-structure of a {112} twin in a shocked zircon crystal from the 2.0 Ga Vredefort impact structure [3]. Focused-ion-beam lift-out techniques were used to prepare a TEM foil with a 1 µm wide {112}-twin lamella. The foil was characterized by TEM imaging and electron diffraction using a FEI CM200-FEG transmission electron microscope. Selected area diffraction from the {112}-twin boundary, along a <111> zone, showed no apparent evidence of twining. However, the domain boundaries displayed weak diffraction contrast in this orientation. High-resolution images show a 50-nm wide zone of heterogeneous structural disorder and locally amorphous domains along the twin boundaries that is inferred to be a localized metamict zone. The detailed lattice structure of the interface was not discernable because of this structural disorder. Diffraction and imaging along <021> confirms that the {112}-twin composition plane is a mirror plane. The crystallographic relations observed along <110> and <021> are consistent with the 65°/<110> twin structure previously determined from EBSD [2]. Enhanced metamict disorder suggests a higher concentration of actinides along the twin boundaries and implies actinide mobility near twin boundaries. [1] Moser et al, 2011 Can J Earth Sci. [2] Erickson et al. 2013 Am Min. [3] Cavosie et al. 2015 Geol.

Investigation of Synthetic Mg(1.3)V(1.7)O4 Spinel with MgO Inclusions: Case Study of a Spinel with an Apparently occupied Interstitial Site

NASA Technical Reports Server (NTRS)

Uchida, Hinako; Righter, Kevin; Lavina, Barbara; Nowell, Matthew M.; Wright, Stuart I.; Downs, Robert T.; Yang, Hexiong

2007-01-01

A magnesium vanadate spinel crystal, ideally MgV2O4, synthesized at 1 bar, 1200 C and equilibrated under FMQ + 1.3 log f(sub o2) condition, was investigated using single-crystal X-ray diffraction, electron microprobe, and electron backscatter (EBSD). The initial X-ray structure refinements gave tetrahedral and octahedral site occupancies, along with the presence of 0.053 apfu Mg at an interstitial octahedral site . Back-scattered electron (BSE) images and electron microprobe analyses revealed the existence of an Mg-rich phase in the spinel matrix, which was too small (less than or equal to 3microns) for an accurate chemical determination. The EBSD analysis combined with X-ray energy dispersive spectroscop[y (XEDS) suggested that the Mg-rich inclusions are periclase oriented coherently with the spinel matrix. The final structure refinements were optimized by subtracting the X-ray intensity contributions (approx. 9%) of periclase reflections, which eliminated the interstitial Mg. This study provides insight into possible origins of refined interstitial cations reported in the the literature for spinel, and points to the difficulty of using only X-ray diffraction data to distinguish a spinel with interstitial cations from one with coherently oriented MgO inclusions.

Microstructure, microtexture and precipitation in the ultrafine-grained surface layer of an Al-Zn-Mg-Cu alloy processed by sliding friction treatment

DOE Office of Scientific and Technical Information (OSTI.GOV)

Chen, Yanxia

2017-01-15

Precipitate redistribution and texture evolution are usually two concurrent aspects accompanying grain refinement induced by various surface treatment. However, the detailed precipitate redistribution characteristics and process, as well as crystallographic texture in the surface refined grain layer, are still far from full understanding. In this study, we focused on the microstructural and crystallographic features of the sliding friction treatment (SFT) induced surface deformation layer in a 7050 aluminum alloy. With the combination of transmission electron microscopy (TEM) and high angle angular dark field scanning TEM (HAADF-STEM) observations, a surface ultrafine grain (UFG) layer composed of both equiaxed and lamellar ultrafinemore » grains and decorated by high density of coarse grain boundary precipitates (GBPs) were revealed. Further precession electron diffraction (PED) assisted orientation mapping unraveled that high angle grain boundaries rather than low angle grain boundaries are the most favorable nucleation sites for GBPs. The prominent precipitate redistribution can be divided into three successive and interrelated stages, i.e. the mechanically induced precipitate dissolution, solute diffusion and reprecipitation. The quantitative prediction based on pipe diffusion along dislocations and grain boundary diffusion proved the distribution feasibility of GBPs around UFGs. Based on PED and electron backscatter diffraction (EBSD) analyses, the crystallographic texture of the surface UFG layer was identified as a shear texture composed of major rotated cube texture (001) 〈110〉 and minor (111) 〈112〉, while that of the adjoining lamellar coarse grained matrix was pure brass. The SFT induced surface severe shear deformation is responsible for texture evolution. - Highlights: •The surface ultrafine grain layer in a 7050 aluminum alloy was focused. •Precipitate redistribution and texture evolution were discussed. •The quantitative prediction proved the distribution feasibility of GBPs. •Precession electron diffraction orientation mapping showed a shear texture.« less

In-situ observation of recrystallization in an AlMgScZr alloy using confocal laser scanning microscopy

DOE Office of Scientific and Technical Information (OSTI.GOV)

Taendl, J., E-mail: johannes.taendl@tugraz.atl; Nambu, S.; Orthacker, A.

2015-10-15

In this work we present a novel in-situ approach to study the recrystallization behavior of age hardening alloys. We use confocal laser scanning microscopy (CLSM) at 400 °C to investigate the static recrystallization of an AlMg4Sc0.4Zr0.12 alloy in-situ. The results are combined with electron backscatter diffraction (EBSD) and transmission electron microscopy (TEM) analyses. It was found that CLSM is a powerful tool to visualize both the local initiation and temporal sequence of recrystallization. After fast nucleation and initial growth, the grain growth rate decreases and the grain boundary migration stops after some minutes due to Zener pinning from Al{sub 3}(Sc,Zr)more » precipitates produced during the heat treatment. EBSD and TEM analyses confirm both the boundary movements and the particle-boundary interactions. - Highlights: • First time that CLSM is used to study recrystallization in-situ. • The start and end of recrystallization can be directly observed. • The procedure is easy to apply and requires only simple data interpretation. • In-situ observations on the surface correlate to modifications inside the bulk. • In-situ observations correlate to EBSD and EFTEM analyses.« less

EBSD analysis of the Shergottite Meteorites: New developments within the technique and their implication on what we know about the preferred orientation of Martian minerals

NASA Astrophysics Data System (ADS)

Stephen, N.; Benedix, G. K.; Bland, P.; Berlin, J.; Salge, T.; Goran, D.

2011-12-01

What we know about the geology and mineralogy of the Martian surface has been characterised by both the use of remote sensing techniques and the analysis of Martian meteorites. Various techniques are employed to conduct these analyses including crystallographic, geochemical and spectral measurements, all of which enable us to infer a geological history for these rocks. Several references have been made to the potential for preferred orientation of crystals within the Shergottites [1] and their implication for the cooling history of the respective magmas on Mars [2]. We have already shown that a preferred orientation of the two pyroxenes, augite and pigeonite, can be seen in the Zagami meteorite using electron back-scatter diffraction (EBSD) analysis [3]. However, when compared to previous modal studies of the same meteorites [4], it becomes apparent that the current EBSD datasets for Martian meteorites are incomplete. Indexing of some minerals can be hampered by the lack of available matches within library databases for EBSD, or become difficult to resolve between minerals where crystallographic differences between similar minerals fall below the technical limitations of the instrument [3]. Recent advances in EBSD technologies combined with the simultaneous acquisition of energy-dispersive spectra (EDS) however now allow us to determine a more comprehensive set of analyses in a much shorter period of time, fully resolving even similar minerals where areas have been left with no indexing previously [5]. Preliminary investigations suggest that the new technology can successfully index >90% of the sample. The most recent EBSD analyses potentially reveals previously unseen fabrics in the meteorites alongside the EDS hyper-spectral imaging helping to resolve any unknown or questionable phases within them. In this study we will present new data from an investigation using EDS alongside EBSD analysis on 2 Shergottite meteorites, SAU 005 and Zagami, to further resolve their constituent minerals and any existing preferred orientations. [1] Stolper E. and McSween, H.Y. Jnr (1979) Geochemica et Cosomochimica Acta, 43, 1475-1498 [2] McCoy, T.J. et al. (1992) Geochimica et Cosomochimica Acta, 56, 3571-3582 [3] N.R. Stephen et al. (2010) Abstract #5008 73rd Annual Meeting of the Meteoritical Society [4] N.R. Stephen et al. (2010) Abstract #2367 Lunar & Planetary Science Conference XLI [5] J. Berlin et al. (2011) Abstract #2723 Lunar & Planetary Science Conference XLII

Magnetic anisotropy and magnetite textures from experimental shear deformation

NASA Astrophysics Data System (ADS)

Till, Jessica; Moskowitz, Bruce

2015-04-01

Magnetite is a common accessory mineral in crustal rocks and exerts a dominant influence on the magnetic anisotropy of rocks when present. Therefore the deformation behavior of magnetite strongly determines how magnetic fabric develops with increasing strain in a deforming rock. Here we show results from experimental deformation of magnetite-silicate aggregates in high-temperature transpressional shear experiments (1000-1200°C) under moderate shear stresses (10-130 MPa) using a gas-medium deformation apparatus. Anisotropy of magnetic susceptibility, shape preferred orientation (SPO) of magnetite, and electron backscatter diffraction (EBSD) were each used to characterize the magnetite deformation fabrics and intragrain microstructures. Magnetic anisotropy and SPO each increase strongly with increasing strain, which ranged between 100-300%. An interesting feature of the deformation fabrics is that both magnetite SPO and magnetic fabric intensity are stronger at higher temperatures, indicating that strain partitioning between magnetite and the plagioclase matrix decreases at higher temperatures. Although flow laws for magnetite predict it to be weaker than dry plagioclase at the experimental conditions, the temperature-dependence of the fabric strength indicates that magnetite is more viscous than the "wet" plagioclase used in the experiments. In contrast to the magnetic and shape fabrics, crystallographic preferred orientation (CPO) of magnetite is very weak in all deformed samples. In EBSD orientation mapping of individual particles, incipient subgrain boundary formation is evident in magnetite grains, indicating that dislocation creep processes were active in magnetite despite the lack of a well-developed CPO. The weak magnetite CPOs are primarily attributed to multiple slip systems acting in parallel. These findings support the observations of previous studies that crystallographic textures in cubic minerals such as magnetite may be inherently weak or slow to develop and that CPO alone is not always a reliable indicator of deformation mechanisms.

Large volume serial section tomography by Xe Plasma FIB dual beam microscopy.

PubMed

Burnett, T L; Kelley, R; Winiarski, B; Contreras, L; Daly, M; Gholinia, A; Burke, M G; Withers, P J

2016-02-01

Ga(+) Focused Ion Beam-Scanning Electron Microscopes (FIB-SEM) have revolutionised the level of microstructural information that can be recovered in 3D by block face serial section tomography (SST), as well as enabling the site-specific removal of smaller regions for subsequent transmission electron microscope (TEM) examination. However, Ga(+) FIB material removal rates limit the volumes and depths that can be probed to dimensions in the tens of microns range. Emerging Xe(+) Plasma Focused Ion Beam-Scanning Electron Microscope (PFIB-SEM) systems promise faster removal rates. Here we examine the potential of the method for large volume serial section tomography as applied to bainitic steel and WC-Co hard metals. Our studies demonstrate that with careful control of milling parameters precise automated serial sectioning can be achieved with low levels of milling artefacts at removal rates some 60× faster. Volumes that are hundreds of microns in dimension have been collected using fully automated SST routines in feasible timescales (<24h) showing good grain orientation contrast and capturing microstructural features at the tens of nanometres to the tens of microns scale. Accompanying electron back scattered diffraction (EBSD) maps show high indexing rates suggesting low levels of surface damage. Further, under high current Ga(+) FIB milling WC-Co is prone to amorphisation of WC surface layers and phase transformation of the Co phase, neither of which have been observed at PFIB currents as high as 60nA at 30kV. Xe(+) PFIB dual beam microscopes promise to radically extend our capability for 3D tomography, 3D EDX, 3D EBSD as well as correlative tomography. Copyright © 2015 The Authors. Published by Elsevier B.V. All rights reserved.

High- and low-Cr chromitite and dunite in a Tibetan ophiolite: evolution from mature subduction system to incipient forearc in the Neo-Tethyan Ocean

NASA Astrophysics Data System (ADS)

Xiong, Qing; Henry, Hadrien; Griffin, William L.; Zheng, Jian-Ping; Satsukawa, Takako; Pearson, Norman J.; O'Reilly, Suzanne Y.

2017-06-01

The microstructures, major- and trace-element compositions of minerals and electron backscattered diffraction (EBSD) maps of high- and low-Cr# [spinel Cr# = Cr3+/(Cr3+ + Al3+)] chromitites and dunites from the Zedang ophiolite in the Yarlung Zangbo Suture (South Tibet) have been used to reveal their genesis and the related geodynamic processes in the Neo-Tethyan Ocean. The high-Cr# (0.77-0.80) chromitites (with or without diopside exsolution) have chromite compositions consistent with initial crystallization by interaction between boninitic magmas, harzburgite and reaction-produced magmas in a shallow, mature mantle wedge. Some high-Cr# chromitites show crystal-plastic deformation and grain growth on previous chromite relics that have exsolved needles of diopside. These features are similar to those of the Luobusa high-Cr# chromitites, possibly recycled from the deep upper mantle in a mature subduction system. In contrast, mineralogical, chemical and EBSD features of the Zedang low-Cr# (0.49-0.67) chromitites and dunites and the silicate inclusions in chromite indicate that they formed by rapid interaction between forearc basaltic magmas (MORB-like but with rare subduction input) and the Zedang harzburgites in a dynamically extended, incipient forearc lithosphere. The evidence implies that the high-Cr# chromitites were produced or emplaced in an earlier mature arc (possibly Jurassic), while the low-Cr# associations formed in an incipient forearc during the initiation of a new episode of Neo-Tethyan subduction at 130-120 Ma. This two-episode subduction model can provide a new explanation for the coexistence of high- and low-Cr# chromitites in the same volume of ophiolitic mantle.

DOE Office of Scientific and Technical Information (OSTI.GOV)

Kutes, Yasemin; Luria, Justin; Sun, Yu

Ion beam milling is the most common modern method for preparing specific features for microscopic analysis, even though concomitant ion implantation and amorphization remain persistent challenges, particularly as they often modify materials properties of interest. Atomic force microscopy (AFM), on the other hand, can mechanically mill specific nanoscale regions in plan-view without chemical or high energy ion damage, due to its resolution, directionality, and fine load control. As an example, AFM-nanomilling (AFM-NM) is implemented for top-down planarization of polycrystalline CdTe thin film solar cells, with a resulting decrease in the root mean square (RMS) roughness by an order of magnitude,more » even better than for a low incidence FIB polished surface. Subsequently AFM-based property maps reveal a substantially stronger contrast, in this case of the short-circuit current or open circuit voltage during light exposure. Furthermore, electron back scattering diffraction (EBSD) imaging also becomes possible upon AFM-NM, enabling direct correlations between the local materials properties and the polycrystalline microstructure. Smooth shallow-angle cross-sections are demonstrated as well, based on targeted oblique milling. As expected, this reveals a gradual decrease in the average short-circuit current and maximum power as the underlying CdS and electrode layers are approached, but a relatively consistent open-circuit voltage through the diminishing thickness of the CdTe absorber. AFM-based nanomilling is therefore a powerful tool for material characterization, uniquely providing ion-damage free, selective area, planar smoothing or low-angle sectioning of specimens while preserving their functionality. This then enables novel, co-located advanced AFM measurements, EBSD analysis, and investigations by related techniques that are otherwise hindered by surface morphology or surface damage.« less

Electron Microscopy Characterization of Vanadium Dioxide Thin Films and Nanoparticles

NASA Astrophysics Data System (ADS)

Rivera, Felipe

Vanadium dioxide (VO_2) is a material of particular interest due to its exhibited metal to insulator phase transition at 68°C that is accompanied by an abrupt and significant change in its electronic and optical properties. Since this material can exhibit a reversible drop in resistivity of up to five orders of magnitude and a reversible drop in infrared optical transmission of up to 80%, this material holds promise in several technological applications. Solid phase crystallization of VO_2 thin films was obtained by a post-deposition annealing process of a VO_{x,x approx 2} amorphous film sputtered on an amorphous silicon dioxide (SiO_2) layer. Scanning electron microscopy (SEM) and electron-backscattered diffraction (EBSD) were utilized to study the morphology of the solid phase crystallization that resulted from this post-deposition annealing process. The annealing parameters ranged in temperature from 300°C up to 1000°C and in time from 5 minutes up to 12 hours. Depending on the annealing parameters, EBSD showed that this process yielded polycrystalline vanadium dioxide thin films, semi-continuous thin films, and films of isolated single-crystal particles. In addition to these films on SiO_2, other VO_2 thin films were deposited onto a-, c-, and r-cuts of sapphire and on TiO_2(001) heated single-crystal substrates by pulsed-laser deposition (PLD). The temperature of the substrates was kept at ˜500°C during deposition. EBSD maps and orientation imaging microscopy were used to study the epitaxy and orientation of the VO_2 grains deposited on the single crystal substrates, as well as on the amorphous SiO_2 layer. The EBSD/OIM results showed that: 1) For all the sapphire substrates analyzed, there is a predominant family of crystallographic relationships wherein the rutile VO_2{001} planes tend to lie parallel to the sapphire's {10-10} and the rutile VO_2{100} planes lie parallel to the sapphire's {1-210} and {0001}. Furthermore, while this family of relationships accounts for the majority of the VO_2 grains observed, due to the sapphire substrate's geometry there were variations within these rules that changed the orientation of VO_2 grains with respect to the substrate's normal direction. 2) For the TiO_2, a substrate with a lower lattice mismatch, we observe the expected relationship where the rutile VO_2 [100], [110], and [001] crystal directions lie parallel to the TiO_2 substrate's [100], [110], and [001] crystal directions respectively. 3) For the amorphous SiO_2 layer, all VO_2 crystals that were measurable (those that grew to the thickness of the deposited film) had a preferred orientation with the the rutile VO_2[001] crystal direction tending to lie parallel to the plane of the specimen. The use of transmission electron microscopy (TEM) is presented as a tool for further characterization studies of this material and its applications. In this work TEM diffraction patterns taken from cross-sections of particles of the a- and r-cut sapphire substrates not only solidified the predominant family mentioned, but also helped lift the ambiguity present in the rutile VO_2{100} axes. Finally, a focused-ion beam technique for preparation of cross-sectional TEM samples of metallic thin films deposited on polymer substrates is demonstrated.

Stress Concentration and Fracture at Inter-variant Boundaries in an Al-Li Alloy

NASA Technical Reports Server (NTRS)

Crooks, Roy; Tayon, Wes; Domack, Marcia; Wagner, John; Beaudoin, Armand

2009-01-01

Delamination fracture has limited the use of lightweight Al-Li alloys. Studies of secondary, delamination cracks in alloy 2090, L-T fracture toughness samples showed grain boundary failure between variants of the brass texture component. Although the adjacent texture variants, designated B(sub s1) and B(sub s2), behave similarly during rolling, their plastic responses to mechanical tests can be quite different. EBSD data from through-thickness scans were used to generate Taylor factor maps. When a combined boundary normal and shear tensor was used in the calculation, the delaminating grains showed the greatest Taylor Factor differences of any grain pairs. Kernel Average Misorientation (KAM) maps also showed damage accumulation on one side of the interface. Both of these are consistent with poor slip accommodation from a crystallographically softer grain to a harder one. Transmission electron microscopy was used to confirm the EBSD observations and to show the role of slip bands in the development of large, interfacial stress concentrations. A viewgraph presentation accompanies the provided abstract.

Reconstruction of the 3-D Shape and Crystal Preferred Orientation of Olivine: A Combined X-ray µ-CT and EBSD-SEM approach

NASA Astrophysics Data System (ADS)

Kahl, Wolf-Achim; Hidas, Károly; Dilissen, Nicole; Garrido, Carlos J.; López-Sánchez Vizcaíno, Vicente; Jesús Román-Alpiste, Manuel

2017-04-01

The complete reconstruction of the microstructure of rocks requires, among others, a full description of the shape preferred orientation (SPO) and crystal preferred orientation (CPO) of the constituent mineral phases. New advances in instrumental analyses, particularly electron backscatter diffraction (EBSD) coupled to focused ion beam-scanning electron microscope (FIB-SEM), allows a complete characterization of SPO and CPO in rocks at the micron scale [1-2]. Unfortunately, the large grain size of many crystalline rocks, such as peridotite, prevents a representative characterization of the CPO and SPO of their constituent minerals by this technique. Here, we present a new approach combining X-ray micro computed tomography (µ-CT) and EBSD to reconstruct the geographically oriented, 3-D SPO and CPO of cm- to mm-sized olivine crystals in two contrasting fabric types of chlorite harzburgites (Almírez ultramafic massif, SE Spain). The semi-destructive sample treatment involves drilling of geographically oriented micro drills in the field and preparation of oriented thin sections from µ-CT scanned cores. This allows for establishing the link among geological structures, macrostructure, fabric, and 3-D SPO-CPO at the thin section scale. Based on EBSD analyses, different CPO groups of olivine crystals can be discriminated in the thin sections and allocated to 3-D SPO in the µ-CT volume data. This approach overcomes the limitations of both methods (i.e., no crystal orientation data in µ-CT and no spatial information in EBSD), hence 3-D orientation of the crystallographic axes of olivines from different orientation groups could be correlated with the crystal shapes of olivine grains. This combined µ-CT and EBSD technique enables the correlation of both SPO and CPO and representative grain size, and is capable to characterize the 3-D microstructure of olivine-bearing rocks at the hand specimen scale. REFERENCES 1. Zaefferer, S., Wright, S.I., Raabe, D., 2008. Three-Dimensional orientation microscopy in a focused ion beam-scanning electron microscope: A new dimension of microstructure characterization. Metallurgical and Materials Transactions A 39, 374-389. 2. Burnett, T.L., Kelley, R., Winiarski, B., Contreras, L., Daly, M., Gholinia, A., Burke, M.G., Withers, P.J., 2016. Large volume serial section tomography by Xe Plasma FIB dual beam microscopy. Ultramicroscopy 161, 119-129.

Microstructural characterization of hydrogen induced cracking in TRIP-assisted steel by EBSD

DOE Office of Scientific and Technical Information (OSTI.GOV)

Laureys, A., E-mail: Aurelie.Laureys@UGent.be; Depover, T.; Petrov, R.

2016-02-15

The present work evaluates hydrogen induced cracking by performing an elaborate EBSD (Electron BackScatter Diffraction) study in a steel with transformation induced plasticity (TRIP-assisted steel). This type of steel exhibits a multiphase microstructure which undergoes a deformation induced phase transformation. Additionally, each microstructural constituent displays a different behavior in the presence of hydrogen. The aim of this study is to obtain a better understanding on the mechanisms governing hydrogen induced crack initiation and propagation in the hydrogen saturated multiphase structure. Tensile tests on notched samples combined with in-situ electrochemical hydrogen charging were conducted. The tests were interrupted at stresses justmore » after reaching the tensile strength, i.e. before macroscopic failure of the material. This allowed to study hydrogen induced crack initiation and propagation by SEM (Scanning Electron Microscopy) and EBSD. A correlation was found between the presence of martensite, which is known to be very susceptible to hydrogen embrittlement, and the initiation of hydrogen induced cracks. Initiation seems to occur mostly by martensite decohesion. High strain regions surrounding the hydrogen induced crack tips indicate that further crack propagation may have occurred by the HELP (hydrogen-enhanced localized plasticity) mechanism. Small hydrogen induced cracks located nearby the notch are typically S-shaped and crack propagation was dominantly transgranularly. The second stage of crack propagation consists of stepwise cracking by coalescence of small hydrogen induced cracks. - Highlights: • Hydrogen induced cracking in TRIP-assisted steel is evaluated by EBSD. • Tensile tests were conducted on notched hydrogen saturated samples. • Crack initiation occurs by a H-Enhanced Interface DEcohesion (HEIDE) mechanism. • Crack propagation involves growth and coalescence of small cracks. • Propagation is governed by the characteristics of phases on the crack path.« less

On the bulk degradation of yttria-stabilized nanocrystalline zirconia dental implant abutments: an electron backscatter diffraction study.

PubMed

Ocelík, V; Schepke, U; Rasoul, H Haji; Cune, M S; De Hosson, J Th M

2017-08-01

Degradation of yttria-stabilized zirconia dental implants abutments due to the tetragonal to monoclinic phase transformation was studied in detail by microstructural characterization using Electron Back Scatter Diffraction (EBSD). The amount and distribution of the monoclinic phase, the grain-size distribution and crystallographic orientations between tetragonal and monoclinic crystals in 3 mol.% yttria-stabilized polycrystalline zirconia (3Y-TZP) were determined in two different types of nano-crystalline dental abutments, even for grains smaller than 400 nm. An important and novel conclusion is that no substantial bulk degradation of 3Y-TZP dental implant abutments was detected after 1 year of clinical use.

Insights to Meteorites and Impact Processes provided by Advanced EBSD Analysis

NASA Astrophysics Data System (ADS)

Palasse, Laurie; Berlin, Jana; Goran, Daniel; Tagle, Roald; Hamers, Maartje; Assis Fernandes, Vera; Deutsch, Alexander; Schulte, Peter; Salge, Tobias

2013-04-01

Electron backscatter diffraction (EBSD) is a powerful analytical technique for assessing the petrographic texture of rocks and the crystallographic orientation of minerals therein using a scanning electron microscope (SEM). Innovations in EBSD technology include colour-coded forescattered electron (FSE) images, high resolution and highly sensitive EBSD detectors, together with advanced EDS integration. It allows to accurately identify and discriminate different phases, and to investigate microstructures related to shock metamorphism. As an example, shocked carbonates and shocked quartz reveal a complex thermal history during post-shock cooling. (A) EBSD studies of calcite ejecta particles from the Chicxulub impact event, at the K-Pg boundary of El Guayal, Mexico (~520 km SW of the Chicxulub crater centre) display various microstructures [1] and spherulitic calcite ejecta particles reveal a fibre texture of elongated crystals with a preferred orientation. This indicates the presence of carbonate melts which were ejected at T>1240°C and P>40 bar from upper target lithologies and crystallized at cooling rates of ~100´s °C/s [2]. The calcite particles of El Guayal and the K/Pg boundary of La Lajilla (~1000 km W of the crater centre) show distinct microstructures represented by unoriented, equiaxed crystals with random orientation distribution. It documents recrystallization upon impact induced thermal stress at T>550°C during prolonged atmospheric transport. (B) Combined EBSD, FSE and cathodoluminescence (CL) studies of semi-amorphous shocked quartz of Chicxulub, Ries and Popigai impactites, reveal various microstructures. Colour-coded FSE imaging reveal recrystallized/deformed bands in Ries and Popigai samples indicative of planar deformation features. EBSD studies of Popigai allow to distinguish twinned Qz, α-Qz and α-cristobalite along the transition zone between shocked gneiss clast and impact melt. Recrystallized Qz grains are associated with amorphous SiO2. For Chicxulub, the brecciated impact melt rock from borehole Yaxcopoil-1 (Unit 5, 861.72 m) [3] reveals that the ballen microstructure is only semi-amorphous and cross cuts a fine grained recrystallised microstructure. (C) CB chondrite Gujba: EDS and EBSD data were acquired simultaneously to study chemical and physical interactions between preexisting metal particles and the invading silicate-rich impact melt matrix. Metal particles appear to have different thermal histories. Some of them consist of many small grains (average diameter ~10 µm), which have a similar orientation when they are surrounded by arcuate Fe,Cr-sulfides. [4]. Acknowledgements: P. Claeys, R.H. Jones, ICDP and the Museum of Natural History Berlin for providing samples. References: [1] T. Salge (2007) PhD thesis, Humboldt Universität zu Berlin, 130p. [2] A. P. Jones et al. (2000) Lect. Notes in Earth Sciences 91: 343-361. [3] M. J. Nelson et al. (2012) GCA 86: 1-20. [4]. J. Berlin et al. (2013) 44th LPSC # 2439

Discontinuous precipitation in a nickel-free high nitrogen austenitic stainless steel on solution nitriding

NASA Astrophysics Data System (ADS)

Mohammadzadeh, Roghayeh; Akbari, Alireza; Grumsen, Flemming B.; Somers, Marcel A. J.

2017-10-01

Chromium-rich nitride precipitates in production of nickel-free austenitic stainless steel plates via pressurised solution nitriding of Fe-22.7Cr-2.4Mo ferritic stainless steel at 1473 K (1200 °C) under a nitrogen gas atmosphere was investigated. The microstructure, chemical and phase composition, morphology and crystallographic orientation between the resulted austenite and precipitates were investigated using optical microscopy, X-ray Diffraction (XRD), Scanning and Transmission Electron Microscopy (TEM) and Electron Back Scatter Diffraction (EBSD). On prolonged nitriding, Chromium-rich nitride precipitates were formed firstly close to the surface and later throughout the sample with austenitic structure. Chromium-rich nitride precipitates with a rod or strip-like morphology was developed by a discontinuous cellular precipitation mechanism. STEM-EDS analysis demonstrated partitioning of metallic elements between austenite and nitrides, with chromium contents of about 80 wt.% in the precipitates. XRD analysis indicated that the Chromium-rich nitride precipitates are hexagonal (Cr, Mo)2N. Based on the TEM studies, (Cr, Mo)2N precipitates presented a (1 1 1)γ//(0 0 2)(Cr, Mo)2N, ?γ//?(Cr, Mo)2N orientation relationship with respect to the austenite matrix. EBSD studies revealed that the austenite in the regions that have transformed into austenite and (Cr, Mo)2N have no orientation relation to the untransformed austenite.

Crack nucleation using combined crystal plasticity modelling, high-resolution digital image correlation and high-resolution electron backscatter diffraction in a superalloy containing non-metallic inclusions under fatigue

PubMed Central

Zhang, Tiantian; Britton, Ben; Shollock, Barbara; Dunne, Fionn

2016-01-01

A crystal plasticity finite-element model, which explicitly and directly represents the complex microstructures of a non-metallic agglomerate inclusion within polycrystal nickel alloy, has been developed to study the mechanistic basis of fatigue crack nucleation. The methodology is to use the crystal plasticity model in conjunction with direct measurement at the microscale using high (angular) resolution-electron backscatter diffraction (HR-EBSD) and high (spatial) resolution-digital image correlation (HR-DIC) strain measurement techniques. Experimentally, this sample has been subjected to heat treatment leading to the establishment of residual (elastic) strains local to the agglomerate and subsequently loaded under conditions of low cyclic fatigue. The full thermal and mechanical loading history was reproduced within the model. HR-EBSD and HR-DIC elastic and total strain measurements demonstrate qualitative and quantitative agreement with crystal plasticity results. Crack nucleation by interfacial decohesion at the nickel matrix/agglomerate inclusion boundaries is observed experimentally, and systematic modelling studies enable the mechanistic basis of the nucleation to be established. A number of fatigue crack nucleation indicators are also assessed against the experimental results. Decohesion was found to be driven by interface tensile normal stress alone, and the interfacial strength was determined to be in the range of 1270–1480 MPa. PMID:27279765

Crack nucleation using combined crystal plasticity modelling, high-resolution digital image correlation and high-resolution electron backscatter diffraction in a superalloy containing non-metallic inclusions under fatigue

NASA Astrophysics Data System (ADS)

Zhang, Tiantian; Jiang, Jun; Britton, Ben; Shollock, Barbara; Dunne, Fionn

2016-05-01

A crystal plasticity finite-element model, which explicitly and directly represents the complex microstructures of a non-metallic agglomerate inclusion within polycrystal nickel alloy, has been developed to study the mechanistic basis of fatigue crack nucleation. The methodology is to use the crystal plasticity model in conjunction with direct measurement at the microscale using high (angular) resolution-electron backscatter diffraction (HR-EBSD) and high (spatial) resolution-digital image correlation (HR-DIC) strain measurement techniques. Experimentally, this sample has been subjected to heat treatment leading to the establishment of residual (elastic) strains local to the agglomerate and subsequently loaded under conditions of low cyclic fatigue. The full thermal and mechanical loading history was reproduced within the model. HR-EBSD and HR-DIC elastic and total strain measurements demonstrate qualitative and quantitative agreement with crystal plasticity results. Crack nucleation by interfacial decohesion at the nickel matrix/agglomerate inclusion boundaries is observed experimentally, and systematic modelling studies enable the mechanistic basis of the nucleation to be established. A number of fatigue crack nucleation indicators are also assessed against the experimental results. Decohesion was found to be driven by interface tensile normal stress alone, and the interfacial strength was determined to be in the range of 1270-1480 MPa.

Electron backscatter diffraction studies of focused ion beam induced phase transformation in cobalt

DOE Office of Scientific and Technical Information (OSTI.GOV)

Jones, H.G., E-mail: helen.jones@npl.co.uk

A focused ion beam microscope was used to induce cubic to hexagonal phase transformation in a cobalt alloy, of similar composition to that of the binder phase in a hardmetal, in a controlled manner at 0°, 45° and 80° ion incident angles. The cobalt had an average grain size of ~ 20 μm, allowing multiple orientations to be studied, exposed to a range of doses between 6 × 10{sup 7} and 2 × 10{sup 10} ions/μm{sup 2}. Electron backscatter diffraction (EBSD) was used to determine the original and induced phase orientations, and area fractions, before and after the ion beammore » exposure. On average, less phase transformation was observed at higher incident angles and after lower ion doses. However there was an orientation effect where grains with an orientation close to (111) planes were most susceptible to phase transformation, and (101) the least, where grains partially and fully transformed at varying ion doses. - Highlights: •Ion-induced phase change in FCC cobalt was observed at multiple incidence angles. •EBSD was used to study the relationship between grain orientation and transformation. •Custom software analysed ion dose and phase change with respect to grain orientation. •A predictive capability of ion-induced phase change in cobalt was enabled.« less

Effect of hydrogenation conditions on the microstructure and mechanical properties of zirconium hydride

NASA Astrophysics Data System (ADS)

Muta, Hiroaki; Nishikane, Ryoji; Ando, Yusuke; Matsunaga, Junji; Sakamoto, Kan; Harjo, Stefanus; Kawasaki, Takuro; Ohishi, Yuji; Kurosaki, Ken; Yamanaka, Shinsuke

2018-03-01

Precipitation of brittle zirconium hydrides deteriorate the fracture toughness of the fuel cladding tubes of light water reactor. Although the hydride embrittlement has been studied extensively, little is known about physical properties of the hydride due to the experimental difficulties. In the present study, to elucidate relationship between mechanical properties and microstructure, two δ-phase zirconium hydrides and one ε-phase zirconium hydride were carefully fabricated considering volume changes at the metal-to-hydride transformation. The δ-hydride that was fabricated from α-zirconium exhibits numerous inner cracks due to the large volume change. Analyses of the neutron diffraction pattern and electron backscatter diffraction (EBSD) data show that the sample displays significant stacking faults in the {111} plane and in the pseudo-layered microstructure. On the other hand, the δ-hydride sample fabricated from β-zirconium at a higher temperature displays equiaxed grains and no cracks. The strong crystal orientation dependence of mechanical properties were confirmed by indentation test and EBSD observation. The δ-hydride hydrogenated from α-zirconium displays a lower Young's modulus than that prepared from β-zirconium. The difference is attributed to stacking faults within the {111} plane, for which the Young's modulus exhibits the highest value in the perpendicular direction. The strong influence of the crystal orientation and dislocation density on the mechanical properties should be considered when evaluating hydride precipitates in nuclear fuel cladding.

A multimodal microcharacterisation of trace-element zonation and crystallographic orientation in natural cassiterite by combining cathodoluminescence, EBSD, EPMA and contribution of confocal Raman-in-SEM imaging.

PubMed

Wille, G; Lerouge, C; Schmidt, U

2018-01-16

In cassiterite, tin is associated with metals (titanium, niobium, tantalum, indium, tungsten, iron, manganese, mercury). Knowledge of mineral chemistry and trace-element distribution is essential for: the understanding of ore formation, the exploration phase, the feasibility of ore treatment, and disposal/treatment of tailings after the exploitation phase. However, the availability of analytical methods make these characterisations difficult. We present a multitechnical approach to chemical and structural data that includes scanning electron microscopy (SEM)-based imaging and microanalysis techniques such as: secondary and backscattered electrons, cathodoluminescence (CL), electron probe microanalyser (EPMA), electron backscattered diffraction (EBSD) and confocal Raman-imaging integrated in a SEM (RISE). The presented results show the complementarity of the used analytical techniques. SEM, CL, EBSD, EPMA provide information from the interaction of an electron beam with minerals, leading to atomistic information about their composition, whereas RISE, Raman spectroscopy and imaging completes the studies with information about molecular vibrations, which are sensitive to structural modifications of the minerals. The correlation of Raman bands with the presence/absence of Nb, Ta, Fe (heterovalent substitution) and Ti (homovalent substitution) is established at a submicrometric scale. Combination of the different techniques makes it possible to establish a direct link between chemical and crystallographic data of cassiterite. © 2018 The Authors Journal of Microscopy © 2018 Royal Microscopical Society.

Studies on microstructure, mechanical and corrosion properties of high nitrogen stainless steel shielded metal arc welds

NASA Astrophysics Data System (ADS)

Mohammed, Raffi; Madhusudhan Reddy, G.; Srinivasa Rao, K.

2018-03-01

The present work is aimed at studying the microstructure, mechanical and corrosion properties of high nitrogen stainless steel shielded metal arc (SMA) welds made with Cromang-N electrode. Basis for selecting this electrode is to increase the solubility of nitrogen in weld metal due to high chromium and manganese content. Microstructures of the welds were characterized using optical microscopy (OM), field emission scanning electron microscopy (FESEM) and electron back scattered diffraction (EBSD) mainly to determine the morphology, phase analysis, grain size and orientation image mapping. Hardness, tensile and ductility bend tests were carried out to determine mechanical properties. Potentio-dynamic polarization testing was carried out to study the pitting corrosion resistance using a GillAC basic electrochemical system. Constant load type testing was carried out to study stress corrosion cracking (SCC) behaviour of welds. The investigation results shown that the selected Cr–Mn–N type electrode resulted in favourable microstructure and completely solidified as single phase coarse austenite. Mechanical properties of SMA welds are found to be inferior when compared to that of base metal and is due to coarse and dendritic structure.

Electromigration and Thermomechanical Fatigue Behavior of Sn0.3Ag0.7Cu Solder Joints

NASA Astrophysics Data System (ADS)

Zuo, Yong; Bieler, Thomas R.; Zhou, Quan; Ma, Limin; Guo, Fu

2017-12-01

The anisotropy of Sn crystal structures greatly affects the electromigration (EM) and thermomechanical fatigue (TMF) of solder joints. The size of solder joint shrinkage in electronic systems further makes EM and TMF an inseparably coupled issue. To obtain a better understanding of failure under combined moderately high (2000 A/cm2) current density and 10-150°C/1 h thermal cycling, analysis of separate, sequential, and concurrent EM and thermal cycling (TC) was imposed on single shear lap joints, and the microstructure and crystal orientations were incrementally characterized using electron backscatter diffraction (EBSD) mapping. First, it was determined that EM did not significantly change the crystal orientation, but the formation of Cu6Sn5 depended on the crystal orientation, and this degraded subsequent TMF behavior. Secondly, TC causes changes in crystal orientation. Concurrent EM and TC led to significant changes in crystal orientation by discontinuous recrystallization, which is facilitated by Cu6Sn5 particle formation. The newly formed Cu6Sn5 often showed its c-axis close to the direction of electron flow.

EBSD characterization of twinning in cold-rolled CP-Ti

DOE Office of Scientific and Technical Information (OSTI.GOV)

Li, X., E-mail: csulixu@hotmail.com; Duan, Y.L., E-mail: 876270744@qq.com; Xu, G.F., E-mail: csuxgf66@csu.edu.cn

2013-10-15

This work presents the use of a mechanical testing system and the electron backscatter diffraction technique to study the mechanical properties and twinning systems of cold-rolled commercial purity titanium, respectively. The dependence of twinning on the matrix orientation is analyzed by the distribution map of Schmid factor. The results showed that the commercial purity titanium experienced strong strain hardening and had excellent formability during rolling. Both the (112{sup ¯}2)<112{sup ¯}3{sup ¯}> compressive twins and (101{sup ¯}2)<101{sup ¯}1{sup ¯}> tensile twins were dependent on the matrix orientation. The Schmid factor of a grain influenced the activation of a particular twinning system.more » The specific rolling deformation of commercial purity titanium controlled the number and species of twinning systems and further changed the mechanical properties. - Highlights: • CP-Ti experienced strain hardening and had excellent formability. • Twins were dependent on the matrix orientation. • Schmid factor of a grain influenced the activation of a twinning system. • Rolling deformation controlled twinning systems and mechanical properties.« less

Electromigration and Thermomechanical Fatigue Behavior of Sn0.3Ag0.7Cu Solder Joints

NASA Astrophysics Data System (ADS)

Zuo, Yong; Bieler, Thomas R.; Zhou, Quan; Ma, Limin; Guo, Fu

2018-03-01

The anisotropy of Sn crystal structures greatly affects the electromigration (EM) and thermomechanical fatigue (TMF) of solder joints. The size of solder joint shrinkage in electronic systems further makes EM and TMF an inseparably coupled issue. To obtain a better understanding of failure under combined moderately high (2000 A/cm2) current density and 10-150°C/1 h thermal cycling, analysis of separate, sequential, and concurrent EM and thermal cycling (TC) was imposed on single shear lap joints, and the microstructure and crystal orientations were incrementally characterized using electron backscatter diffraction (EBSD) mapping. First, it was determined that EM did not significantly change the crystal orientation, but the formation of Cu6Sn5 depended on the crystal orientation, and this degraded subsequent TMF behavior. Secondly, TC causes changes in crystal orientation. Concurrent EM and TC led to significant changes in crystal orientation by discontinuous recrystallization, which is facilitated by Cu6Sn5 particle formation. The newly formed Cu6Sn5 often showed its c-axis close to the direction of electron flow.

Use of EBSD Data in Numerical Analyses

DOE Office of Scientific and Technical Information (OSTI.GOV)

Becker, R; Wiland, H

2000-01-14

Experimentation, theory and modeling have all played vital roles in defining what is known about microstructural evolution and the effects of microstructure on material properties. Recently, technology has become an enabling factor, allowing significant advances to be made on several fronts. Experimental evidence of crystallographic slip and the basic theory of crystal plasticity were established in the early 20th Century, and the theory and models evolved incrementally over the next 60 years. (Asaro provides a comprehensive review of the mechanisms and basic plasticity models.) During this time modeling was primarily concerned with the average response of polycrystalline aggregates. While somemore » detailed finite element modeling (FEM) with crystal plasticity constitutive relations was done in the early 1980s, such simulations over taxed the capabilities of the available computer hardware. Advances in computer capability led to a flurry of activity in finite element modeling in the next 10 years, increasing understanding of microstructure evolution and pushing the limits of theories and material characterization. Automated Electron Back Scatter Diffraction (EBSD) has produced a similar revolution in material characterization. The data collected is extensive and many questions about the evolution of microstructure and its role in determining mechanic properties can now be addressed. It is also now possible to obtain sufficient information about lattice orientations on a fine enough scale to allow detailed quantitative comparisons of experiments and newly emerging large scale numerical simulations. The insight gained from the coupling of EBSD and FEM studies will provide impetus for further development of microstructure models and theories of microstructure evolution. Early studies connecting EBSD data to finite element models used manual measurements to define initial orientations for the simulation. In one study, manual measurements of the deformed structure were also obtained for comparison with the model predictions. More recent work has taken advantage of automated data collection on deformed specimens as a means of collecting detailed and spatially correlated data for model validation. Although it will not be discussed in detail here, another area in which EBSD data is having a great impact is on recrystallization modeling. EBSD techniques can be used to collect data for quantitative microstructural analysis. This data can be used to infer growth kinetics of specific orientations, and this information can be synthesized into more accurate grain growth or recrystallization models. Another role which EBSD techniques may play is in determining initial structures for recrystallization models. A realistic starting structure is vital for evaluating the models, and attempts at predicting realistic structures with finite element simulations are not yet successful. As methodologies and equipment resolution continue to improve, it is possible that measured structures will serve as input for recrystallization models. Simulations have already been run using information obtained manually from a TEM.« less

Geometrically Necessary Dislocation Density Evolution in Interstitial Free Steel at Small Plastic Strains

NASA Astrophysics Data System (ADS)

Kundu, Amrita; Field, David P.

2018-06-01

Measurement of geometrically necessary dislocation (GND) density using electron backscatter diffraction (EBSD) has become rather common place in modern metallurgical research. The utility of this measure as an indicator of the expected flow behavior of the material is not obvious. Incorporation of total dislocation density into the Taylor equation relating flow stress to dislocation density is generally accepted, but this does not automatically extend to a similar relationship for the GND density. This is discussed in the present work using classical equations for isotropic metal plasticity in a rather straight-forward theoretical framework. This investigation examines the development of GND structure in a commercially produced interstitial free steel subject to tensile deformation. Quantification of GND density was carried out using conventional EBSD at various strain levels on the surface of a standard dog-bone-shaped tensile specimen. There is linear increase of the average GND density with imposed macroscopic strain. This is in agreement with the established framework.

EBSD investigation of the effect of the solidification rate on the nucleation behavior of eutectic components in a hypoeutectic Al-Si-Cu alloy

NASA Astrophysics Data System (ADS)

Mohsen Sadrossadat, S.; Johansson, Sten; Peng, Ru Lin

2012-06-01

This article represents a study of the influence of the solidification rate on the crystallographic orientation of eutectic components with respect to the primary α-Al in the tested hypoeutectic alloy. Electron backscattering diffraction (EBSD) patterns were produced from the Al-Si cast specimens that were solidified with different cooling rates and prepared via ion etch polishing as a complementary method after mechanical polishing. The results indicated a strong orientation relationship between the primary α-Al and eutectic Al phase at all cooling rates. It was also found that the silicon eutectic flakes were heterogeneously nucleated in the interdendritic eutectic liquid. The increase of the cooling rate from 2 to 80 mm/min was found to be effective in lowering the intensity of the relationship between the primary α-Al and eutectic Al phases, and changing the misorientation angle clustering between the primary α-Al and eutectic Si phases in the interval from 41-60° to lower angle intervals.

3D Microstructural Characterization of Uranium Oxide as a Surrogate Nuclear Fuel: Effect of Oxygen Stoichiometry on Grain Boundary Distributions

DOE Office of Scientific and Technical Information (OSTI.GOV)

Rudman, K.; Dickerson, P.; Byler, Darrin David

The initial microstructure of an oxide fuel can play a key role in its performance. At low burn-ups, the diffusion of fission products can depend strongly on grain size and grain boundary (GB) characteristics, which in turn depend on processing conditions and oxygen stoichiometry. Serial sectioning techniques using Focused Ion Beam were developed to obtain Electron Backscatter Diffraction (EBSD) data for depleted UO2 pellets that were processed to obtain 3 different oxygen stoichiometries. The EBSD data were used to create 3D microstructure reconstructions and to gather statistical information on the grain and GB crystallography, with emphasis on identifying the charactermore » (twist, tilt, mixed) for GBs that meet the Coincident Site Lattice (CSL) criterion as well as GBs with the most common misorientation angles. Data on dihedral angles at triple points were also collected. The results were compared across different samples to understand effects of oxygen content on microstructure evolution.« less

Investigation of Microstructural Features Determining the Toughness of 980 MPa Bainitic Weld Metal

NASA Astrophysics Data System (ADS)

Cao, R.; Zhang, X. B.; Wang, Z.; Peng, Y.; Du, W. S.; Tian, Z. L.; Chen, J. H.

2014-02-01

The microstructural features that control the impact toughness of weld metals of a 980 MPa 8 pct Ni high-strength steel are investigated using instrumented Charpy V tester, optical microscope (OM), scanning electron microscope (SEM), transmission electron microscope (TEM), electron back-scattered diffraction (EBSD), and finite-element method (FEM) calculation. The results show that the critical event for cleavage fracture in this high-strength steel and weld metals is the propagation of a bainite packet-sized crack across the packet boundary into contiguous packets, and the bainitic packet sizes control the impact toughness. The high-angle misorientation boundaries detected in a bainite packet by EBSD form fine tear ridges on fracture surfaces. However, they are not the decisive factors controlling the cleavage fracture. The effects of Ni content are essential factors for improving the toughness. The extra large cleavage facets seriously deteriorate the toughness, which are formed on the interfaces of large columnar crystals growing in welding pools with high heat input.

Deformation Characteristics and Recrystallization Response of a 9310 Steel Alloy

NASA Astrophysics Data System (ADS)

Snyder, David; Chen, Edward Y.; Chen, Charlie C.; Tin, Sammy

2013-01-01

The flow behavior and recrystallization response of a 9310 steel alloy deformed in the ferrite temperature range were studied in this work. Samples were compressed under various conditions of strain (0.6, 0.8 and multi-axial), strain rate (10-4 seconds-1 to 10-1 seconds-1) and temperature [811 K to 1033 K (538 °C to 760 °C)] using a Gleeble thermo-mechanical simulator. Deformation was characterized by both qualitative and quantitative means, using standard microscopy, electron backscatter diffraction (EBSD) analysis and flow stress modeling. The results indicate that deformation is primarily accommodated through dynamic recovery in sub-grain formation. EBSD analysis shows a continuous increase in sub-grain boundary misorientation with increasing strain, ultimately producing recrystallized grains from the sub-grains at high strains. This suggests that a sub-grain rotation recrystallization mechanism predominates in this temperature range. Analyses of the results reveal a decreasing mean dynamically recrystallized grain size with increasing Zener-Hollomon parameter, and an increasing recrystallized fraction with increasing strain.

A Study of Submicron Grain Boundary Precipitates in Ultralow Carbon 316LN Steels

NASA Astrophysics Data System (ADS)

Downey, S.; Han, K.; Kalu, P. N.; Yang, K.; Du, Z. M.

2010-04-01

This article reports our efforts in characterization of an ultralow carbon 316LN-type stainless steel. The carbon content in the material is one-third that in a conventional 316LN, which further inhibits the formation of grain boundary carbides and therefore sensitizations. Our primary effort is focused on characterization of submicron size precipitates in the materials with the electron backscatter diffraction (EBSD) technique complemented by Auger electron spectroscopy (AES). Thermodynamic calculations suggested that several precipitates, such as M23C6, Chi, Sigma, and Cr2N, can form in a low carbon 316LN. In the steels heat treated at 973 K (700 °C) for 100 hours, a combination of EBSD and AES conclusively identified the grain boundary precipitates (≥100 nm) as Cr2N, which has a hexagonal closed-packed crystallographic structure. Increases of the nitrogen content promote formation of large size Cr2N precipitates. Therefore, prolonged heat treatment at relatively high temperatures of ultralow carbon 316LN steels may result in a sensitization.

Use of reciprocal lattice layer spacing in electron backscatter diffraction pattern analysis

PubMed

Michael; Eades

2000-03-01

In the scanning electron microscope using electron backscattered diffraction, it is possible to measure the spacing of the layers in the reciprocal lattice. These values are of great use in confirming the identification of phases. The technique derives the layer spacing from the higher-order Laue zone rings which appear in patterns from many materials. The method adapts results from convergent-beam electron diffraction in the transmission electron microscope. For many materials the measured layer spacing compares well with the calculated layer spacing. A noted exception is for higher atomic number materials. In these cases an extrapolation procedure is described that requires layer spacing measurements at a range of accelerating voltages. This procedure is shown to improve the accuracy of the technique significantly. The application of layer spacing measurements in EBSD is shown to be of use for the analysis of two polytypes of SiC.

Characterization of ultrafine grained Cu-Ni-Si alloys by electron backscatter diffraction

NASA Astrophysics Data System (ADS)

Altenberger, I.; Kuhn, H. A.; Gholami, M.; Mhaede, M.; Wagner, L.

2014-08-01

A combination of rotary swaging and optimized precipitation hardening was applied to generate ultra fine grained (UFG) microstructures in low alloyed high performance Cu-based alloy CuNi3Si1Mg. As a result, ultrafine grained (UFG) microstructures with nanoscopically small Ni2Si-precipitates exhibiting high strength, ductility and electrical conductivity can be obtained. Grain boundary pinning by nano-precipitates enhances the thermal stability. Electron channeling contrast imaging (ECCI) and especially electron backscattering diffraction (EBSD) are predestined to characterize the evolving microstructures due to excellent resolution and vast crystallographic information. The following study summarizes the microstructure after different processing steps and points out the consequences for the most important mechanical and physical properties such as strength, ductility and conductivity.

Strain distribution across a partially molten middle crust: Insights from the AMS mapping of the Carlos Chagas Anatexite, Araçuaí belt (East Brazil)

NASA Astrophysics Data System (ADS)

Cavalcante, Geane C. G.; Egydio-Silva, Marcos; Vauchez, Alain; Camps, Pierre; Oliveira, Eurídice

2013-10-01

The easternmost part of the Neoproterozoic Araçuaí belt comprises an anatectic domain that involves anatexites (the Carlos Chagas unit), leucogranites and migmatitic granulites that display a well-developed fabric. Microstructural observations support that the deformation occurred in the magmatic to submagmatic state. Structural mapping integrating field and anisotropy of magnetic susceptibility (AMS) revealed a complex, 3D structure. The northern domain displays gently dipping foliations bearing a NW-trending lineation, southward, the lineation trend progressively rotates to EW then SW and the foliation is gently folded. The eastern domain displays E-W and NE-SW trending foliations with moderate to steeply dips bearing a dominantly NS trending lineation. Magnetic mineralogy investigation suggests biotite as the main carrier of the magnetic susceptibility in the anatexites and ferromagnetic minerals in the granulites. Crystallographic preferred orientation (CPO) measurements using the electron backscatter diffraction (EBSD) technique suggest that the magnetic fabric comes from the crystalline anisotropy of biotite and feldspar grains, especially. The delineation of several structural domains with contrasted flow fabric suggests a 3D flow field involving westward thrusting orthogonal to the belt, northwestward orogen-oblique escape tectonics and NS orogen-parallel flow. This complex deformation pattern may be due to interplay of collision-driven and gravity-driven deformations.

Mineral Replacement Reactions as a Precursor to Strain Localisation: an (HR-)EBSD approach

NASA Astrophysics Data System (ADS)

Gardner, J.; Wheeler, J.; Wallis, D.; Hansen, L. N.; Mariani, E.

2017-12-01

Much remains to be learned about the links between metamorphism and deformation. Our work investigates the behaviour of fluid-mediated mineral replacement reaction products when exposed to subsequent shear stresses. We focus on albite from a metagabbro that has experienced metamorphism and subsequent deformation at greenschist facies, resulting in a reduction in grain size and associated strain localisation. EBSD maps show that prior to grain size reduction, product grains are highly distorted, yet they formed, and subsequently deformed, at temperatures at which extensive dislocation creep is unlikely. The Weighted Burgers Vector can be used to quantitatively describe the types of Burgers vectors present in geometrically necessary dislocation (GND) populations derived from 2-D EBSD map data. Application of this technique to the distorted product grains reveals the prominence of, among others, dislocations with apparent [010] Burgers vectors. This supports (with some caveats) the idea that dislocation creep is not responsible for the observed lattice distortion, as there are no known slip systems in plagioclase with a [010] Burgers vector. Distortion in a replacement microstructure has also been attributed to the presence of nanoscale product grains, which share very similar, but not identical, orientations due to topotactic nucleation from adjacent sites on the same substrate. As a precipitate, the product grains should be expected to be largely free of elastic strain. However, high angular resolution EBSD results demonstrate that product grains contain both elastic strains (> 10-3) and residual stresses (several hundred MPa), as well as GND densities on the order of 1014-1015 m-2. Thus we suggest the observed distortion (elastic strain plus rotations) in the lattice is produced during the mineral replacement reaction by a lattice mismatch and volume change between parent and product. Stored strain energy then provides a driving force for recovery and recrystallization. Recrystallization produces smaller grains with high angle boundaries, reducing the strength of, and allowing deformation to localise in, the albite phase. Grain size reduction in turn facilitates shear deformation to high strains by a grain size sensitive mechanism (fluid-assisted diffusion creep).

Strain analysis in quartzites with negative magnetic susceptibility using AMS and EBSD data

NASA Astrophysics Data System (ADS)

Rajendraprasad Renjith, A.; Mamtani, Manish A.

2016-04-01

This study is being done with the objective of trying to understand whether the anisotropy of magnetic susceptibility (AMS) data can provide information about strain in quartzites with negative magnetic susceptibility. For this, nine quartzite samples have been collected from Rengali Province (located in the eastern part of India) with bulk magnetic susceptibility between -13.6 x 10-6 SI units and -3.06 x 10-6 SI units. Since these rocks did not show any visible foliation or lineation, AMS analysis was performed using KLY-4S Kappabridge and the orientation of three principal axes of the AMS ellipsoid (K1>K2>K3) were determined. Thin sections were prepared parallel to the K1K3 plane of the AMS ellipsoid (plane parallel to lineation and perpendicular to foliation), which is equivalent to the XZ plane of the strain ellipsoid. SEM based electron backscatter diffraction (EBSD) analysis, shape preferred orientation (SPO) analysis and strain analysis were carried out in these sections. Recently, Renjith et al. (2016) used the same samples to establish that the AMS in quartzites gives information about the SPO and not the CPO. To further evaluate the robustness of AMS in strain analysis, the authors have integrated the degree of magnetic anisotropy (Pj - a measure of the eccentricity of AMS ellipsoid; Tarling and Hrouda, 1993) with the intensity of SPO (κ ; Piazolo and Passchier, 2002), and the strain (E - calculated using AMOCADO; Gerik and Kruhl, 2009) from the same samples from Rengali. EBSD data were used as the basis for the above calculations. Whilst the orientation of long axis of quartz grains from EBSD statistical data was used to calculate κ , the grain boundary map generated from EBSD analysis was used as the basis to determine strain (E). It is found that the sample with minimum Pj also has a minimum κ and E, and vice-versa. Hence it is concluded that one-to-one correlation exists between the degree of magnetic anisotropy, strain and intensity of SPO in deformed quartzites that have a negative magnetic susceptibility. Since the application of AMS as a strain-intensity gauge in quartzites with mean susceptibility below 50 x 10-6 SI units has been questioned in the past (Hrouda, 1986), the present findings open up a further avenue of research that can be addressed using AMS. References: Gerik, A., Kruhl, J.H., 2009. Towards automated pattern quantification: time-efficient assessment of anisotropy of 2D patterns with AMOCADO. Computers and Geoscience 35, 1087-1097. Hrouda, F., 1986. The effect of quartz on the magnetic anisotropy of quartzite. Studia Geophysica et Geodaetica 30, 39-45. Piazolo, S., Passchier, C.W., 2002. Controls on lineation development in low to medium grade shear zones: a study from the Cap de Creus peninsula, NE Spain. Journal of Structural Geology 24, 25-44. Renjith, A.R., Mamtani, M.A., Urai, J.L., 2016. Fabric analysis of quartzites with negative magnetic susceptibility -- does AMS provide information of SPO or CPO of quartz? Journal of Structural Geology 82, 48-59. Tarling, D.H., Hrouda, F., 1993. The Magnetic Anisotropy of Rocks. Chapman and Hall, London, p. 217.

Effect of high-pressure torsion on the microstructural evolution and mechanical properties of an Fe-10Ni-7Mn (wt. %) lath martensitic steel

NASA Astrophysics Data System (ADS)

Kalahroudi, Faezeh Javadzadeh; Koohdar, Hamidreza; Jafarian, Hamidreza; Nili-Ahmadabadi, Mahmoud; Huang, Yi; Langdon, Terence. G.

2018-01-01

The high-pressure torsion (HPT) process is a severe plastic deformation (SPD) technique which imposes exceptionally high strains to produce extremely small grain sizes in bulk materials. In this paper, the HPT process was carried out on an Fe-10Ni-7Mn (wt.%) martensitic steel up to 20 revolutions at a rotation speed of 1 rpm under a pressure of 6.0 GPa at room temperature. The effects of the HPT process on the microstructure evolution and mechanical properties of the alloy were investigated by X-ray diffraction (XRD) analysis, electron backscatter diffraction (EBSD), micro-hardness measurement and conventional tensile testing. The XRD analysis revealed no changes in the detected phases after deformation. A significant refinement in grain size from 200 µm in the initial microstructure to around 230 nm after HPT was observed by EBSD. Although based on a rigid body assumption the imposed strain is linearly proportional to the distance from the center in HPT-processed disks, after 20 revolutions a uniform micro-hardness increment up to 650 Hv was achieved. Moreover, the tensile strength of the alloy increased from ˜800 MPa in the solution annealed condition to about 2300 MPa after the HPT process with a total tensile strain of 4%. Experimental results indicated that the HPT process leads to improvement of the tensile strength with a reasonable ductility due to the significant refinement of the microstructure.

Effect of wheel speed and annealing temperature on microstructure and texture evolution of Ni{sub 45}Mn{sub 36.6}In{sub 13.4}Co{sub 5} ribbon

DOE Office of Scientific and Technical Information (OSTI.GOV)

Feng, Yan, E-mail: yanfeng@nwpu.edu.cn

Ni{sub 45}Mn{sub 36.6}In{sub 13.4}Co{sub 5} magnetic shape memory alloy was successfully produced as preferentially textured ribbon by melting spinning with different wheel speed. X-ray diffraction (XRD) and electron back scatter diffraction (EBSD) were used to study structure and texture evolution of these melt-spun ribbons. The thickness of melt-spun ribbon is 42 μm, 65 μm and 30 μm depending on wheel speed of 1 0 m/s, 15 m/s and 20 m/s, respectively. Density of α fiber texture (〈100〉//ND) vary with wheel speed changes, and is most intensive in the ribbon with wheel speed of 15 m/s. Grains of the ribbons growmore » after being annealed at 873 K, 973 K, 1073 K and 1173 K, recrystallization was not observed in ribbons after being annealed at 873 K but occurred in ribbons after being annealed at higher temperatures. The α fiber texture becomes weaker to some extent after annealing at different temperatures, due to new recrystallization texture formed at the process of annealing. - Highlights: •Sectional part of shape memory ribbon is firstly investigated by EBSD method. •Thickness and texture of ribbons vary with wheel speed. •Annealing temperature affect texture and microstructure evolution greatly. •Recrystallization textures were observed in ribbons after being annealed.« less

Precession electron diffraction for SiC grain boundary characterization in unirradiated TRISO fuel

DOE Office of Scientific and Technical Information (OSTI.GOV)

Lillo, T. M.; van Rooyen, I. J.; Wu, Y. Q.

Precession electron diffraction (PED), a transmission electron microscopy-based technique, has been evaluated for the suitability for evaluating grain boundary character in the SiC layer of tristructural isotropic (TRISO) fuel. Although the ultimate goal is to determine the grain boundary characteristics of fission product containing grain boundaries of neutron irradiated SiC, our work reports the effect of transmission electron microscope (TEM) lamella thickness on quality of data and establishes a baseline comparison on grain boundary characteristics determined previously using a conventional EBSD scanning electron microscope (SEM) based technique. In general, it was determined that the lamella thickness produced using the standardmore » FIB fabrication process, is sufficient to provide reliable PED measurements with thicker lamellae (~120 nm) produce higher quality orientation data. Analysis of grain boundary character from the TEM-based PED data showed a much lower fraction of low angle grain boundaries compared to SEM-based EBSD data from the SiC layer of the same TRISO-coated particle as well as a SiC layer deposited at a slightly lower temperature. The fractions of high angle and CSL-related grain boundaries determined by PED are similar to those found using SEM-based EBSD. Since the grain size of the SiC layer of TRSIO fuel can be as small as 250 nm [12], depending on the fabrication parameters, and grain boundary fission product precipitates can be nano-sized, the TEM-based PED orientation data collection method is preferred to determine an accurate representation of the relative fractions of low angle, high angle and CSL-related grain boundaries. It was concluded that although the resolution of the PED data is better by more than an order of magnitude, data acquisition times may be significantly longer or the number of areas analyzed significantly larger than the SEM-based method to obtain a statistically relevant distribution. Also, grain size could be accurately determined but significantly larger analysis areas than those used in this study would be required.« less

Distinguishing Biologically Controlled Calcareous Biomineralization in Fossil Organisms Using Electron Backscatter Diffraction (EBSD)

NASA Astrophysics Data System (ADS)

Päßler, Jan-Filip; Jarochowska, Emilia; Bestmann, Michel; Munnecke, Axel

2018-02-01

Although carbonate-precipitating cyanobacteria are ubiquitous in aquatic ecosystems today, the criteria used to identify them in the geological record are subjective and rarely testable. Differences in the mode of biomineralization between cyanobacteria and eukaryotes, i.e. biologically induced calcification (BIM) vs. biologically controlled calcification (BCM), result in different crystallographic structures which might be used as a criterion to test cyanobacterial affinities. Cyanobacteria are often used as a ‘wastebasket taxon’, to which various microfossils are assigned. The lack of a testable criterion for the identification of cyanobacteria may bias their fossil record severely. We employed electron backscatter diffraction (EBSD) to investigate the structure of calcareous skeletons in two microproblematica widespread in Palaeozoic marine ecosystems: Rothpletzella, hypothesized to be a cyanobacterium, and an incertae sedis microorganism Allonema. We used a calcareous trilobite shell as a BCM reference. The mineralized structure of Allonema has a simple single-layered structure of acicular crystals perpendicular to the surface of the organism. The c-axes of these crystals are parallel to the elongation and thereby normal to the surface of the organism. EBSD pole figures and misorientation axes distribution reveal a fibre texture around the c-axis with a small degree of variation (up to 30°), indicating a highly ordered structure. A comparable pattern was found in the trilobite shell. This structure allows excluding biologically induced mineralization as the mechanism of shell formation in Allonema. In Rothpletzella, the c-axes of the microcrystalline sheath show a broader clustering compared to Allonema, but still reveal crystals tending to be perpendicular to the surface of the organism. The misorientation axes of adjacent crystals show an approximately random distribution. Rothpletzella also shares morphological similarities with extant cyanobacteria. We propose that the occurrence of a strong misorientation relationship between adjacent crystals with misorientation axes clustering around the c-axis can be used as a proxy for the degree of control exerted by an organism on its mineralized structures. Therefore, precisely constrained distributions of misorientations (misorientation angle and misorientation axis) may be used to identify BCM in otherwise problematic fossils and can be used to ground-truth the cyanobacterial affinities commonly proposed for problematic extinct organisms.

Precession electron diffraction for SiC grain boundary characterization in unirradiated TRISO fuel

DOE PAGES

Lillo, T. M.; van Rooyen, I. J.; Wu, Y. Q.

2016-06-16

Precession electron diffraction (PED), a transmission electron microscopy-based technique, has been evaluated for the suitability for evaluating grain boundary character in the SiC layer of tristructural isotropic (TRISO) fuel. Although the ultimate goal is to determine the grain boundary characteristics of fission product containing grain boundaries of neutron irradiated SiC, our work reports the effect of transmission electron microscope (TEM) lamella thickness on quality of data and establishes a baseline comparison on grain boundary characteristics determined previously using a conventional EBSD scanning electron microscope (SEM) based technique. In general, it was determined that the lamella thickness produced using the standardmore » FIB fabrication process, is sufficient to provide reliable PED measurements with thicker lamellae (~120 nm) produce higher quality orientation data. Analysis of grain boundary character from the TEM-based PED data showed a much lower fraction of low angle grain boundaries compared to SEM-based EBSD data from the SiC layer of the same TRISO-coated particle as well as a SiC layer deposited at a slightly lower temperature. The fractions of high angle and CSL-related grain boundaries determined by PED are similar to those found using SEM-based EBSD. Since the grain size of the SiC layer of TRSIO fuel can be as small as 250 nm [12], depending on the fabrication parameters, and grain boundary fission product precipitates can be nano-sized, the TEM-based PED orientation data collection method is preferred to determine an accurate representation of the relative fractions of low angle, high angle and CSL-related grain boundaries. It was concluded that although the resolution of the PED data is better by more than an order of magnitude, data acquisition times may be significantly longer or the number of areas analyzed significantly larger than the SEM-based method to obtain a statistically relevant distribution. Also, grain size could be accurately determined but significantly larger analysis areas than those used in this study would be required.« less

Effect of Morphological Differences on the Cold Formability of an Isothermally Heat-Treated Advanced High-Strength Steel

NASA Astrophysics Data System (ADS)

Weißensteiner, Irmgard; Suppan, Clemens; Hebesberger, Thomas; Winkelhofer, Florian; Clemens, Helmut; Maier-Kiener, Verena

2018-04-01

Steel sheets of Fe-0.2C-2Mn-0.2Si-0.03Ti-0.003B (m%) for the automotive industry were isothermally heat-treated, comprising austenitizing and subsequent isothermal annealing at temperatures between 300°C and 500°C. As a consequence, microstructures ranging from granular bainite over lower bainite to auto-tempered and untempered martensite were obtained. In tensile, hole expansion and bending tests, the performances in different forming conditions were compared and the changes of microstructure and texture were studied by complementary electron backscatter diffraction (EBSD) analyses. Samples with granular bainitic microstructures exhibited high total elongations but lower hole expansion ratios; in subsequent EBSD and texture analyses, evidence for inhomogeneous deformation was found. In contrast, the lath-like bainitic/martensitic microstructure showed higher strength and lower elongation to fracture. This results in a reduced bendability, but also in a high tolerance against damage induced by the shearing of edges, and, thus, allows homogeneous deformation to higher strains in the hole expansion test.

High-Temperature Deformation Behavior of MnS in 1215MS Steel

NASA Astrophysics Data System (ADS)

Huang, Fei-Ya; Su, Yen-Hao Frank; Kuo, Jui-Chao

2018-06-01

The effect of manganese sulfide (MnS) inclusions on the machinability of free-cutting steel is based on their morphology, size and distribution. Furthermore, the plasticity of MnS is high during the hot working caused different characterization of MnS. In this study, the deformation behavior of MnS in 1215MS steel after a thermomechanical process was investigated at 1323 K. The microstructures of MnS inclusions were characterized by optical microscopy, scanning electron microscopy, energy-dispersive spectrometry, and electron backscattering diffraction (EBSD). As the thickness reduction of the inclusions increased from 10 to 70%, their average aspect ratio increased from 1.20 to 2.39. In addition, the deformability of MnS inclusions was lower than that of the matrix. The possible slip systems of A, B, C, and D plane traces were ( {\\bar{1}0\\bar{1}} )[ {\\bar{1}01} ],( {10\\bar{1}} )[ {101} ],( {011} )[ {01\\bar{1}} ] , and ( {110} )[ {1\\bar{1}0} ] . Furthermore, the EBSD measurements suggested that slip planes in MnS inclusions occur on {110} planes.

Residual-stress-induced grain growth of twinned grains and its effect on formability of magnesium alloy sheet at room temperature

DOE Office of Scientific and Technical Information (OSTI.GOV)

Kim, Se-Jong; Kim, Daeyong, E-mail: daeyong@kims.re.kr; Lee, Keunho

2015-11-15

A magnesium alloy sheet was subjected to in-plane compression along with a vertical load to avoid buckling during compression. Pre-compressed specimens machined from the sheet were annealed at different temperatures and the changes in microstructure and texture were observed using electron back scattered diffraction (EBSD). Twinned grains preferentially grew during annealing at 300 °C, so that a strong texture with the < 0001 > direction parallel to the transverse direction developed. EBSD analysis confirmed that the friction caused by the vertical load induced inhomogeneous distribution of residual stress, which acted as an additional driving force for preferential grain growth ofmore » twinned grain during annealing. The annealed specimen showed excellent formability. - Highlights: • A magnesium alloy sheet subjected to in-plane compression under a vertical load • The vertical load induced inhomogeneous distribution of the residual stress. • The residual stress acted as an additional driving force for grain growth. • The annealed specimen with strong non-basal texture showed excellent formability.« less

Electron Microscopic Study of the Structure of Tetragonal Martensite in In-4.5% Cd Alloy

NASA Astrophysics Data System (ADS)

Khlebnikova, Yu. V.; Egorova, L. Yu.; Rodionov, D. P.

2018-04-01

In this work, the formation of a packet structure composed of colonies of lamellar plates separated by twin boundary {101}fct in In-4.5 wt % Cd alloy upon cooling below the fcc → fct martensitic transition temperature has been shown using the methods of metallography, X-ray diffraction, transmission electron microscopy, and EBSD analysis. Two neighboring lamellae differ from each other by the direction of their tetragonality axes. Using EBSD analysis, it has been established that neighboring packets always contain three types of tetragonal martensite lamellae, which are in twin positions and differ from each other by the direction of their tetragonality axes. In turn, each martensite lamella consists of a set of smaller lamellae, which are in twin positions. After the cycle of fct → fcc → fct transitions, the alloy recrystallizes with a decrease in the grain size by several times compared with the initial structure such that the size of packets and the length and width of martensitic lamellae in a packet correlate with a change in the size of an alloy grain.

Element-resolved Kikuchi pattern measurements of non-centrosymmetric materials

DOE Office of Scientific and Technical Information (OSTI.GOV)

Vos, Maarten, E-mail: maarten.vos@anu.edu.au

2017-01-15

Angle-resolved electron Rutherford backscattering (ERBS) measurements using an electrostatic electron energy analyser can provide unique access to element-resolved crystallographic information. We present Kikuchi pattern measurements of the non-centrosymmetric crystal GaP, separately resolving the contributions of electrons backscattered from Ga and P. In comparison to element-integrated measurements like in the method of electron backscatter diffraction (EBSD), the effect of the absence of a proper 4-fold rotation axis in the point group of GaP can be sensed with a much higher visibility via the element-resolved Ga to P intensity ratio. These element-resolved measurements make it possible to experimentally attribute the previously observedmore » point-group dependent effect in element-integrated EBSD measurements to the larger contribution of electrons scattered from Ga compared to P. - Highlights: •Element specific Kikuchi patterns are presented for GaP. •Absence of a proper four-fold rotation axis is demonstrated. •Ga and P intensity variations after 90 degree rotation have opposite phase. •The asymmetry in the total intensity distribution resembles that of Ga.« less

Electron microscopy characterization of Ni-Cr-B-Si-C laser deposited coatings.

PubMed

Hemmati, I; Rao, J C; Ocelík, V; De Hosson, J Th M

2013-02-01

During laser deposition of Ni-Cr-B-Si-C alloys with high amounts of Cr and B, various microstructures and phases can be generated from the same chemical composition that results in heterogeneous properties in the clad layer. In this study, the microstructure and phase constitution of a high-alloy Ni-Cr-B-Si-C coating deposited by laser cladding were analyzed by a combination of several microscopy characterization techniques including scanning electron microscopy in secondary and backscatter imaging modes, energy dispersive spectroscopy (EDS), electron backscatter diffraction (EBSD), and transmission electron microscopy (TEM). The combination of EDS and EBSD allowed unequivocal identification of micron-sized precipitates as polycrystalline orthorhombic CrB, single crystal tetragonal Cr5B3, and single crystal hexagonal Cr7C3. In addition, TEM characterization showed various equilibrium and metastable Ni-B, Ni-Si, and Ni-Si-B eutectic products in the alloy matrix. The findings of this study can be used to explain the phase formation reactions and to tune the microstructure of Ni-Cr-B-Si-C coatings to obtain the desired properties.

DOE Office of Scientific and Technical Information (OSTI.GOV)

Paillard, Pascal

Two try-out campaigns of friction stir welding (FSW) were performed with different friction parameters to join S690QL high yield strength steel. The welds were investigated at macroscopic and microscopic scales using optical and electronic microscopy and microhardness mapping. Welds of the second campaign exhibit microstructures and mechanical properties in accordance with requirements for service use. Microtexture measurements were carried out in different zones of welds by electron backscattered diffraction (EBSD). It is shown that that texture of the bottom of the weld is similar to that of the base metal, suggesting a diffusion bonding mechanism. Finally, the mechanical properties (tensilemore » strength, resilience, bending) were established on the most promising welds. It is shown that it is possible to weld this high yield strength steel using FSW process with satisfactory geometric, microstructural and mechanical properties. - Highlights: •1000 mm ∗ 400 mm ∗ 8 mm S690QL steel plates are joined by friction stir welding (FSW). •Maximum hardness is reduced by optimization of process parameters. •Various microstructures are formed but no martensite after process optimization. •Texture is modified in mechanically affected zones of the weld. •Texture in the bottom of the weld is preserved, suggesting diffusion bonding.« less

Microstructure characterization based on the type of deformed grains in cold-rolled, Cu-added, bake-hardenable steel

DOE Office of Scientific and Technical Information (OSTI.GOV)

Kim, J.S.; Kim, S.I.; Choi, S.-H., E-mail: shihoon@sunchon.ac.kr

2014-06-01

The electron backscatter diffraction technique has been used to characterize the microstructure of deformed grains in cold-rolled, Cu-added, bake-hardenable steel. A new scheme based on the kind and number of average orientations, as determined from a unique grain map of the deformed grains, was developed in order to classify deformed grains by type. The α-fiber components, γ-fiber components and random orientations, those which could not be assigned to either γ-fiber or α-fiber components, were used to define the average orientation of unique grains within individual deformed grains. The microstructures of deformed grains in as-rolled specimens were analyzed based on themore » Taylor factor, stored energy, and misorientation. The relative levels and distributions of the Taylor factor, the stored energy and the misorientation were examined in terms of the types of deformed grains. - Highlights: • We characterized the microstructure of Cu-added BH steel using EBSD. • A new scheme was developed in order to classify deformed grains by type. • Stored energy and misorientation are strongly dependent on the type of deformed grains. • Microstructure was examined in terms of the types of deformed grains.« less

Twin nucleation and migration in FeCr single crystals

DOE Office of Scientific and Technical Information (OSTI.GOV)

Patriarca, L.; Abuzaid, Wael; Sehitoglu, Huseyin, E-mail: huseyin@illinois.edu

2013-01-15

Tension and compression experiments were conducted on body-centered cubic Fe -47.8 at pct. Cr single crystals. The critical resolved shear stress (CRSS) magnitudes for slip nucleation, twin nucleation and twin migration were established. We show that the nucleation of slip occurs at a CRSS of about 88 MPa, while twinning nucleates at a CRSS of about 191 MPa with an associated load drop. Following twin nucleation, twin migration proceeds at a CRSS that is lower than the initiation stress ( Almost-Equal-To 114-153 MPa). The experimental results of the nucleation stresses indicate that the Schmid law holds to a first approximationmore » for the slip and twin nucleation cases, but to a lesser extent for twin migration particularly when considerable slip strains preceded twinning. The CRSSs were determined experimentally using digital image correlation (DIC) in conjunction with electron back scattering diffraction (EBSD). The DIC measurements enabled pinpointing the precise stress on the stress-strain curves where twins or slip were activated. The crystal orientations were obtained using EBSD and used to determine the activated twin and slip systems through trace analysis. - Highlights: Black-Right-Pointing-Pointer Digital image correlation allows to capture slip/twin initiation for bcc FeCr. Black-Right-Pointing-Pointer Crystal orientations from EBSD allow slip/twin system indexing. Black-Right-Pointing-Pointer Nucleation of slip always precedes twinning. Black-Right-Pointing-Pointer Twin growth is sustained with a lower stress than required for nucleation. Black-Right-Pointing-Pointer Twin-slip interactions provide high hardening at the onset of plasticity.« less

Strain induced grain boundary migration effects on grain growth of an austenitic stainless steel during static and metadynamic recrystallization

DOE Office of Scientific and Technical Information (OSTI.GOV)

Paggi, A., E-mail: alpaggi@tenaris.com; Angella, G.; Donnini, R.

Static and metadynamic recrystallization of an AISI 304L austenitic stainless steel was investigated at 1100 °C and 10{sup −} {sup 2} s{sup −} {sup 1} strain rate. The kinetics of recrystallization was determined through double hit compression tests. Two strain levels were selected for the first compression hit: ε{sub f} = 0.15 for static recrystallization (SRX) and 0.25 for metadynamic recrystallization (MDRX). Both the as-deformed and the recrystallized microstructures were investigated through optical microscopy and electron back-scattered diffraction (EBSD) technique. During deformation, strain induced grain boundary migration appeared to be significant, producing a square-like grain boundary structure aligned along themore » directions of the maximum shear stresses in compression. EBSD analysis revealed to be as a fundamental technique that the dislocation density was distributed heterogeneously in the deformed grains. Grain growth driven by surface energy reduction was also investigated, finding that it was too slow to explain the experimental data. Based on microstructural results, it was concluded that saturation of the nucleation sites occurred in the first stages of recrystallization, while grain growth driven by strain induced grain boundary migration (SIGBM) dominated the subsequent stages. - Highlights: • Recrystallization behavior of a stainless steel was investigated at 1100 °C. • EBSD revealed that the dislocation density distribution was heterogeneous during deformation. • Saturation of nucleation sites occurred in the first stages of recrystallization. • Strain induced grain boundary migration (SIGBM) effects were significant. • Grain growth driven by SIGBM dominated the subsequent stages.« less

Microstructure-Texture-Mechanical Properties in Hot Rolling of a Centrifugal Casting Ring Blank

NASA Astrophysics Data System (ADS)

Qin, Fang-cheng; Li, Yong-tang; Qi, Hui-ping; Ju, Li

2016-03-01

Deformation characteristic of centrifugal casting 25Mn steel was investigated by compression tests, and then processing maps were established. According to the deformation parameters identified from the established processing maps and hot ring rolling (HRR) process, the industrial test for the 25Mn ring blank was performed. Optical microscope (OM) and electron backscatter diffraction (EBSD) techniques were used for detecting grain boundary features and textures of deformation structures. The morphologies and mechanisms of tensile and impact fracture were revealed. The results show that softening effect plays a dominant role in higher temperatures of 1050-1150 °C and strain rates lower than 0.1 s-1. The average grain size of the rolled 25Mn ring is about 28 μm, but the grains are more coarse and inhomogeneous on the middle layer than that on rest of the areas. The texture on the outer layer is characterized by strong {110} <112> and weak {112} <111>, followed by {001} <100> and {001} <110> on the inner layer and {110} <110> on the center layer, which is mainly associated with the shear deformation. The rolled ring with precise geometrical dimensions and sound mechanical properties is fabricated by HRR. Tensile fracture is composed of clear river-shaped pattern and a little dimple near the inner layer and outer layer, and the fracture mechanism is mainly quasi-cleavage fracture, accompanied by dimple fracture. The morphologies of impact fracture consist of tear ridge and cleavage platform.

A pseudo-3D approach based on electron backscatter diffraction and backscatter electron imaging to study the character of phase boundaries between Mg and long period stacking ordered phase in a Mg–2Y–Zn alloy

DOE Office of Scientific and Technical Information (OSTI.GOV)

Afshar, Mehran, E-mail: m.afshar@mpie.de; Zaefferer, Stefan, E-mail: s.zaefferer@mpie.de

2015-03-15

In Mg–2 at.% Y–1 at.% Zn alloys, the LPSO (Long Period Stacking Ordered) phase is important to improve mechanical properties of the material. The aim of this paper is to present a study on the phase boundary character in these two-phase alloys. Using EBSD pattern analysis it was found that the 24R structure is the dominant LPSO phase structure in the current alloy. The phase boundary character between the Mg matrix and the LPSO phase was investigated using an improved pseudo-3D EBSD (electron backscatter diffraction) technique in combination with BSE or SE (backscatter or secondary electron) imaging. A large amountmore » of very low-angle phase boundaries was detected. The (0 0 0 2) plane in the Mg matrix which is parallel to the (0 0 0 24) plane in the LPSO phase was found to be the most frequent plane for these phase boundaries. This plane is supposed to be the habit plane of the eutectic co-solidification of the Mg matrix and the LPSO phase. - Highlights: • It is shown that for the investigated alloy the LPSO phase has mainly 24R crystal structure. • A new method is presented which allows accurate determination of the 5-parameter grain or phase boundary character. • It is found that the low-angle phase boundaries appearing in the alloy all have basal phase boundary planes.« less

Genesis of diamond inclusions: An integrated cathodoluminescence (CL) and Electron backscatter diffraction (EBSD) study on eclogitic and peridotitic inclusions and their diamond host.

NASA Astrophysics Data System (ADS)

van den Heuvel, Quint; Matveev, Sergei; Drury, Martyn; Gress, Michael; Chinn, Ingrid; Davies, Gareth

2017-04-01

Diamond inclusions are potentially fundamental to understanding the formation conditions of diamond and the volatile cycles in the deep mantle. In order to fully understand the implications of the compositional information recorded by inclusions it is vital to know whether the inclusions are proto-, syn-, or epigenetic and the extent to which they have equilibrated with diamond forming fluids. In previous studies, the widespread assumption was made that the majority of diamond inclusions are syngenetic, based upon observation of cubo-octahedral morphology imposed on the inclusions. Recent work has reported the crystallographic relationship between inclusions and the host diamond to be highly complex and the lack of crystallographic relationships between inclusions and diamonds has led some to question the significance of imposed cubo-octahedral morphology. This study presents an integrated EBSD and CL study of 9 diamonds containing 20 pyropes, 2 diopsides, 1 forsterite and 1 rutile from the Jwaneng and Letlhakane kimberlite clusters, Botswana. A new method was developed to analyze the crystallographic orientation of the host diamond and the inclusions with EBSD. Diamonds plates were sequentially polished to expose inclusions at different levels in the diamond. CL imaging at different depths was performed in order to produce a 3D view of diamond growth zones around the inclusions. Standard diamond polishing techniques proved too aggressive for silicate inclusions as they were damaged to such a degree that EBSD measurements on the inclusions were impossible. The inclusions were milled with a Ga+ focused ion beam (FIB) at a 12° angle to clean the surface for EBSD measurements. Of the 24 inclusions, 9 have an imposed cubo-octahedral morphology. Of these inclusions, 6 have faces orientated parallel to diamond growth zones and/or appear to have nucleated on a diamond growth surface, implying syngenesis. In contrast, other diamonds record resorption events such that inclusions now cut diamond growth zones. In most cases, the growth zonation around inclusions is not well defined due to CL haloes but some inclusions clearly disrupt diamond growth. Crystallographic orientations of diamond and the inclusions, determined using EBSD, revealed that each inclusion has a homogeneous orientation and record no compositional zonation. The diamonds also showed no angular deviations despite many having multiple growth and resorption zones; implying epitaxial growth of diamond. Crystallographic alignment between diamond and inclusions was not recorded for the principle planes and limited to 3 possible coincidences on minor planes from the 24 inclusions studied. The CL data show no evidence of syngenesis for these 3 inclusions. Analyses of two diamonds with inclusion clusters in different growth zones, 400 µm apart, revealed the same chemical composition and orientation, potentially implying they originated from an original larger inclusion. Combined EBSD and CL data suggest that there is no direct orientational correlation (epitaxial growth) between silicate inclusions and the host diamond, even when the mineral phases are of the same symmetry group. The presentation will provide a detailed evaluation of the genesis of individual inclusions.

Twinning-mediated work hardening and texture evolution in CrCoFeMnNi high entropy alloys at cryogenic temperature

DOE Office of Scientific and Technical Information (OSTI.GOV)

Liu, T. K.; Wu, Z.; Stoica, A. D.

The cryogenic plastic deformation of CrCoFeMnNi high entropy alloy is characterized by three distinct stages based on the change of the work hardening rate. Microstructure and bulk texture at different strain levels were studied by electron backscatter diffraction (EBSD) and neutron diffraction. Our findings indicate that the deformation twins led to the constant work hardening rate at Stage II and resulted in the appearance of <115 >//TA texture component, while the dislocation slip was involved all though the entire plastic deformation. As a result, the twinning-mediated tensile plastic deformation at cryogenic temperature finally induced the strong {111}- < 112 >more » texture component and minor {001} < 110 > texture component accompanied with twinning-induced {115}< 552 > texture component.« less

Stable tetragonal phase and magnetic properties of Fe-doped HfO2 nanoparticles

NASA Astrophysics Data System (ADS)

Sales, T. S. N.; Cavalcante, F. H. M.; Bosch-Santos, B.; Pereira, L. F. D.; Cabrera-Pasca, G. A.; Freitas, R. S.; Saxena, R. N.; Carbonari, A. W.

2017-05-01

In this paper, the effect in structural and magnetic properties of iron doping with concentration of 20% in hafnium dioxide (HfO2) nanoparticles is investigated. HfO2 is a wide band gap oxide with great potential to be used as high-permittivity gate dielectrics, which can be improved by doping. Nanoparticle samples were prepared by sol-gel chemical method and had their structure, morphology, and magnetic properties, respectively, investigated by X-ray diffraction (XRD), transmission electron microscopy (TEM) and scanning electron microscopy (SEM) with electron back scattering diffraction (EBSD), and magnetization measurements. TEM and SEM results show size distribution of particles in the range from 30 nm to 40 nm with small dispersion. Magnetization measurements show the blocking temperature at around 90 K with a strong paramagnetic contribution. XRD results show a major tetragonal phase (94%).

Investigating the Effects of Pin Tool Design on Friction Stir Welded Ti-6Al-4V

NASA Technical Reports Server (NTRS)

Rubisoff, H. A.; Querin, J. A.; Schneider, Judy A.; Magee, D.

2009-01-01

Friction stir welding (FSWing), a solid state joining technique, uses a non-consumable rotating pin tool to thermomechanically join materials. Heating of the weldment caused by friction and deformation is a function of the interaction between the pin tool and the work piece. Therefore, the geometry of the pin tool is in part responsible for the resulting microstructure and mechanical properties. In this study microwave sintered tungsten carbide (WC) pin tools with tapers and flats were used to FSW Ti-6Al-4V. Transverse sections of welds were mechanically tested, and the microstructure was characterized using optical microscopy (OM) and scanning election microscopy (SEM). X-ray diffraction (XRD) and electron back-scatter diffraction (EBSD) were used to characterize the texture within the welds produced from the different pin tool designs.

Twinning-mediated work hardening and texture evolution in CrCoFeMnNi high entropy alloys at cryogenic temperature

DOE PAGES

Liu, T. K.; Wu, Z.; Stoica, A. D.; ...

2017-06-17

The cryogenic plastic deformation of CrCoFeMnNi high entropy alloy is characterized by three distinct stages based on the change of the work hardening rate. Microstructure and bulk texture at different strain levels were studied by electron backscatter diffraction (EBSD) and neutron diffraction. Our findings indicate that the deformation twins led to the constant work hardening rate at Stage II and resulted in the appearance of <115 >//TA texture component, while the dislocation slip was involved all though the entire plastic deformation. As a result, the twinning-mediated tensile plastic deformation at cryogenic temperature finally induced the strong {111}- < 112 >more » texture component and minor {001} < 110 > texture component accompanied with twinning-induced {115}< 552 > texture component.« less

A comparison of deformation and failure behaviors of AZ31 and E-form Mg alloys under V-bending test

NASA Astrophysics Data System (ADS)

Choi, Shi-Hoon; Singh, Jaiveer; Kim, Min-Seong; Yoon, Jeong-Whan

2016-08-01

Deformation and failure behaviors of magnesium (Mg) alloys (AZ31 and E-form) were investigated using V-bending test. Formability of these Mg alloys was discussed in terms of minimum bending radius. Microtexture evolution in the deformed Mg alloys was examined via electron back-scattered diffraction (EBSD) technique. Two level simulation technique which combined continuum finite element method (FEM) and crystal plasticity FEM successfully simulated the microtexture evolution in Mg alloys during V-bending test. The effect of deformation twinning on the failure in Mg alloys was also examined.

Phase Transformation Study in Nb-Mo Microalloyed Steels Using Dilatometry and EBSD Quantification

NASA Astrophysics Data System (ADS)

Isasti, Nerea; Jorge-Badiola, Denis; Taheri, Mitra L.; Uranga, Pello

2013-08-01

A complete microstructural characterization and phase transformation analysis has been performed for several Nb and Nb-Mo microalloyed low-carbon steels using electron backscattered diffraction (EBSD) and dilatometry tests. Compression thermomechanical schedules were designed resulting in the undeformed and deformed austenite structures before final transformation. The effects of microalloying additions and accumulated deformation were analyzed after CCT diagram development and microstructural quantification. The resulting microstructures ranged from polygonal ferrite and pearlite at slow cooling ranges, to a combination of quasipolygonal ferrite and granular ferrite for intermediate cooling rates, and finally, to bainitic ferrite with martensite for fast cooling rates. The addition of Mo promotes a shift in the CCT diagrams to lower transformation start temperatures. When the amount of Nb is increased, CCT diagrams show little variations for transformations from the undeformed austenite and higher initial transformation temperatures in the transformations from the deformed austenite. This different behavior is due to the effect of niobium on strain accumulation in austenite and its subsequent acceleration of transformation kinetics. This article shows the complex interactions between chemical composition, deformation, and the phases formed, as well as their effect on microstructural unit sizes and homogeneity.

Microstructure of Reaction Zone Formed During Diffusion Bonding of TiAl with Ni/Al Multilayer

NASA Astrophysics Data System (ADS)

Simões, Sónia; Viana, Filomena; Koçak, Mustafa; Ramos, A. Sofia; Vieira, M. Teresa; Vieira, Manuel F.

2012-05-01

In this article, the characterization of the interfacial structure of diffusion bonding a TiAl alloy is presented. The joining surfaces were modified by Ni/Al reactive multilayer deposition as an alternative approach to conventional diffusion bonding. TiAl substrates were coated with alternated Ni and Al nanolayers. The nanolayers were deposited by dc magnetron sputtering with 14 nm of period (bilayer thickness). Joining experiments were performed at 900 °C for 30 and 60 min with a pressure of 5 MPa. Cross sections of the joints were prepared for characterization of their interfaces by scanning electron microscopy (SEM), transmission electron microscopy (TEM), scanning transmission electron microscopy (STEM), high resolution TEM (HRTEM), energy dispersive x-ray spectroscopy (EDS), and electron backscatter diffraction (EBSD). Several intermetallic compounds form at the interface, assuring the bonding of the TiAl. The interface can be divided into three distinct zones: zone 1 exhibits elongated nanograins, very small equiaxed grains are observed in zone 2, while zone 3 has larger equiaxed grains. EBSD analysis reveals that zone 1 corresponds to the intermetallic Al2NiTi and AlNiTi, and zones 2 and 3 to NiAl.

Error analysis of the crystal orientations obtained by the dictionary approach to EBSD indexing.

PubMed

Ram, Farangis; Wright, Stuart; Singh, Saransh; De Graef, Marc

2017-10-01

The efficacy of the dictionary approach to Electron Back-Scatter Diffraction (EBSD) indexing was evaluated through the analysis of the error in the retrieved crystal orientations. EBSPs simulated by the Callahan-De Graef forward model were used for this purpose. Patterns were noised, distorted, and binned prior to dictionary indexing. Patterns with a high level of noise, with optical distortions, and with a 25 × 25 pixel size, when the error in projection center was 0.7% of the pattern width and the error in specimen tilt was 0.8°, were indexed with a 0.8° mean error in orientation. The same patterns, but 60 × 60 pixel in size, were indexed by the standard 2D Hough transform based approach with almost the same orientation accuracy. Optimal detection parameters in the Hough space were obtained by minimizing the orientation error. It was shown that if the error in detector geometry can be reduced to 0.1% in projection center and 0.1° in specimen tilt, the dictionary approach can retrieve a crystal orientation with a 0.2° accuracy. Copyright © 2017 Elsevier B.V. All rights reserved.

Crystallographic texture and microstructural changes in fusion welds of recrystallized Zry-4 rolled plates

NASA Astrophysics Data System (ADS)

Moya Riffo, A.; Vicente Alvarez, M. A.; Santisteban, J. R.; Vizcaino, P.; Limandri, S.; Daymond, M. R.; Kerr, D.; Okasinski, J.; Almer, J.; Vogel, S. C.

2017-05-01

This work presents a detailed characterization of the microstructural and crystallographic texture changes observed in the transition region in a weld between two Zircaloy-4 cold rolled and recrystallized plates. The microstructural study was performed by optical microscopy under polarized light and scanning electron microscopy (SEM). Texture changes were characterized at different lengthscales: in the micrometric size, orientation imaging maps (OIM) were constructed by electron backscatter diffraction (EBSD), in the millimetre scale, high energy XRD experiments were done at the Advanced Photon Source (USA) and compared to neutron diffraction texture determinations performed in the HIPPO instrument at Los Alamos National Laboratory. In the heat affected zone (HAZ) we observed the development of Widmanstätten microstructures, typical of the α(hcp) to β(bcc) phase transformation. Associated with these changes a rotation of the c-poles is found in the HAZ and fusion zone. While the base material shows the typical texture of a cold rolled plate, with their c-poles pointing 35° apart from the normal direction of the plate in the normal-transversal line, in the HAZ, c-poles align along the transversal direction of the plate and then re-orient along different directions, all of these changes occurring within a lengthscale in the order of mm. The evolution of texture in this narrow region was captured by both OIM and XRD, and is consistent with previous measurements done by Neutron Diffraction in the HIPPO diffractometer at Los Alamos National Laboratory, USA. The microstructural and texture changes along the HAZ were interpreted as arising due to the effect of differences in the cooling rate and β grain size on the progress of the different α variants during transformation. Fast cooling rates and large β grains are associated to weak variant selection during the β->α transformation, while slow cooling rates and fine β grains result in strong variant selection.

Crystallographic texture and microstructural changes in fusion welds of recrystallized Zry-4 rolled plates

DOE PAGES

Riffo, A. Moya; Vicente Alvarez, M. A.; Santisteban, J. R.; ...

2017-02-08

This study presents a detailed characterization of the microstructural and crystallographic texture changes observed in the transition region in a weld between two Zircaloy-4 cold rolled and recrystallized plates. The microstructural study was performed by optical microscopy under polarized light and scanning electron microscopy (SEM). Texture changes were characterized at different lengthscales: in the micrometric size, orientation imaging maps (OIM) were constructed by electron backscatter diffraction (EBSD), in the millimetre scale, high energy XRD experiments were done at the Advanced Photon Source (USA) and compared to neutron diffraction texture determinations performed in the HIPPO instrument at Los Alamos National Laboratory.more » In the heat affected zone (HAZ) we observed the development of Widmanstätten microstructures, typical of the α( hcp) to β( bcc) phase transformation. Associated with these changes a rotation of the c-poles is found in the HAZ and fusion zone. While the base material shows the typical texture of a cold rolled plate, with their c-poles pointing 35° apart from the normal direction of the plate in the normal-transversal line, in the HAZ, c-poles align along the transversal direction of the plate and then re-orient along different directions, all of these changes occurring within a lengthscale in the order of mm. The evolution of texture in this narrow region was captured by both OIM and XRD, and is consistent with previous measurements done by Neutron Diffraction in the HIPPO diffractometer at Los Alamos National Laboratory, USA. The microstructural and texture changes along the HAZ were interpreted as arising due to the effect of differences in the cooling rate and β grain size on the progress of the different α variants during transformation. Fast cooling rates and large β grains are associated to weak variant selection during the β–>α transformation, while slow cooling rates and fine β grains result in strong variant selection.« less

Crystallographic texture and microstructural changes in fusion welds of recrystallized Zry-4 rolled plates

DOE Office of Scientific and Technical Information (OSTI.GOV)

Riffo, A. Moya; Vicente Alvarez, M. A.; Santisteban, J. R.

This study presents a detailed characterization of the microstructural and crystallographic texture changes observed in the transition region in a weld between two Zircaloy-4 cold rolled and recrystallized plates. The microstructural study was performed by optical microscopy under polarized light and scanning electron microscopy (SEM). Texture changes were characterized at different lengthscales: in the micrometric size, orientation imaging maps (OIM) were constructed by electron backscatter diffraction (EBSD), in the millimetre scale, high energy XRD experiments were done at the Advanced Photon Source (USA) and compared to neutron diffraction texture determinations performed in the HIPPO instrument at Los Alamos National Laboratory.more » In the heat affected zone (HAZ) we observed the development of Widmanstätten microstructures, typical of the α( hcp) to β( bcc) phase transformation. Associated with these changes a rotation of the c-poles is found in the HAZ and fusion zone. While the base material shows the typical texture of a cold rolled plate, with their c-poles pointing 35° apart from the normal direction of the plate in the normal-transversal line, in the HAZ, c-poles align along the transversal direction of the plate and then re-orient along different directions, all of these changes occurring within a lengthscale in the order of mm. The evolution of texture in this narrow region was captured by both OIM and XRD, and is consistent with previous measurements done by Neutron Diffraction in the HIPPO diffractometer at Los Alamos National Laboratory, USA. The microstructural and texture changes along the HAZ were interpreted as arising due to the effect of differences in the cooling rate and β grain size on the progress of the different α variants during transformation. Fast cooling rates and large β grains are associated to weak variant selection during the β–>α transformation, while slow cooling rates and fine β grains result in strong variant selection.« less

Applications of Real Space Crystallography in Characterization of Dislocations in Geological Materials in a Scanning Electron Microscope (SEM)

NASA Astrophysics Data System (ADS)

Kaboli, S.; Burnley, P. C.

2017-12-01

Imaging and characterization of defects in crystalline materials is of significant importance in various disciplines including geoscience, materials science, and applied physics. Linear defects such as dislocations and planar defects such as twins and stacking faults, strongly influence many of the properties of crystalline materials and also reflect the conditions and degree of deformation. Dislocations have been conventionally imaged in thin foils in a transmission electron microscope (TEM). Since the development of field emission scanning electron microscopes (FE-SEM) with high gun brightness and small spot size, extensive efforts have been dedicated to the imaging and characterization of dislocations in semi-conductors using electron channeling contrast imaging (ECCI) in the SEM. The obvious advantages of using SEM over TEM include easier and non-destructive sample preparation and a large field of view enabling statistical examination of the density and distribution of dislocations and other defects. In this contribution, we extend this technique to geological materials and introduce the Real Space Crystallography methodology for imaging and complete characterization of dislocations based on bend contour contrast obtained by ECCI in FE-SEM. Bend contours map out the distortion in the crystal lattice across a deformed grain. The contrast of dislocations is maximum in the vicinity of bend contours where crystal planes diffract at small and positive deviations from the Bragg positions (as defined by Bragg's law of electron diffraction). Imaging is performed in a commercial FE-SEM equipped with a standard silicon photodiode backscattered (BSE) detector and an electron backscatter diffraction (EBSD) system for crystal orientation measurements. We demonstrate the practice of this technique in characterization of a number of geological materials in particular quartz, forsterite olivine and corundum, experimentally deformed at high pressure-temperature conditions. This new approach in microstructure characterization of deformed geologic materials in FE-SEM, without the use of etching or decoration techniques, has valuable applications to both experimentally deformed and naturally deformed specimens.

Correlative characterization of primary particles formed in as-cast Al-Mg alloy containing a high level of Sc

DOE Office of Scientific and Technical Information (OSTI.GOV)

Zhou, Shi'ang

Primary particles formed in as-cast Al-5Mg-0.6Sc alloy and their role in microstructure and mechanical properties of the alloy were investigated using optical microscopy (OM), scanning electron microscopy (SEM), electron back-scatter diffraction (EBSD) and tensile testing. It was found that primary particles due to a close orientation to matrix could serve as the potent heterogeneous nucleation sites for α-Al during solidification and thus impose a remarkable grain refinement effect. Eutectic structure consisted of layer by layer of ‘Al{sub 3}Sc + α-Al + Al{sub 3}Sc + ⋯’ and cellular-dendritic substructure were simultaneously observed at the particles inside, indicating that these particles couldmore » be identified as the eutectics rather than individual Al{sub 3}Sc phase. A calculating method, based on EBSD results, was introduced for the spatial distribution of these particles in matrix. The results showed that these eutectic particles randomly distributed in matrix. In addition, the formation of primary eutectic particles significant improved the strength of the Al-Mg alloy in as-cast condition, which is ascribed to the structural evolution from coarse dendrites to prefect fine equiaxed grains. On the other hand, these large-sized particles due to the tendency to act as the microcrack sources could cause a harmful effect in the ductility of Al-Mg-Sc alloy. - Highlights: •Primary particles exhibit an ‘Al{sub 3}Sc + α-Al + Al{sub 3}Sc + ⋯’ multilayer feature with a cellular-dendritic mode of growth. •EBSD analyses the mechanism of grain refinement and the distribution of primary particles in α-Al matrix. •A computational method was presented to calculate the habit planes of primary particles.« less

Subgrain boundary analyses in deformed orthopyroxene by TEM/STEM with EBSD-FIB sample preparation technique

NASA Astrophysics Data System (ADS)

Kogure, Toshihiro; Raimbourg, Hugues; Kumamoto, Akihito; Fujii, Eiko; Ikuhara, Yuichi

2014-12-01

High-resolution structure analyses using electron beam techniques have been performed for the investigation of subgrain boundaries (SGBs) in deformed orthopyroxene (Opx) in mylonite from Hidaka Metamorphic Belt, Hokkaido, Japan, to understand ductile deformation mechanism of silicate minerals in shear zones. Scanning electron microscopy (SEM) and electron backscatter diffraction (EBSD) analysis of Opx porphyroclasts in the mylonitic rock indicated that the crystal orientation inside the Opx crystals gradually changes by rotation about the b-axis by SGBs and crystal folding. In order to observe the SGBs along the b-axis by transmission electron microscopy (TEM) or scanning TEM (STEM), the following sample preparation protocol was adopted. First, petrographic thin sections were slightly etched with hydrofluoric acid to identify SGBs in SEM. The Opx crystals whose b-axes were oriented close to the normal of the surface were identified by EBSD, and the areas containing SGBs were picked and thinned for (S) TEM analysis with a focused ion beam instrument with micro-sampling system. High-resolution TEM imaging of the SGBs in Opx revealed various boundary structures from a periodic array of dissociated (100) [001] edge dislocations to partially or completely incoherent crystals, depending on the misorientation angle. Atomic-resolution STEM imaging clearly confirmed the formation of clinopyroxene (Cpx) structure between the dissociated partial dislocations. Moreover, X-ray microanalysis in STEM revealed that the Cpx contains a considerable amount of calcium replacing iron. Such chemical inhomogeneity may limit glide motion of the dislocation and eventually the plastic deformation of the Opx porphyroclasts at a low temperature. Chemical profiles across the high-angle incoherent SGB also showed an enrichment of the latter in calcium at the boundary, suggesting that SGBs are an efficient diffusion pathway of calcium out of host Opx grain during cooling.

Three-Dimensional FIB/EBSD Characterization of Irradiated HfAl3-Al Composite

DOE Office of Scientific and Technical Information (OSTI.GOV)

Hua, Zilong; Guillen, Donna Post; Harris, William

2016-09-01

A thermal neutron absorbing material, comprised of 28.4 vol% HfAl3 in an Al matrix, was developed to serve as a conductively cooled thermal neutron filter to enable fast flux materials and fuels testing in a pressurized water reactor. In order to observe the microstructural change of the HfAl3-Al composite due to neutron irradiation, an EBSD-FIB characterization approach is developed and presented in this paper. Using the focused ion beam (FIB), the sample was fabricated to 25µm × 25µm × 20 µm and mounted on the grid. A series of operations were carried out repetitively on the sample top surface tomore » prepare it for scanning electron microscopy (SEM). First, a ~100-nm layer was removed by high voltage FIB milling. Then, several cleaning passes were performed on the newly exposed surface using low voltage FIB milling to improve the SEM image quality. Last, the surface was scanned by Electron Backscattering Diffraction (EBSD) to obtain the two-dimensional image. After 50 to 100 two-dimensional images were collected, the images were stacked to reconstruct a three-dimensional model using DREAM.3D software. Two such reconstructed three-dimensional models were obtained from samples of the original and post-irradiation HfAl3-Al composite respectively, from which the most significant microstructural change caused by neutron irradiation apparently is the size reduction of both HfAl3 and Al grains. The possible reason is the thermal expansion and related thermal strain from the thermal neutron absorption. This technique can be applied to three-dimensional microstructure characterization of irradiated materials.« less

Post Deformation Annealing Behaviour of Mg-Al-Sn Alloys

NASA Astrophysics Data System (ADS)

Kabir, Abu Syed Humaun; Su, Jing; Sanjari, Mehdi; Jung, In-Ho; Yue, Stephen

In this study, effects of dynamically formed precipitates on the microstructure and texture evolutions were investigated after the post deformation annealing for various times. Two ternary alloys of Mg, Al and Sn were designed, produced and deformed at 300°C at a strain rate of 0.01s-1 to form different amounts of strain induced precipitates during deformation. Subsequent annealing at deformation temperature was performed for up to 4 hours. Microstructures and precipitation were investigated by optical and scanning electron microscopes and macro and micro-texture were measured by X-ray diffraction (XRD) and Electron Back-Scattered Diffraction (EBSD) techniques, respectively. It was found that certain amount of strain induced precipitates was necessary to prevent grain growth for a certain time during annealing by grain boundary pinning effect. Also, texture randomization was possible with the presence of precipitates after certain time of annealing.

Energy dependence of the spatial distribution of inelastically scattered electrons in backscatter electron diffraction

NASA Astrophysics Data System (ADS)

Ram, Farangis; De Graef, Marc

2018-04-01

In an electron backscatter diffraction pattern (EBSP), the angular distribution of backscattered electrons (BSEs) depends on their energy. Monte Carlo modeling of their depth and energy distributions suggests that the highest energy BSEs are more likely to hit the bottom of the detector than the top. In this paper, we examine experimental EBSPs to validate the modeled angular BSE distribution. To that end, the Kikuchi bandlet method is employed to measure the width of Kikuchi bands in both modeled and measured EBSPs. The results show that in an EBSP obtained with a 15 keV primary probe, the width of a Kikuchi band varies by about 0 .4∘ from the bottom of the EBSD detector to its top. The same is true for a simulated pattern that is composed of BSEs with 5 keV to 15 keV energies, which validates the Monte Carlo simulations.

Complete grain boundaries from incomplete EBSD maps: the influence of segmentation on grain size determinations

NASA Astrophysics Data System (ADS)

Heilbronner, Renée; Kilian, Ruediger

2017-04-01

Grain size analyses are carried out for a number of reasons, for example, the dynamically recrystallized grain size of quartz is used to assess the flow stresses during deformation. Typically a thin section or polished surface is used. If the expected grain size is large enough (10 µm or larger), the images can be obtained on a light microscope, if the grain size is smaller, the SEM is used. The grain boundaries are traced (the process is called segmentation and can be done manually or via image processing) and the size of the cross sectional areas (segments) is determined. From the resulting size distributions, 'the grain size' or 'average grain size', usually a mean diameter or similar, is derived. When carrying out such grain size analyses, a number of aspects are critical for the reproducibility of the result: the resolution of the imaging equipment (light microscope or SEM), the type of images that are used for segmentation (cross polarized, partial or full orientation images, CIP versus EBSD), the segmentation procedure (algorithm) itself, the quality of the segmentation and the mathematical definition and calculation of 'the average grain size'. The quality of the segmentation depends very strongly on the criteria that are used for identifying grain boundaries (for example, angles of misorientation versus shape considerations), on pre- and post-processing (filtering) and on the quality of the recorded images (most notably on the indexing ratio). In this contribution, we consider experimentally deformed Black Hills quartzite with dynamically re-crystallized grain sizes in the range of 2 - 15 µm. We compare two basic methods of segmentations of EBSD maps (orientation based versus shape based) and explore how the choice of methods influences the result of the grain size analysis. We also compare different measures for grain size (mean versus mode versus RMS, and 2D versus 3D) in order to determine which of the definitions of 'average grain size yields the most stable results.

Microstructures of ancient and modern cast silver–copper alloys

DOE Office of Scientific and Technical Information (OSTI.GOV)

Northover, S.M., E-mail: s.m.northover@open.ac.uk; Northover, J.P., E-mail: peter.northover@materials.ox.ac.uk

The microstructures of modern cast Sterling silver and of cast silver objects about 2500 years old have been compared using optical microscopy (OM), scanning electron microscopy (SEM), transmission electron microscopy (TEM), scanning transmission electron microscopy (STEM), energy dispersive X-ray microanalysis (EDX) and electron backscatter diffraction (EBSD). Microstructures of both ancient and modern alloys were typified by silver-rich dendrites with a few pools of eutectic and occasional cuprite particles with an oxidised rim on the outer surface. EBSD showed the dendrites to have a complex internal structure, often involving extensive twinning. There was copious intragranular precipitation within the dendrites, in themore » form of very fine copper-rich rods which TEM, X-ray diffraction (XRD), SEM and STEM suggest to be of a metastable face-centred-cubic (FCC) phase with a cube–cube orientation relationship to the silver-rich matrix but a higher silver content than the copper-rich β in the eutectic. Samples from ancient objects displayed a wider range of microstructures including a fine scale interpenetration of the adjoining grains not seen in the modern material. Although this study found no unambiguous evidence that this resulted from microstructural change produced over archaeological time, the copper supersaturation remaining after intragranular precipitation suggests that such changes, previously proposed for wrought and annealed material, may indeed occur in ancient silver castings. - Highlights: • Similar twinned structures and oxidised surfaces seen in ancient and modern cast silver • General precipitation of fine Cu-rich rods apparently formed by discontinuous precipitation is characteristic of as-cast silver. • The fine rods are cube-cube related to the matrix in contrast with the eutectic. • The silver-rich phase remains supersaturated with copper. • Possibly age-related grain boundary features seen in ancient cast silver.« less

Tetragonal Almandine, (Fe,Mg,Ca,Na)3(Al,Si,Mg)2Si3O12, a New High-Pressure Mineral from the Shergotty Impact on Mars: an Integrated FESEM-EPMA-Synchrotron Diffraction Investigation

NASA Astrophysics Data System (ADS)

Ma, C.; Tschauner, O. D.

2016-12-01

The combination of FESEM-EDS-EBSD, EPMA, and synchrotron microdiffraction is developing into a powerful tool for identification of micron-scale minerals in rocks such as high-pressure phases in shocked meteorites. During a nanomineralogy investigation of the Shergotty meteorite using this approach, we have identified a new shock-induced high-pressure silicate, majoritic almandine with a tetragonal I41/a structure, in an impact melt pocket. The Shergotty meteorite, which fell in the Gaya district, Bihar, India in 1865, is a Martian basaltic shergottite with shock features. Tetragonal almandine in Shergotty occurs as aggregates of subhedral crystals, 0.8 - 2.5 µm in diameter, along with stishovite in the central region of a shock melt pocket, showing an empirical formula of (Fe1.16Ca0.75Mg0.61Na0.42Mn0.03K0.01)(Al1.16Si0.63Mg0.19Ti0.02)Si3O12. Its general formula is (Fe,Mg,Ca,Na)3(Al,Si,Mg)2Si3O12. EBSD indicated this phase has a garnet-related structure. Synchrotron X-ray diffraction revealed that this garnet has actually a tetragonal structure (I41/a) with unit cell dimensions: a = 11.585(9) Å, c = 11.63(4) Å, V = 1561(7) Å3, and Z = 8. Tetragonal almandine is the polymorph of cubic almandine, a new high-pressure garnet mineral, formed by shock metamorphism via the Shergotty impact event on Mars. It apparently crystallized from Fe-rich shock-induced melt under high-pressure and high-temperature conditions.

Stress Corrosion Cracking Susceptibility of 304L Substrate and 308L Weld Metal Exposed to a Salt Spray

PubMed Central

Hsu, Chia-Hao; Chen, Tai-Cheng; Huang, Rong-Tan; Tsay, Leu-Wen

2017-01-01

304 stainless steels (SS) were considered as the materials for a dry storage canister. In this study, ER (Electrode Rod) 308L was utilized as the filler metal for the groove and overlay welds of a 304L stainless steel substrate, which was prepared via a gas tungsten arc-welding process in multiple passes. The electron backscatter diffraction (EBSD) map was used to identify the inherent microstructures in distinct specimens. U-bend and weight-loss tests were conducted by testing the 304L substrates and welds in a salt spray containing 5 wt % NaCl at 80 °C to evaluate their susceptibility to stress corrosion cracking (SCC). Generally, the weight loss of the ER 308L deposit was higher than that of the 304L substrate in a salt spray in the same sample-prepared condition. The dissolution of the skeletal structure in the fusion zone (FZ) was responsible for a greater weight loss of the 308L deposit, especially for the cold-rolled and sensitized specimen. Cold rolling was detrimental and sensitization after cold rolling was very harmful to the SCC resistance of the 304L substrate and 308L deposit. Overall, the SCC susceptibility of each specimen was correlated with its weight loss in each group. PMID:28772547

Effect of heat treatment on the crystal structure of deformed samples of chromium-manganese steel

NASA Astrophysics Data System (ADS)

Chezganov, D. S.; Chikova, O. A.; Borovykh, M. A.

2017-09-01

Results of studying microstructures and the crystal structure of samples of 35KhGF steel (0.31-0.38 wt % C, 0.17-0.37 wt % Si, 0.95-1.25 wt % Mn, 1.0-1.3 wt % Cr, 0.06-0.12 wt % V, and the remainder was Fe) have been presented. The samples have been selected from hot-rolled pipes subjected to different heat treatments. A study has been carried out in order to explain the choice of the heat-treatment regime based on determining the structure-properties relationship that provides an increase in the corrosion resistance of pipes to the effect of hydrocarbons. Methods of the energy-dispersive X-ray spectroscopy (EDS) and electron backscatter diffraction (EBSD) have been used. In the microstructure of samples, oxide inclusions and discontinuities with sizes of 1-50 μm that presumably consist of the scale were detected. The ferrite grain size and the orientations of crystals were determined; the data on the local mechanical stresses in the Taylor orientation- factor maps were obtained. The grain refinement; the increase in the fraction of the low-angle boundaries; and the decrease in the local mechanical stresses and, therefore, the highest corrosion resistance to the effect of hydrocarbons is achieved by normalizing at 910°C.

Microstructural characterization of weld joints of 9Cr reduced activation ferritic martensitic steel fabricated by different joining methods

DOE Office of Scientific and Technical Information (OSTI.GOV)

Thomas Paul, V.; Saroja, S.; Albert, S.K.

This paper presents a detailed electron microscopy study on the microstructure of various regions of weldment fabricated by three welding methods namely tungsten inert gas welding, electron beam welding and laser beam welding in an indigenously developed 9Cr reduced activation ferritic/martensitic steel. Electron back scatter diffraction studies showed a random micro-texture in all the three welds. Microstructural changes during thermal exposures were studied and corroborated with hardness and optimized conditions for the post weld heat treatment have been identified for this steel. Hollomon–Jaffe parameter has been used to estimate the extent of tempering. The activation energy for the tempering processmore » has been evaluated and found to be corresponding to interstitial diffusion of carbon in ferrite matrix. The type and microchemistry of secondary phases in different regions of the weldment have been identified by analytical transmission electron microscopy. - Highlights: • Comparison of microstructural parameters in TIG, electron beam and laser welds of RAFM steel • EBSD studies to illustrate the absence of preferred orientation and identification of prior austenite grain size using phase identification map • Optimization of PWHT conditions for indigenous RAFM steel • Study of kinetics of tempering and estimation of apparent activation energy of the process.« less

Stage-Rocked Electron Channeling for Crystal Orientation Mapping (Postprint)

DTIC Science & Technology

2018-03-26

SUPPLEMENTARY NOTES PA Case Number: 88ABW-2017-6217; Clearance Date: 11 Dec 2017. This document contains color . Journal article published in...broad adoption of this technique. In addition, it suffers from poor spatial resolution (~500 nm) and limited angular field of view (FOV) (typically 10...EBSD (or less commonly SACP) the specimen can be tilted into a “ two -beam” condition19. By capturing BSE images at several condi- tions, the Burger’s

Physics-based simulation models for EBSD: advances and challenges

NASA Astrophysics Data System (ADS)

Winkelmann, A.; Nolze, G.; Vos, M.; Salvat-Pujol, F.; Werner, W. S. M.

2016-02-01

EBSD has evolved into an effective tool for microstructure investigations in the scanning electron microscope. The purpose of this contribution is to give an overview of various simulation approaches for EBSD Kikuchi patterns and to discuss some of the underlying physical mechanisms.

A Coupled EBSD/EDS Method to Determine the Primary- and Secondary-Alpha Textures in Titanium Alloys With Duplex Microstructures (Preprint)

DTIC Science & Technology

2007-07-01

primary and secondary alpha in micrographs and thus to correlate microstructural features and texture data [3- 6 ]. For instance, Germain, et al. [3, 4 ...Following electropolishing , the sample was mounted 7/3/2007 6 on the tilting stage inside an XL30 field-emission-gun scanning-electron-microscope (FEG...AFRL-RX-WP-TP-2008-4338 A COUPLED EBSD/EDS METHOD TO DETERMINE THE PRIMARY–AND SECONDARY–ALPHA TEXTURES IN TITANIUM ALLOYS WITH DUPLEX

Comprehensive Characterization of Extended Defects in Semiconductor Materials by a Scanning Electron Microscope.

PubMed

Hieckmann, Ellen; Nacke, Markus; Allardt, Matthias; Bodrov, Yury; Chekhonin, Paul; Skrotzki, Werner; Weber, Jörg

2016-05-28

Extended defects such as dislocations and grain boundaries have a strong influence on the performance of microelectronic devices and on other applications of semiconductor materials. However, it is still under debate how the defect structure determines the band structure, and therefore, the recombination behavior of electron-hole pairs responsible for the optical and electrical properties of the extended defects. The present paper is a survey of procedures for the spatially resolved investigation of structural and of physical properties of extended defects in semiconductor materials with a scanning electron microscope (SEM). Representative examples are given for crystalline silicon. The luminescence behavior of extended defects can be investigated by cathodoluminescence (CL) measurements. They are particularly valuable because spectrally and spatially resolved information can be obtained simultaneously. For silicon, with an indirect electronic band structure, CL measurements should be carried out at low temperatures down to 5 K due to the low fraction of radiative recombination processes in comparison to non-radiative transitions at room temperature. For the study of the electrical properties of extended defects, the electron beam induced current (EBIC) technique can be applied. The EBIC image reflects the local distribution of defects due to the increased charge-carrier recombination in their vicinity. The procedure for EBIC investigations is described for measurements at room temperature and at low temperatures. Internal strain fields arising from extended defects can be determined quantitatively by cross-correlation electron backscatter diffraction (ccEBSD). This method is challenging because of the necessary preparation of the sample surface and because of the quality of the diffraction patterns which are recorded during the mapping of the sample. The spatial resolution of the three experimental techniques is compared.

Comprehensive Characterization of Extended Defects in Semiconductor Materials by a Scanning Electron Microscope

PubMed Central

Hieckmann, Ellen; Nacke, Markus; Allardt, Matthias; Bodrov, Yury; Chekhonin, Paul; Skrotzki, Werner; Weber, Jörg

2016-01-01

Extended defects such as dislocations and grain boundaries have a strong influence on the performance of microelectronic devices and on other applications of semiconductor materials. However, it is still under debate how the defect structure determines the band structure, and therefore, the recombination behavior of electron-hole pairs responsible for the optical and electrical properties of the extended defects. The present paper is a survey of procedures for the spatially resolved investigation of structural and of physical properties of extended defects in semiconductor materials with a scanning electron microscope (SEM). Representative examples are given for crystalline silicon. The luminescence behavior of extended defects can be investigated by cathodoluminescence (CL) measurements. They are particularly valuable because spectrally and spatially resolved information can be obtained simultaneously. For silicon, with an indirect electronic band structure, CL measurements should be carried out at low temperatures down to 5 K due to the low fraction of radiative recombination processes in comparison to non-radiative transitions at room temperature. For the study of the electrical properties of extended defects, the electron beam induced current (EBIC) technique can be applied. The EBIC image reflects the local distribution of defects due to the increased charge-carrier recombination in their vicinity. The procedure for EBIC investigations is described for measurements at room temperature and at low temperatures. Internal strain fields arising from extended defects can be determined quantitatively by cross-correlation electron backscatter diffraction (ccEBSD). This method is challenging because of the necessary preparation of the sample surface and because of the quality of the diffraction patterns which are recorded during the mapping of the sample. The spatial resolution of the three experimental techniques is compared. PMID:27285177

Evolution of microstructure in stainless martensitic steel for seamless tubing

NASA Astrophysics Data System (ADS)

Pyshmintsev, I. Yu.; Bityukov, S. M.; Pastukhov, V. I.; Danilov, S. V.; Vedernikova, L. O.; Lobanov, M. L.

2017-12-01

Scanning electron microscopy with orientation analysis by the electron backscatter diffraction (EBSD) method is used to study microstructures and textures formed in the 0.08C-13Cr-3Ni-Mo-V-Nb steel through seamless tube production route: after hot deformation by extrusion; after quenching from various temperatures and subsequent high tempering. It is shown that the martensitic microstructure formed both after hot deformation and after quenching is characterized by the presence of deformation crystallographic texture, which is predetermined by the texture of austenite. The effect of heat treatment on texture, packet refinement, lath width, precipitation of carbides and Charpy impact energy is analyzed.

A comparison of EBSD based strain indicators for the study of Fe-3Si steel subjected to cyclic loading

DOE Office of Scientific and Technical Information (OSTI.GOV)

Schayes, Claire; Valeo Engine Electrical Systems, 2 Rue André Boulle, 94046 Créteil; Bouquerel, Jérémie, E-mail: jeremie.bouquerel@univ-lille1.fr

The current work aims at proposing an EBSD-based indicator for fatigue damage of a Fe-3Si steel. At the same time direct observation of dislocation structures is provided by electron channelling contrast imaging (ECCI). The investigation consisted in processing the EBSD data from patterns collected on specimen subjected to low cycle fatigue. It revealed two different regimes depending on the applied total strain variation which is explained by the identification of the dislocations structures and their evolution. At low strain variation, strain accommodation occurs by planar glide of dislocations uniformly distributed throughout the grains. No misorientation evolution is observed. At highermore » strain variation, the vein-channel structure is observed within the grain and the wall-channel structure in the vicinity of grain boundaries. The misorientation between these two dislocation structures is evaluated at about 0.7° which is detected by the EBSD analyses and explains the increase of the different misorientation based criteria. The EBSD study enables also the prediction of crack initiation mode. Finally, this study points out the limits of the EBSD technique as no misorientation evolution is detected at small strain variation. Indeed, the lattice distortion is too weak to be detected by conventional EBSD. - Highlights: • Microstructure investigation of the fatigue behaviour of an iron-silicon steel • Use of cECCI to investigate the fatigue dislocations structures • Characterisation of local plastic accommodation through EBSD misorientation criteria.« less

Sub-µm structure and volatile distribution of shocked lunar apatite

NASA Astrophysics Data System (ADS)

Cernok, A.; White, L. F.; Darling, J.; Dunlop, J.; Fougerouse, D.; William, R. D. A.; Reddy, S.; Saxey, D. W.; Zhao, X.; Franchi, I.; Anand, M.

2017-12-01

Apatite is a key mineral broadly used for studying volatiles in planetary materials. Most studies in this recent frontier of planetary exploration focus on volatile content and respective isotopic composition in apatite. However, there is an imperative to contextualize geochemical data with impact-induced features, given that most planetary materials experienced at least some shock deformation. This study aims at understanding the effect of high-level shock deformation on volatile distribution in apatite from lunar highlands samples. Combining Electron Backscatter Diffraction (EBSD), NanoSIMS and Atom Probe Microscopy (APM) analyses we are gaining an insight into the µm- and nm-scale structural variation in apatite from a shocked, maskelynite- and impact-melt-bearing norite. EBSD revealed degraded crystallinity, high density of low angle grain boundaries and domains of sub-µm granular features that appear amorphous at this length scales ( 80 x 40 nm). Texture component maps show up to 25° misorientation within a single grain - evidence of severe crystal-plastic deformation, but with no obvious evidence of recrystallization. APM revealed complex microstructure of the apparently amorphous domains defined by well developed, straight to slightly curved grain boundaries meeting at 120° triple junctions. This equilibrium texture is probably accommodated by annealing and recrystallization of apatite due to the post-shock heating. Crystallites range in size from 50 to 100 nm. Grain boundaries are defined by segregation of Mg, Si and Fe impurities, which possibly originate from surrounding phases. Cl and F show homogenous distribution over the length scale of the APM analysis (1 to 500 nm). H2O content measurements of 250-600 ppm by NanoSIMS are consistent with the lower range of previously reported values for this rock, with no obvious correlation with the level of crystallinity. δD values are confirmed to be terrestrial-like and relatively constant. These preliminary data suggest that impact event(s) either did not disturb the volatile distribution and composition of homogenous magmatic apatite, or that it induced diffusion and homogenisation of primary volatile species during annealing. Apatites in a range of variably shocked lunar samples are currently being examined to further clarify this question.

A quasi-in-situ EBSD observation of the transformation from rolling texture to recrystallization texture in V-4Cr-4Ti alloy

DOE Office of Scientific and Technical Information (OSTI.GOV)

Peng, Lixia

Recrystallization texture evolution of rolled V-4Cr-4Ti alloy has been investigated by quasi-in-situ EBSD (electron back-scattering diffraction) method. Concurrently, the precipitates were characterized by SEM (Scanning Electron Microscopy). It was found that both the initial rolling textures and the distribution of the precipitates affected the formation of the recrystallization texture. It was revealed that the texture transformations of (558) 〈110〉 + (665) 〈110〉 to (334) 〈483〉 + (665) 〈1 1 2.4〉 were possibly attributed to the selective drag induced by the sparsely dispersed Ti-rich precipitates. While the densely distributed Ti-rich precipitates were responsible for the randomized recrystallization texture. Finally, when themore » precipitates were absent, the orientation changes from (112) 〈110〉 and (558) 〈110〉 to (111) 〈112〉 and (001) <110> to (001) <520> were observed. - Highlights: • Micro recrystallization texture evolution in V-4Cr-4Ti alloys is reported for the first time. • The volume fraction of Ti-rich precipitates has significant effect on the recrystallization texture evolution. • The dissolution of the Ti-rich precipitates above 1100 °C induces the strengthening of (111) <112> texture.« less

Electron-beam-induced current at absorber back surfaces of Cu(In,Ga)Se{sub 2} thin-film solar cells

DOE Office of Scientific and Technical Information (OSTI.GOV)

Kavalakkatt, J.; Abou-Ras, D., E-mail: daniel.abou-ras@helmholtz-berlin.de; Nichterwitz, M.

2014-01-07

The present work reports on investigations of the influence of the microstructure on electronic properties of Cu(In,Ga)Se{sub 2} (CIGSe) thin-film solar cells. For this purpose, ZnO/CdS/CIGSe stacks of these solar cells were lifted off the Mo-coated glass substrates. The exposed CIGSe backsides of these stacks were investigated by means of electron-beam-induced current (EBIC) and cathodoluminescence (CL) measurements as well as by electron backscattered diffraction (EBSD). EBIC and CL profiles across grain boundaries (GBs), which were identified by EBSD, do not show any significant changes at Σ3 GBs. Across non-Σ3 GBs, on the other hand, the CL signals exhibit local minimamore » with varying peak values, while by means of EBIC, decreased and also increased short-circuit current values are measured. Overall, EBIC and CL signals change across non-Σ3 GBs always differently. This complex situation was found in various CIGSe thin films with different [Ga]/([In]+[Ga]) and [Cu]/([In]+[Ga]) ratios. A part of the EBIC profiles exhibiting reduced signals across non-Σ3 GBs can be approximated by a simple model based on diffusion of generated charge carriers to the GBs.« less

Room temperature creep behavior of Ti–Nb–Ta–Zr–O alloy

DOE Office of Scientific and Technical Information (OSTI.GOV)

Zhang, Wei-dong

The room temperature creep behavior and deformation mechanisms of a Ti–Nb–Ta–Zr–O alloy, which is also called “gum metal”, were investigated with the nanoindentation creep and conventional creep tests. The microstructure was observed with electron backscattered diffraction analysis (EBSD) and transmission electron microscopy (TEM). The results show that the creep stress exponent of the alloy is sensitive to cold deformation history of the alloy. The alloy which was cold swaged by 85% shows high creep resistance and the stress exponent is approximately equal to 1. Microstructural observation shows that creep process of the alloy without cold deformation is controlled by dislocationmore » mechanism. The stress-induced α' martensitic phase transformation also occurs. The EBSD results show that the grain orientation changes after the creep tests, and thus, the creep of the cold-worked alloy is dominated by the shear deformation of giant faults without direct assistance from dislocations. - Highlights: •Nanoindentation was used to investigate room temperature creep behavior of gum metal. •The creep stress exponent of gum metal is sensitive to the cold deformation history. •The creep stress exponent of cold worked gum metal is approximately equal to 1. •The creep of the cold-worked gum metal is governed by the shear deformation of giant faults.« less

Microstructural evolution of garnet in a greenschist facies transpression zone

NASA Astrophysics Data System (ADS)

Massey, M. A.; Prior, D. J.; Moecher, D. P.

2007-12-01

Natural observations, laboratory experiments, and theoretical modeling support the interpretation of Grt plasticity in the lower crust and upper mantle; however, these processes are thought to be of little importance in shallow to middle crustal levels. Multiple textural varieties of Grt from the western boundary (Mt. Dumplin high strain zone) of an upper greenschist facies dextral transpression zone in southern New England, USA, display mesoscopic and microscopic evidence of syn-tectonic deformation and recrystallization. These microstructures were examined further by optical microscopy, electron probe microanalysis, orientation contrast imaging (OCI), and automated electron backscatter diffraction (EBSD) in order to understand possible low-grade deformation mechanisms and their significance. The N-S-striking shear zone dips steeply W, the mylonitic foliation is defined by aligned Ms- Chl-Rt, layers of Qtz and fine-grained Grt; Qtz-Chl-Ms and fine-grained Grt aggregates define lineations that plunge moderately SW. S-C-C¡¦ fabrics, asymmetric folds and porphyroclasts (delta- and sigma-type) are well developed on foliation-normal/lineation-parallel planes, and display sinistral kinematics; surfaces normal to foliation and normal to lineation exhibit strong asymmetries that indicate normal motion. Pre-tectonic mineral parageneses consist of St pseudomorphed by Chl-Ms-Ctd, Als pseudomorphed by Ms, and coarse-grained Grt and Ab porphyroclasts with associated asymmetric tails. Grt is manifest as three types: 1) equant Grt porphyroclasts; 2) elongate Grt aggregates consisting of 50-100 Ým equant Grt porphyroblasts; 3) type 1-type 2 transitional Grt morphology. Elemental x-ray mapping of Ca and Mn reveals at least two periods of growth in Grt types 1 and 3, and one period of growth in type 2 that correlates with type 1 and 3 rims; Mg is completely homogenized. Detailed mapping of type 3 Grt cores reveals ¡¥fractured¡¦ Ca-enriched cores ¡¥healed¡¦ with Ca- depleted composition. OCI of type 1 Grt shows no internal substructure. OCI of type 2 Grt also shows rare internal substructure (finer-grained equant inclusions with low angle boundaries), and EBSD shows aggregates have CPO symmetrical to tectonic fabric (parallel to lineation), high angle grain boundaries, and neighbor- neighbor grain pairs correlate with random grain pair distributions. Type 2 Grt also displays ¡¥stacking¡¦ structures where individual porphyroblasts are stacked vertically and grain boundaries are at low angle. OCI of type 3 Grt shows considerable internal substructure of three varieties: A) substructure boundaries that coincide with Ca-depleted compositions in cores; B) 50-100 Ým equant substructures included in rims; C) substructure boundaries in rims that ¡¥nucleate¡¦ from substructure A boundaries in cores. Detailed EBSD traverses across all substructure boundaries indicate rotation around rational crystallographic axes. Observations suggest that early amphibolite facies Grt (type 1 and 3 cores) was deformed non-penetratively by plastic deformation or sub-critical fracture (type 3 Grt, substructure A). Type 2 Grt nucleated pre- to syn-tectonically, at least partially through the consumption of type 3 Grt porphyroclasts, and was included in type 1 and 3 rims by rigid body rotations (substructure B). Substructures C in type 3 Grt rims are inherited from pre-existing crystallographic anisotropies in cores (substructure A). Additionally, type 2 Grt was deformed syn-tectonically to produce CPOs, likely as a result of flattening associated with transpression.

Microstructure Evolution During Warm Working of Ti-6Al-4V with a Colony Alpha Microstructure (Preprint)

DTIC Science & Technology

2008-09-01

6 maps such as those shown in Fig. 4 ; typical examples of the cumulative misorientation are given in Figs. 5 and 6 , respectively...misorientation line scans shown in Figs. 5 and 6 . Fig. 5. Typical line scans from EBSD maps in Fig. 4 showing the variation of orientation over a long...e g 0 2 4 6 8 10 12 14 16 (b) Distance, μm 0 20 40 60 80 100 C u m u l a t i v e m i s o r i e n t a t i o n , d e g 0 5 10 15

A diffraction based study of the deformation mechanisms in anomalously ductile B2 intermetallics

NASA Astrophysics Data System (ADS)

Mulay, Rupalee Prashant

For many decades, the brittle nature of most intermetallic compounds (e.g. NiAl) has been the limiting factor in their practical application. Many B2 (CsCl prototypical structure) intermetallics are known to exhibit slip on the <001>{110} slip mode, which provides only 3 independent slip systems and, hence, is unable to satisfy the von Mises (a.k.a. Taylor) criterion for polycrystalline ductility. As a result, inherent polycrystalline ductility is unexpected. Recent discovery of a number of ductile B2 intermetallics has raised questions about possible violation of the von Mises criterion by these alloys. These ductile intermetallic compounds are MR (metal (M) combined with a rare earth metal or group IV refractory metal (R)) alloys and are stoichiometric, ordered compounds. Single crystal slip trace analyses have only identified the presence of <100>{011} or <100>{010} slip systems. More than 100 other B2 MR compounds are known to exist and many of them have already been shown to be ductile (e.g., CuY, AgY, CuDy, CoZr, CoTi, etc.). Furthermore, these alloys exhibit a large Bauschinger effect. The present work uses several diffraction based techniques including electron back scattered diffraction (EBSD), X-ray diffraction (XRD) and in-situ neutron diffraction; in conjunction with scanning electron microscopy (SEM), transmission electron microscopy (TEM), mechanical testing, and crystal plasticity modeling, to elucidate the reason for ductility in select B2 alloys, explore the spread of this ductility over the B2 family, and understand the Bauschinger effect in these alloys. Several possible explanations (e.g., slip of <111> dislocations, strong texture, phase transformations and twinning) for the anomalous ductility were explored. An X-ray diffraction based analysis ruled out texture, phase purity and departure from order as explanations for the anomalous ductility in MR alloys. In-situ neutron diffraction and post deformation SEM, EBSD, and TEM were unable to detect any evidence for phase transformations in CoTi and CoZr. Also, post deformation characterization did not reveal any evidence of twinning. However, TEM based g·b analysis and EBSD based in-grain misorientation axis (IGMA) analysis showed that beyond a transition in the strain hardening behavior in CoTi, slip modes involving dislocations with <110> and <111> Burgers vectors are activated. The slip of such dislocations can reduce stress concentrations that could otherwise lead to premature fracture, thus providing a satisfying explanation for the anomalous ductility of CoTi and related compounds, like CoZr. Dislocation self-energy calculations accounting for elastic anisotropy suggest that the choice of slip direction in these alloys is mobility-, rather than source-, limited. The reach of this "ductilizing effect" over B2 alloys was explored by producing, characterizing, and testing a number of simple metal-rare earth metal compounds, namely MgY, MgNd and MgCe. MgR intermetallics with the B2 structure were found to be brittle and exhibit a cleavage type fracture indicating that the ductilizing effect is not as widespread as was initially thought. MgY and MgNd were found to primarily cleave along the {100} planes, while MgCe was found to cleave on the {111} planes. A large Bauschinger effect was observed in several of the anomalously ductile B2 compounds, such that the material actually begins to yield in the reverse direction on unloading. When only the primary slip mode <100>{011} is active in CoZr (prior to a transition in strain hardening), the buildup of intergranular stresses is large and is chiefly responsible for the observed Bauschinger effect. However, past the aforementioned transition in strain hardening, the effect of intergranular stresses diminishes. The results demonstrate that the activation of hard, secondary slip modes causes the internal strains to develop more uniformly among the grains, thus reducing the intergranular stresses which cause the Bauschinger effect. Crystal plasticity modeling, which accounts for the initial paucity of independent slip modes and allows for the activation of complementary hard slip modes, reproduces these trends in the Bauschinger effect and provides additional evidence that the experimental observations have correctly identified the cause of the anomalous ductility.

Role of deformation temperature on the evolution and heterogeneity of texture during equal channel angular pressing of magnesium

DOE Office of Scientific and Technical Information (OSTI.GOV)

Biswas, Somjeet, E-mail: somjeetbiswas@gmail.com; Department of Materials Engineering, Indian Institute of Science, Bangalore 560012; Laboratory of Excellence on Design of Alloy Metals for low-mAss Structures

Investigations on texture evolution and through-thickness texture heterogeneity during equal channel angular pressing (ECAP) of pure magnesium at 200 °C, 150 °C and room temperature (RT) was carried out by neutron, high energy synchrotron X-ray and electron back-scatter diffraction. Irrespective of the ECAP temperature, a distinctive basal (B) and pyramidal (C{sub 2}) II type of fibers forms. The texture differs in the bottom 1 mm portion, where the B-fiber is shifted ~ 55° due to negative shear attributed to friction. - Highlights: • ECAP of magnesium was carried out at 200 °C, 150 °C and room temperature. • Microstructure andmore » micro-texture evolution was examined using EBSD in FEG–SEM. • Bulk-texture was studied using neutron diffraction and compared with micro-texture. • Through thickness texture heterogeneity was observed by synchrotron radiation. • Changes in these parameters with respect to deformation temperature are discussed.« less

Hexagonal OsB 2: Sintering, microstructure and mechanical properties

DOE PAGES

Xie, Zhilin; Lugovy, Mykola; Orlovskaya, Nina; ...

2015-02-07

In this study, the metastable high pressure ReB 2-type hexagonal OsB 2 bulk ceramics was produced by spark plasma sintering. The phase composition, microstructure, and mechanical behavior of the sintered OsB 2 were studied by X-ray diffraction, optical microscopy, TEM, SEM, EDS, and nanoindentation. The produced ceramics was rather porous and contained a mixture of hexagonal (~80 wt.%) and orthorhombic (~20 wt.%) phases as identified by X-ray diffraction and EBSD analysis. Two boron-rich phases, which do not contain Os, were also identified by TEM and SEM/EDS analysis. Nanoindentation measurements yielded a hardness of 31 ± 9 GPa and Young’s modulusmore » of 574 ± 112 GPa, indicating that the material is rather hard and very stiff; but, it is very prone to crack formation and propagation, which is indicative of a very brittle nature of this material. Improvements in the sintering regime are required in order to produce dense, homogeneous and single phase hexagonal OsB 2 bulk ceramics.« less

Large-size TlBr single crystal growth and defect study

NASA Astrophysics Data System (ADS)

Zhang, Mingzhi; Zheng, Zhiping; Chen, Zheng; Zhang, Sen; Luo, Wei; Fu, Qiuyun

2018-04-01

Thallium bromide (TlBr) is an attractive semiconductor material for fabrication of radiation detectors due to its high photon stopping power originating from its high atomic number, wide band gap and high resistivity. In this paper the vertical Bridgman method was used for crystal growth and TlBr single crystals with diameter of 15 mm were grown. X-ray diffraction (XRD) was used to identify phase and orientation. Electron backscatter diffraction (EBSD) was used to investigate crystal microstructure and crystallographic orientation. The optical and electric performance of the crystal was characterized by infrared (IR) transmittance spectra and I-V measurement. The types of point defects in the crystals were investigated by thermally stimulated current (TSC) spectra and positron annihilation spectroscopy (PAS). Four types of defects, with ionization energy of each defect fitting as follows: 0.1308, 0.1540, 0.3822 and 0.538 eV, were confirmed from the TSC result. The PAS result showed that there were Tl vacancies in the crystal.

Measurements of Shock Effects Recorded by Hayabusa Samples

NASA Technical Reports Server (NTRS)

Zolensky, Michael; Mikouchi, Takashi; Hagiya, Kenji; Ohsumi, Kazumasa; Martinez, James; Komatsu, Mutsumi; Chan, Queenie H-.S.

2015-01-01

We requested and have been approved for 5 Hayabusa samples in order definitively establish the degree of shock experienced by the regolith of asteroid Itokawa, and to devise a bridge between shock determinations by standard light optical petrography, crystal structures as determined by synchrotron X-ray diffraction (SXRD), and degree of crystallinity as determined by electron back-scattered diffraction (EBSD) [1,2]. As of the writing of this abstract we are awaiting the approved samples. We propose measurements of astromaterial crystal structures and regolith processes. The proposed research work will improve our understanding of how small, primitive solar system bodies formed and evolved, and improve understanding of the processes that determine the history and future of habitability of environments on other solar system bodies. The results of the proposed research will directly enrich the ongoing asteroid and comet exploration missions by NASA, JAXA and ESA, and broaden our understanding of the origin and evolution of small bodies in the early solar system, and elucidate the nature of asteroid and comet regolith.

Measurements of Shock Effects Recorded by Itokawa Samples

NASA Technical Reports Server (NTRS)

Zolensky, Michael; Mikouchi, Takashi; Hagiya, Kenji; Ohsumi, Kazumasa; Martinez, James; Komatsu, Mutsumi; Chan, Queenie H-.S.

2016-01-01

We requested and have been approved for 5 Hayabusa samples in order definitively establish the degree of shock experienced by the regolith of asteroid Itokawa, and to devise a bridge between shock determinations by standard light optical petrography, crystal structures as determined by synchrotron X-ray diffraction (SXRD), and degree of crystallinity as determined by electron back-scattered diffraction (EBSD). As of the writing of this abstract we are awaiting the approved samples. We propose measurements of astromaterial crystal structures and regolith processes. The proposed research work will improve our understanding of how small, primitive solar system bodies formed and evolved, and improve understanding of the processes that determine the history and future of habitability of environments on other solar system bodies. The results of the proposed research will directly enrich the ongoing asteroid and comet exploration missions by NASA, JAXA and ESA, and broaden our understanding of the origin and evolution of small bodies in the early solar system, and elucidate the nature of asteroid and comet regolith.

Dependence of Crystallographic Orientation on Pitting Corrosion Behavior of Ni-Fe-Cr Alloy 028

NASA Astrophysics Data System (ADS)

Zhang, LiNa; Szpunar, Jerzy A.; Dong, JianXin; Ojo, Olanrewaju A.; Wang, Xu

2018-06-01

The influence of crystallographic orientation on the pitting corrosion behavior of Ni-Fe-Cr alloy 028 was studied using a combination of X-ray diffraction (XRD), electron backscatter diffraction (EBSD), potentiodynamic polarization technique, and atomic force microscopy (AFM). The results show that there is anisotropy of pitting corrosion that strongly depends on crystallographic orientation of the surface plane. The distribution of pit density in a standard stereographic triangle indicates that the crystallographic planes close to {100} are more prone to pitting corrosion compared to planes {110} and {111}. The surface energy calculation of (001) and (111) shows that the plane with a high atomic packing density has a low surface energy with concomitant strong resistance to pitting corrosion. A correlation function between crystallographic orientation and pitting corrosion susceptibility suggests a method that not only predicts the pitting resistance of known textured materials, but also could help to improve corrosion resistance by controlling material texture.

Texture evolution in Oxide Dispersion Strengthened (ODS) steel tubes during pilgering process

NASA Astrophysics Data System (ADS)

Vakhitova, E.; Sornin, D.; Barcelo, F.; François, M.

2017-10-01

Oxide Dispersion Strengthened (ODS) steels are foreseen as fuel cladding material in the coming generation of Sodium Fast Reactors (SFR). Cladding tubes are manufactured by hot extrusion and subsequent cold forming steps. In this study, a 9 wt% Cr ODS steel exhibiting α-γ phase transformation at high temperature is cold formed under industrial conditions with a large section reduction in two pilgering steps. The influence of pilgering process parameters and intermediate heat treatment on the microstructure evolution is studied experimentally using Electron Backscattering Diffraction (EBSD) and X-ray Diffraction (XRD) methods. Pilgered samples show elongated grains and a high texture formation with a preferential orientation along the rolling direction. During the heat treatment, grain morphology is recovered from elongated grains to almost equiaxed ones, while the well-known α-fiber texture presents an unexpected increase in intensity. The remarkable temperature stability of this fiber is attributed to a crystallographic structure memory effect during phase transformations.

Grain growth mechanism and magnetic properties in L10-FePt thin films

NASA Astrophysics Data System (ADS)

Li, W.; Chen, L.

2017-08-01

This paper focuses on the grain growth mechanisms and magnetic properties of FePt thin films during an annealing process. The grain size and grain orientation distribution have been quantitatively investigated by electron backscatter diffraction (EBSD), and the grain growth kinetics of thin films were described by the phenomenological kinetic grain growth model. The results show that the grain growth exponent and activation energy of the FePt thin films were 4.26 and 136 kJ/mol respectively, indicating that the grain growth mechanism is mainly controlled by the stochastic jumping of atoms crossing the grain boundaries. X-ray diffraction (XRD) results show that disorder-order transformation was concurrent with grain growth during the annealing process, slowing down the velocity of grain growth. The hysteresis loops reveal that the out-of-plane coercivity and squareness is enhanced with increasing annealing temperature and this can be attributed to the improvement of L10-ordered phase volume fraction and texture intensity.

Mechanism of Martensitic to Equiaxed Microstructure Evolution during Hot Deformation of a Near-Alpha Ti Alloy

NASA Astrophysics Data System (ADS)

Shams, Seyed Amir Arsalan; Mirdamadi, Shamsoddin; Abbasi, Seyed Mahdi; Kim, Daehwan; Lee, Chong Soo

2017-06-01

In this study, mechanisms of microstructural evolution during hot deformation of Ti-1100 were investigated by EBSD analysis. Misorientation angle distribution of initial microstructure showed that diffusionless martensitic phase transformation in Ti-1100 obeys Burgers orientation relationship, and most of the high-angle-grain boundaries consist of angles of 60 and 63 deg. Calculated activation energy of hot deformation ( 338 kJ/mol) and EBSD grain boundary maps revealed that continuous dynamic recrystallization (CDRX) is the dominant mechanism during hot compression at 1073 K (800 °C) and strain rate of 0.005 s-1. At a temperature range of 1073 K to 1173 K (800 °C to 900 °C), not only the array of variants lying perpendicular to compression axis but also CDRX contributes to flow softening. Increasing the rolling temperature from 1123 K to 1273 K (850 °C to 1000 °C) brought about changes in spheroidization mechanism from CDRX to conventional boundary splitting and termination migration correlated with the higher volume fraction of beta phase at higher temperatures.

On the shock response of the magnesium alloy Elektron 675

NASA Astrophysics Data System (ADS)

Hazell, Paul; Appleby-Thomas, Gareth; Siviour, Clive; Wielewski, Euan

2011-06-01

Alloying elements such as aluminium, zinc or rare-earths allow precipitation hardening of magnesium (Mg). The low densities of such strengthened Mg alloys have led to their adoption as aerospace materials and (more recently) they are being considered as armour materials. Consequently, understanding their response to high-strain rate loading is becoming increasingly important. Here, the plate-impact technique was employed to measure longitudinal stress evolution in armour-grade wrought Mg-alloy Elektron 675 under 1D shock loading. The strength and spall behaviour was interrogated, with an estimate made of the material's Hugoniot elastic limit. Finally, electron backscatter diffraction (EBSD) techniques were employed to investigate post-shock microstructural changes.

Monte Carlo modeling of recrystallization processes in α-uranium

DOE PAGES

Steiner, M. A.; McCabe, R. J.; Garlea, E.; ...

2017-08-01

In this study, starting with electron backscattered diffraction (EBSD) data obtained from a warm clock-rolled α-uranium deformation microstructure, a Potts Monte Carlo model was used to simulate static site-saturated recrystallization while testing a number of different conditions for the assignment of recrystallized nuclei within the microstructure. The simulations support observations that recrystallized nuclei within α-uranium form preferentially on non-twin high-angle grain boundary sites at 450 °C, and demonstrate that the most likely nucleation sites on these boundaries can be identified by the surrounding degree of Kernel Average Misorientation (KAM), which may be considered as a proxy for the local geometricallymore » necessary dislocation (GND) density.« less

Effect of Microstructure on Diffusional Solidification of 4343/3005/4343 Multi-Layer Aluminum Brazing Sheet

NASA Astrophysics Data System (ADS)

Tu, Yiyou; Tong, Zhen; Jiang, Jianqing

2013-04-01

The effect of microstructure on clad/core interactions during the brazing of 4343/3005/4343 multi-layer aluminum brazing sheet was investigated employing differential scanning calorimetry (DSC) and electron back-scattering diffraction (EBSD). The thickness of the melted clad layer gradually decreased during the brazing operation. It could be completely removed isothermally as a result of diffusional solidification at the brazing temperature. During the brazing cycle, the rate of loss of the melt in the brazing sheet, with small equiaxed grains' core layer, was higher than that with the core layer consisting of elongated large grains. The difference in microstructure affected the amount of liquid formed during brazing.

Laboratory Instruments Available to Support Space Station Researchers at Marshall Space Flight Center

NASA Technical Reports Server (NTRS)

Panda, Binayak; Gorti, Sridhar

2013-01-01

A number of research instruments are available at NASA's Marshall Space Flight Center (MSFC) to support ISS researchers and their investigations. These modern analytical tools yield valuable and sometimes new informative resulting from sample characterization. Instruments include modern scanning electron microscopes equipped with field emission guns providing analytical capabilities that include angstron-level image resolution of dry, wet and biological samples. These microscopes are also equipped with silicon drift X-ray detectors (SDD) for fast yet precise analytical mapping of phases, as well as electron back-scattered diffraction (EBSD) units to map grain orientations in crystalline alloys. Sample chambers admit large samples, provide variable pressures for wet samples, and quantitative analysis software to determine phase relations. Advances in solid-state electronics have also facilitated improvements for surface chemical analysis that are successfully employed to analyze metallic materials and alloys, ceramics, slags, and organic polymers. Another analytical capability at MSFC is a mganetic sector Secondary Ion Mass Spectroscopy (SIMS) that quantitatively determines and maps light elements such as hydrogen, lithium, and boron along with their isotopes, identifies and quantifies very low level impurities even at parts per billion (ppb) levels. Still other methods available at MSFC include X-ray photo-electron spectroscopy (XPS) that can determine oxidation states of elements as well as identify polymers and measure film thicknesses on coated materials, Scanning Auger electron spectroscopy (SAM) which combines surface sensitivity, spatial lateral resolution (approximately 20 nm), and depth profiling capabilities to describe elemental compositions in near surface regions and even the chemical state of analyzed atoms. Conventional Transmission Electron Microscope (TEM) for observing internal microstructures at very high magnifications and the Electron Probe Micro-analyzer (EPMA) for very precise microanalysis are available as needed by the researcher. Space Station researchers are invited to work with MSFC in analyzing their samples using these techniques.

Microstructure and mechanical behavior of direct metal laser sintered Inconel alloy 718

DOE Office of Scientific and Technical Information (OSTI.GOV)

Smith, Derek H.; Bicknell, Jonathan; Jorgensen, Luke

2016-03-15

In this paper, we investigate microstructure and quasi-static mechanical behavior of the direct metal laser sintered Inconel 718 superalloy as a function of build direction (BD). The printed material was further processed by annealing and double-aging, hot isostatic pressing (HIP), and machining. We characterize porosity fraction and distribution using micro X-ray computed tomography (μXCT), grain structure and crystallographic texture using electron backscattered diffraction (EBSD), and mechanical response in quasi-static tension and compression using standard mechanical testing at room temperature. Analysis of the μXCT imaging shows that majority of porosity develops in the outer layer of the printed material. However, porositymore » inside the material is also present. The EBSD measurements reveal formation of columnar grains, which favor < 001 > fiber texture components along the BD. These measurements also show evidence of coarse-grained microstructure present in the samples treated by HIP. Finally, analysis of grain boundaries reveal that HIP results in a large number of annealing twins compared to that in samples that underwent annealing and double-aging. The yield strength varies with the testing direction by approximately 7%, which is governed by a combination of grain morphology and crystallographic texture. In particular, we determine tension–compression asymmetry in the yield stress as well as anisotropy of the material flow during compression. We find that HIP lowers yield stress but improves ductility relative to the annealed and aged material. These results are discussed and critically compared with the data reported for wrought material in the same condition. - Highlights: • Microstructure and mechanical properties of DMLS Inconel 718 are studied in function of build direction. • Inhomogeneity of microstructure in the material in several conditions is quantified by μXCT and EBSD. • Anisotropy and asymmetry in the mechanical response are determined by tension and compression testing.« less

Effects of homogenization treatment on recrystallization behavior of 7150 aluminum sheet during post-rolling annealing

DOE Office of Scientific and Technical Information (OSTI.GOV)

Guo, Zhanying; Department of Applied Science, University of Québec at Chicoutimi, Saguenay, QC G7H 2B1; Zhao, Gang

2016-04-15

The effects of two homogenization treatments applied to the direct chill (DC) cast billet on the recrystallization behavior in 7150 aluminum alloy during post-rolling annealing have been investigated using the electron backscatter diffraction (EBSD) technique. Following hot and cold rolling to the sheet, measured orientation maps, the recrystallization fraction and grain size, the misorientation angle and the subgrain size were used to characterize the recovery and recrystallization processes at different annealing temperatures. The results were compared between the conventional one-step homogenization and the new two-step homogenization, with the first step being pretreated at 250 °C. Al{sub 3}Zr dispersoids with highermore » densities and smaller sizes were obtained after the two-step homogenization, which strongly retarded subgrain/grain boundary mobility and inhibited recrystallization. Compared with the conventional one-step homogenized samples, a significantly lower recrystallized fraction and a smaller recrystallized grain size were obtained under all annealing conditions after cold rolling in the two-step homogenized samples. - Highlights: • Effects of two homogenization treatments on recrystallization in 7150 Al sheets • Quantitative study on the recrystallization evolution during post-rolling annealing • Al{sub 3}Zr dispersoids with higher densities and smaller sizes after two-step treatment • Higher recrystallization resistance of 7150 sheets with two-step homogenization.« less

Growth characteristics of primary M7C3 carbide in hypereutectic Fe-Cr-C alloy.

PubMed

Liu, Sha; Zhou, Yefei; Xing, Xiaolei; Wang, Jibo; Ren, Xuejun; Yang, Qingxiang

2016-09-06

The microstructure of the hypereutectic Fe-Cr-C alloy is observed by optical microscopy (OM). The initial growth morphology, the crystallographic structure, the semi-molten morphology and the stacking faults of the primary M7C3 carbide are observed by scanning electron microscopy (SEM) and transmission electron microscopy (TEM). The in-suit growth process of the primary M7C3 carbide was observed by confocal laser microscope (CLM). It is found that the primary M7C3 carbide in hypereutectic Fe-Cr-C alloy is irregular polygonal shape with several hollows in the center and gaps on the edge. Some primary M7C3 carbides are formed by layers of shell or/and consist of multiple parts. In the initial growth period, the primary M7C3 carbide forms protrusion parallel to {} crystal planes. The extending and revolving protrusion forms the carbide shell. The electron backscattered diffraction (EBSD) maps show that the primary M7C3 carbide consists of multiple parts. The semi-molten M7C3 carbide contains unmelted shell and several small-scale carbides inside, which further proves that the primary M7C3 carbide is not an overall block. It is believed that the coalescence of the primary M7C3 carbides is ascribed to the growing condition of the protrusion and the gap filling process.

Interpreting U-Pb data from primary and secondary features in lunar zircon

NASA Astrophysics Data System (ADS)

Grange, M. L.; Pidgeon, R. T.; Nemchin, A. A.; Timms, N. E.; Meyer, C.

2013-01-01

In this paper, we describe primary and secondary microstructures and textural characteristics found in lunar zircon and discuss the relationships between these features and the zircon U-Pb isotopic systems and the significance of these features for understanding lunar processes. Lunar zircons can be classified according to: (i) textural relationships between zircon and surrounding minerals in the host breccias, (ii) the internal microstructures of the zircon grains as identified by optical microscopy, cathodoluminescence (CL) imaging and electron backscattered diffraction (EBSD) mapping and (iii) results of in situ ion microprobe analyses of the Th-U-Pb isotopic systems. Primary zircon can occur as part of a cogenetic mineral assemblage (lithic clast) or as an individual mineral clast and is unzoned, or has sector and/or oscillatory zoning. The age of primary zircon is obtained when multiple ion microprobe analyses across the polished surface of the grain give reproducible and essentially concordant data. A secondary set of microstructures, superimposed on primary zircon, include localised recrystallised domains, localised amorphous domains, crystal-plastic deformation, planar deformation features and fractures, and are associated with impact processes. The first two secondary microstructures often yield internally consistent and close to concordant U-Pb ages that we interpret as dating impact events. Others secondary microstructures such as planar deformation features, crystal-plastic deformation and micro-fractures can provide channels for Pb diffusion and result in partial resetting of the U-Pb isotopic systems.

Quantifying the effects of tempering on individual phase properties of DP980 steel with nanoindentation

DOE Office of Scientific and Technical Information (OSTI.GOV)

Cheng, G.; Zhang, F.; Ruimi, A.

2016-06-01

We conduct a series of thermal and mechanical testing on a commercial dual phase (DP) 980 steel in order to quantify the effects of tempering on its individual phase properties. Tempering treatment is conducted at 250 °C and 400 °C for 60 minutes each. Ferrite and martensite grains are distinguished using electron backscatter diffraction (EBSD) and scanning probe microscopy (SPM), and the martensite volume fractions (MVF) are determined based on the image quality (IQ) map. Multi-scale indentation tests combined with a newly developed inverse method are used to obtain the individual phase flow properties in each tempered DP980 sample. Themore » results show that, i) tempering significantly reduces martensite yield strength, while it only slightly reduces the ferrite yield strength; ii) tempering temperature has a more significant influence on the work hardening exponent of ferrite than that of martensite; iii) the elastic modulus of martensite is consistently higher than that of ferrite. As a validation, a simple rule of mixtures is used to verify the above-predicted individual phase flow stresses with the experimentally obtained overall true stress vs. true strain curves. The methodology and the corresponding results shown in this study can help guide the selection of tempering parameters in optimizing the mechanical properties of DP steels for their intended applications.« less

SILICON CARBIDE GRAIN BOUNDARY DISTRIBUTIONS, IRRADIATION CONDITIONS, AND SILVER RETENTION IN IRRADIATED AGR-1 TRISO FUEL PARTICLES

DOE Office of Scientific and Technical Information (OSTI.GOV)

Lillo, T. M.; Rooyen, I. J.; Aguiar, J. A.

Precession electron diffraction in the transmission electron microscope was used to map grain orientation and ultimately determine grain boundary misorientation angle distributions, relative fractions of grain boundary types (random high angle, low angle or coincident site lattice (CSL)-related boundaries) and the distributions of CSL-related grain boundaries in the SiC layer of irradiated TRISO-coated fuel particles. Two particles from the AGR-1 experiment exhibiting high Ag-110m retention (>80%) were compared to a particle exhibiting low Ag-110m retention (<19%). Irradiated particles with high Ag-110m retention exhibited a lower fraction of random, high angle grain boundaries compared to the low Ag-110m retention particle. Anmore » inverse relationship between the random, high angle grain boundary fraction and Ag-110m retention is found and is consistent with grain boundary percolation theory. Also, comparison of the grain boundary distributions with previously reported unirradiated grain boundary distributions, based on SEM-based EBSD for similarly fabricated particles, showed only small differences, i.e. a greater low angle grain boundary fraction in unirradiated SiC. It was, thus, concluded that SiC layers with grain boundary distributions susceptible to Ag-110m release were present prior to irradiation. Finally, irradiation parameters were found to have little effect on the association of fission product precipitates with specific grain boundary types.« less

Growth characteristics of primary M7C3 carbide in hypereutectic Fe-Cr-C alloy

PubMed Central

Liu, Sha; Zhou, Yefei; Xing, Xiaolei; Wang, Jibo; Ren, Xuejun; Yang, Qingxiang

2016-01-01

The microstructure of the hypereutectic Fe-Cr-C alloy is observed by optical microscopy (OM). The initial growth morphology, the crystallographic structure, the semi-molten morphology and the stacking faults of the primary M7C3 carbide are observed by scanning electron microscopy (SEM) and transmission electron microscopy (TEM). The in-suit growth process of the primary M7C3 carbide was observed by confocal laser microscope (CLM). It is found that the primary M7C3 carbide in hypereutectic Fe-Cr-C alloy is irregular polygonal shape with several hollows in the center and gaps on the edge. Some primary M7C3 carbides are formed by layers of shell or/and consist of multiple parts. In the initial growth period, the primary M7C3 carbide forms protrusion parallel to {} crystal planes. The extending and revolving protrusion forms the carbide shell. The electron backscattered diffraction (EBSD) maps show that the primary M7C3 carbide consists of multiple parts. The semi-molten M7C3 carbide contains unmelted shell and several small-scale carbides inside, which further proves that the primary M7C3 carbide is not an overall block. It is believed that the coalescence of the primary M7C3 carbides is ascribed to the growing condition of the protrusion and the gap filling process. PMID:27596718

Phase transitions and melting on the Hugoniot of Mg2SiO4 forsterite: new diffraction and temperature results

NASA Astrophysics Data System (ADS)

Asimow, P. D.; Akin, M. C.; Homel, M.; Crum, R. S.; Pagan, D.; Lind, J.; Bernier, J.; Mosenfelder, J. L.; Dillman, A. M.; Lavina, B.; Lee, S.; Fat'yanov, O. V.; Newman, M. G.

2017-06-01

The phase transitions of forsterite under shock were studied by x-ray diffraction and pyrometry. Samples of 2 mm thick, near-full density (>98% TMD) polycrystalline forsterite were characterized by EBSD and computed tomography and shock compressed to 50 and 75 GPa by two-stage gas gun at the Dynamic Compression Sector, Advanced Photon Source, with diffraction imaged during compression and release. Changes in diffraction confirm a phase transition by 75 GPa. In parallel, single-crystal forsterite shock temperatures were taken from 120 to 210 GPa with improved absolute calibration procedures on the Caltech 6-channel pyrometer and two-stage gun and used to examine the interpretation of superheating and P-T slope of the liquid Hugoniot. This work performed under the auspices of the U.S. Department of Energy (DOE) by Lawrence Livermore National Laboratory under Contract DE-AC52-07NA27344, supported in part by LLNL's LDRD program under Grants 15-ERD-012 and 16-ERD-010. The Dynamic Compression Sector (35) is supported by DOE / National Nuclear Security Administration under Award Number DE-NA0002442. This research used resources of the Advanced Photon Source, a U.S. DOE Office of Science User Facility operated for the DOE Office of Science by Argonne National Laboratory under Contract No. DE-AC02-06CH11357. Caltech lab supported by NSF EAR-1426526.

Transmission Electron Microscopy of Magnetite Plaquettes in Orgueil

NASA Technical Reports Server (NTRS)

Chan, Q. H. S.; Han, J.; Zolensky, M.

2016-01-01

Magnetite sometimes takes the form of a plaquette - barrel-shaped stack of magnetite disks - in carbonaceous chondrites (CC) that show evidence of aqueous alteration. The asymmetric nature of the plaquettes caused Pizzarello and Groy to propose magnetite plaquettes as a naturally asymmetric mineral that can indroduce symmetry-breaking in organic molecules. Our previous synchrotron X-ray computed microtomography (SXRCT) and electron backscatter diffraction (EBSD) analyses of the magnetite plaquettes in fifteen CCs indicate that magnetite plaquettes are composed of nearly parallel discs, and the crystallographic orientations of the discs change around a rotational axis normal to the discs surfaces. In order to further investigate the nanostructures of magnetite plaquettes, we made two focused ion beam (FIB) sections of nine magnetite plaquettes from a thin section of CI Orgueil for transmission electron microscope (TEM) analysis. The X-ray spectrum imaging shows that the magnetite discs are purely iron oxide Fe3O4 (42.9 at% Fe and 57.1 at% O), which suggest that the plaquettes are of aqueous origin as it is difficult to form pure magnetite as a nebular condensate. The selected area electron diffraction (SAED) patterns acquired across the plaquettes show that the magnetite discs are single crystals. SEM and EBSD analyses suggest that the planar surfaces of the magnetite discs belong to the {100} planes of the cubic inverse spinel structure, which are supported by our TEM observations. Kerridge et al. suggested that the epitaxial relationship between magnetite plaquette and carbonate determines the magnetite face. However, according to our TEM observation, the association of magnetite with porous networks of phyllosilicate indicates that the epitaxial relationship with carbonate is not essential to the formation of magnetite plaquettes. It was difficult to determine the preferred rotational orientation of the plaquettes due to the symmetry of the cubic structure, however, we are able to observe small but consistent rotational orientation across several discs within a plaquette.

Determination of grain boundary mobility during recrystallization by statistical evaluation of electron backscatter diffraction measurements

DOE Office of Scientific and Technical Information (OSTI.GOV)

Basu, I., E-mail: basu@imm.rwth-aachen.de; Chen, M.; Loeck, M.

One of the key aspects influencing microstructural design pathways in metallic systems is grain boundary motion. The present work introduces a method by means of which direct measurement of grain boundary mobility vs. misorientation dependence is made possible. The technique utilizes datasets acquired by means of serial electron backscatter diffraction (EBSD) measurements. The experimental EBSD measurements are collectively analyzed, whereby datasets were used to obtain grain boundary mobility and grain aspect ratio with respect to grain boundary misorientation. The proposed method is further validated using cellular automata (CA) simulations. Single crystal aluminium was cold rolled and scratched in order tomore » nucleate random orientations. Subsequent annealing at 300 °C resulted in grains growing, in the direction normal to the scratch, into a single deformed orientation. Growth selection was observed, wherein the boundaries with misorientations close to Σ7 CSL orientation relationship (38° 〈111〉) migrated considerably faster. The obtained boundary mobility distribution exhibited a non-monotonic behavior with a maximum corresponding to misorientation of 38° ± 2° about 〈111〉 axes ± 4°, which was 10–100 times higher than the mobility values of random high angle boundaries. Correlation with the grain aspect ratio values indicated a strong growth anisotropy displayed by the fast growing grains. The observations have been discussed in terms of the influence of grain boundary character on grain boundary motion during recrystallization. - Highlights: • Statistical microstructure method to measure grain boundary mobility during recrystallization • Method implementation independent of material or crystal structure • Mobility of the Σ7 boundaries in 5N Al was calculated as 4.7 × 10{sup –8} m{sup 4}/J ⋅ s. • Pronounced growth selection in the recrystallizing nuclei in Al • Boundary mobility values during recrystallization 2–3 orders of magnitude larger vis-à-vis curvature driven motion.« less

Microstructure and hot corrosion behavior of the Ni-based superalloy GH202 treated by laser shock processing

DOE Office of Scientific and Technical Information (OSTI.GOV)

Cao, Jiangdong

The effects of laser shock processing on microstructure, the residual stress, and hot corrosion behavior of the Ni-based superalloy GH202 were investigated. The microstructures of GH202 before and after laser shock processing (LSP) were characterized by electron backscattered diffraction (EBSD) and transmission electron microscope (TEM). A large number of crystal defects (twins, dislocation arrays, and high dense tangles) were generated on the surface of GH202 treated with LSP. The cross-sectional compressive residual stress and micro-hardness of specimens treated by LSP were improved significantly. The corrosion kinetics of GH202 with or without LSP treatment at 800 °C and 900 °C weremore » investigated. Analysis by X-ray diffraction (XRD) revealed that the corrosion products mainly consist of Cr{sub 2}O{sub 3}, TiO{sub 2}, Al{sub 2}O{sub 3}, NiO, CrS, Ni{sub 3}S{sub 2}, and Na{sub 2}CrO{sub 4}. The surface and cross-section morphologies were observed by scanning electron microscope (SEM) combined with energy dispersive spectroscopy (EDS). The results confirmed that the crystal defects induced by LSP promotes the creation of diffusion paths for elements (Cr, Al, and Ti), allowing the formation of tiny homogeneous oxidation films in a very short time. Additionally, the spallation of oxidation film on the treated specimens was alleviated significantly. Overall, the hot corrosion resistance of Ni-based GH202 induced by LSP was improved in Na{sub 2}SO{sub 4} and NaCl molten salt from 800 °C to 900 °C. - Highlights: • Microstructure changes of GH202 before and after LSP were observed by EBSD and TEM. • The hardness and residual compressive stress after LSP were significantly increased. • The increased diffusion paths for elements helped to form oxidation films quickly. • Hot corrosion resistance of GH202 after LSP was significantly improved.« less

Dislocation Content Measured Via 3D HR-EBSD Near a Grain Boundary in an AlCu Oligocrystal

NASA Technical Reports Server (NTRS)

Ruggles, Timothy; Hochhalter, Jacob; Homer, Eric

2016-01-01

Interactions between dislocations and grain boundaries are poorly understood and crucial to mesoscale plasticity modeling. Much of our understanding of dislocation-grain boundary interaction comes from atomistic simulations and TEM studies, both of which are extremely limited in scale. High angular resolution EBSD-based continuum dislocation microscopy provides a way of measuring dislocation activity at length scales and accuracies relevant to crystal plasticity, but it is limited as a two-dimensional technique, meaning the character of the grain boundary and the complete dislocation activity is difficult to recover. However, the commercialization of plasma FIB dual-beam microscopes have made 3D EBSD studies all the more feasible. The objective of this work is to apply high angular resolution cross correlation EBSD to a 3D EBSD data set collected by serial sectioning in a FIB to characterize dislocation interaction with a grain boundary. Three dimensional high angular resolution cross correlation EBSD analysis was applied to an AlCu oligocrystal to measure dislocation densities around a grain boundary. Distortion derivatives associated with the plasma FIB serial sectioning were higher than expected, possibly due to geometric uncertainty between layers. Future work will focus on mitigating the geometric uncertainty and examining more regions of interest along the grain boundary to glean information on dislocation-grain boundary interaction.

Pyrite deformation and connections to gold mobility: Insight from micro-structural analysis and trace element mapping

NASA Astrophysics Data System (ADS)

Dubosq, R.; Lawley, C. J. M.; Rogowitz, A.; Schneider, D. A.; Jackson, S.

2018-06-01

The metamorphic transition of pyrite to pyrrhotite results in the liberation of lattice-bound and nano-particulate metals initially hosted within early sulphide minerals. This process forms the basis for the metamorphic-driven Au-upgrading model applied to many orogenic Au deposits, however the role of syn-metamorphic pyrite deformation in controlling the retention and release of Au and related pathfinder elements is poorly understood. The lower amphibolite facies metamorphic mineral assemblage (Act-Bt-Pl-Ep-Alm ± Cal ± Qz ± Ilm; 550 °C) of Canada's giant Detour Lake deposit falls within the range of pressure-temperature conditions (450 °C) for crystal plastic deformation of pyrite. We have applied a complementary approach of electron backscatter diffraction (EBSD) mapping and laser ablation inductively coupled plasma mass spectrometry (LA-ICP-MS) 2D element mapping on pyrite from the Detour Lake deposit. Chemical element maps document an early generation of Au-rich sieve textured pyrite domains and a later stage of syn-metamorphic oscillatory-zoned Au-poor pyrite. Both pyrite types are cut by Au-rich fractures as a consequence of remobilization of Au with trace element enrichment of first-row transition elements, post-transition metals, chalcogens and metalloids during a late brittle deformation stage. However, similar enrichment in trace elements and Au can be observed along low-angle grain boundaries within otherwise Au-poor pyrite, indicating that heterogeneous microstructural misorientation patterns and higher strain domains are also relatively Au-rich. We therefore propose that the close spatial relationship between pyrite and Au at the microscale, features typical of orogenic Au deposits, reflects the entrapment of Au within deformation-induced microstructures in pyrite rather than the release of Au during the metamorphic transition from pyrite to pyrrhotite. Moreover, mass balance calculations at the deposit scale suggest that only a small percentage of Au could have been sourced from pyrite and instead point to the role of substructures in pyrite as depositional traps for Au during syn-metamorphic deformation- and fluid-assisted diffusion Au-upgrading.

DOE Office of Scientific and Technical Information (OSTI.GOV)

Guo, Rui; Gao, Liming, E-mail: liming.gao@sjtu.edu.cn; Li, Ming, E-mail: mingli90@sjtu.edu.cn

As the continuous shrinkage of the interconnect line width in microelectronics devices, there is a growing concern about the electromigration (EM) failure of bonding wire. In addition, an innovative Ag–8Au–3Pd alloy wire has shown promise as an economical substitute for gold wire interconnects due to the cost pressure of gold in the last decade. In present study of the Ag–8Au–3Pd alloy wire, the surface diffusion occupied the dominant position during EM failure, and the activation energy was found to be 0.61 eV. In order to reveal the failure mechanism, the cross-sections of the Ag–8Au–3Pd alloy wire during EM were preparedmore » by focused ion beam (FIB) micro-machining for electron backscatter diffraction (EBSD) analysis. The microstructure evolution of the Ag–8Au–3Pd alloy wire was characterized by the grain size and grain boundary. As a result, the EM failure originates in the atom transportation, which causes grain size increasing and atom diffusion on the wire surface. - Highlights: • The activation energy of Ag–8Au–3Pd alloy wire was obtained as 0.61 eV. • During EM, the silver atoms diffused from negative to the positive terminal on the wire surface. • The microstructure (grain size and grain boundary) was characterized by FIB-EBSD. • During EM, the atom transportation was found to cause grain size growth and atom diffusion on the wire surface.« less

Crystallization of Electrodeposited Germanium Thin Film on Silicon (100).

PubMed

Abidin, Mastura Shafinaz Zainal; Matsumura, Ryo; Anisuzzaman, Mohammad; Park, Jong-Hyeok; Muta, Shunpei; Mahmood, Mohamad Rusop; Sadoh, Taizoh; Hashim, Abdul Manaf

2013-11-06

We report the crystallization of electrodeposited germanium (Ge) thin films on n-silicon (Si) (100) by rapid melting process. The electrodeposition was carried out in germanium (IV) chloride: propylene glycol (GeCl₄:C₃H₈O₂) electrolyte with constant current of 50 mA for 30 min. The measured Raman spectra and electron backscattering diffraction (EBSD) images show that the as-deposited Ge thin film was amorphous. The crystallization of deposited Ge was achieved by rapid thermal annealing (RTA) at 980 °C for 1 s. The EBSD images confirm that the orientations of the annealed Ge are similar to that of the Si substrate. The highly intense peak of Raman spectra at 300 cm -1 corresponding to Ge-Ge vibration mode was observed, indicating good crystal quality of Ge. An additional sub peak near to 390 cm -1 corresponding to the Si-Ge vibration mode was also observed, indicating the Ge-Si mixing at Ge/Si interface. Auger electron spectroscopy (AES) reveals that the intermixing depth was around 60 nm. The calculated Si fraction from Raman spectra was found to be in good agreement with the value estimated from Ge-Si equilibrium phase diagram. The proposed technique is expected to be an effective way to crystallize Ge films for various device applications as well as to create strain at the Ge-Si interface for enhancement of mobility.

Seismic properties and mineral crystallographic preferred orientations from EBSD data: Results from a crustal-scale detachment system, Aegean region

NASA Astrophysics Data System (ADS)

Cossette, Élise; Schneider, David; Audet, Pascal; Grasemann, Bernhard; Habler, Gerlinde

2015-05-01

The crystallographic preferred orientations (CPOs) were measured on a suite of samples representative of different structural depths along the West Cycladic Detachment System, Greece. Electron backscatter diffraction (EBSD) analyses were conducted on calcitic and mica schists, impure quartzites, and a blueschist, and the average seismic properties of the rocks were calculated with the Voigt-Reuss-Hill average of the single minerals' elastic stiffness tensor. The calcitic and quartzitic rocks have P- and S-wave velocity anisotropies (AVp, AVs) averaging 8.1% and 7.1%, respectively. The anisotropy increases with depth represented by the blueschist, with AVp averaging 20.3% and AVs averaging 14.5%, due to the content of aligned glaucophane and mica, which strongly control the seismic properties of the rocks. Localised anisotropies of very high magnitudes are caused by the presence of mica schists as they possess the strongest anisotropies, with values of ~ 25% for AVp and AVs. The direction of the fast and slow P-wave velocities occurs parallel and perpendicular to the foliation, respectively, for most samples. The fast propagation has the same NE-SW orientation as the lithospheric stretching direction experienced in the Cyclades since the Late Oligocene. The maximum shear wave anisotropy is subhorizontal, similarly concordant with mineral alignment that developed during extension in the Aegean. Radial anisotropy in the Aegean mid-crust is strongly favoured to azimuthal anisotropy by our results.

High stresses stored in fault zones: example of the Nojima fault (Japan)

NASA Astrophysics Data System (ADS)

Boullier, Anne-Marie; Robach, Odile; Ildefonse, Benoît; Barou, Fabrice; Mainprice, David; Ohtani, Tomoyuki; Fujimoto, Koichiro

2018-04-01

During the last decade pulverized rocks have been described on outcrops along large active faults and attributed to damage related to a propagating seismic rupture front. Questions remain concerning the maximal lateral distance from the fault plane and maximal depth for dynamic damage to be imprinted in rocks. In order to document these questions, a representative core sample of granodiorite located 51.3 m from the Nojima fault (Japan) that was drilled after the Hyogo-ken Nanbu (Kobe) earthquake is studied by using electron backscattered diffraction (EBSD) and high-resolution X-ray Laue microdiffraction. Although located outside of the Nojima damage fault zone and macroscopically undeformed, the sample shows pervasive microfractures and local fragmentation. These features are attributed to the first stage of seismic activity along the Nojima fault characterized by laumontite as the main sealing mineral. EBSD mapping was used in order to characterize the crystallographic orientation and deformation microstructures in the sample, and X-ray microdiffraction was used to measure elastic strain and residual stresses on each point of the mapped quartz grain. Both methods give consistent results on the crystallographic orientation and show small and short wavelength misorientations associated with laumontite-sealed microfractures and alignments of tiny fluid inclusions. Deformation microstructures in quartz are symptomatic of the semi-brittle faulting regime, in which low-temperature brittle plastic deformation and stress-driven dissolution-deposition processes occur conjointly. This deformation occurred at a 3.7-11.1 km depth interval as indicated by the laumontite stability domain. Residual stresses are calculated from deviatoric elastic strain tensor measured using X-ray Laue microdiffraction using the Hooke's law. The modal value of the von Mises stress distribution is at 100 MPa and the mean at 141 MPa. Such stress values are comparable to the peak strength of a deformed granodiorite from the damage zone of the Nojima fault. This indicates that, although apparently and macroscopically undeformed, the sample is actually damaged. The homogeneously distributed microfracturing of quartz is the microscopically visible imprint of this damage and suggests that high stresses were stored in the whole sample and not only concentrated on some crystal defects. It is proposed that the high residual stresses are the sum of the stress fields associated with individual dislocations and dislocation microstructures. These stresses are interpreted to be originated from the dynamic damage related to the propagation of rupture fronts or seismic waves at a depth where confining pressure prevented pulverization. Actually, M6 to M7 earthquakes occurred during the Paleocene on the Nojima fault and are good candidates for inducing this dynamic damage. The high residual stresses and the deformation microstructures would have contributed to the widening of the damaged fault zone with additional large earthquakes occurring on the Nojima fault.

Nanometres-resolution Kikuchi patterns from materials science specimens with transmission electron forward scatter diffraction in the scanning electron microscope.

PubMed

Brodusch, N; Demers, H; Gauvin, R

2013-04-01

A charge-coupled device camera of an electron backscattered diffraction system in a scanning electron microscope was positioned below a thin specimen and transmission Kikuchi patterns were collected. Contrary to electron backscattered diffraction, transmission electron forward scatter diffraction provides phase identification and orientation mapping at the nanoscale. The minimum Pd particle size for which a Kikuchi diffraction pattern was detected and indexed reliably was 5.6 nm. An orientation mapping resolution of 5 nm was measured at 30 kV. The resolution obtained with transmission electron forward scatter diffraction was of the same order of magnitude than that reported in electron nanodiffraction in the transmission electron microscope. An energy dispersive spectrometer X-ray map and a transmission electron forward scatter diffraction orientation map were acquired simultaneously. The high-resolution chemical, phase and orientation maps provided at once information on the chemical form, orientation and coherency of precipitates in an aluminium-lithium 2099 alloy. © 2013 The Authors Journal of Microscopy © 2013 Royal Microscopical Society.

Microstructure of Transparent Strontium Fresnoite Glass-Ceramics

PubMed Central

Wisniewski, Wolfgang; Takano, Kazuya; Takahashi, Yoshihiro; Fujiwara, Takumi; Rüssel, Christian

2015-01-01

Glass-ceramics grown from a glass of the composition Sr2TiSi2.45O8.9 (STS 45) are analyzed by scanning electron microscopy (SEM) and electron backscatter diffraction (EBSD). Oriented nucleation with the c-axes preferably perpendicular to the surface is detected. A very strong 001-texture is observed after only 10 μm of growth into the bulk, making this the first system in which an orientation preferred during nucleation prevails during growth into the bulk in glass-ceramics. Piezoelectric measurements are performed and d33-values presented and discussed. The obtained results are critically viewed with respect to the two growth models describing Sr2TiSi2O8 growth in glasses. PMID:25780988

Crystallography and Morphology of MC Carbides in Niobium-Titanium Modified As-Cast HP Alloys

NASA Astrophysics Data System (ADS)

Buchanan, Karl G.; Kral, Milo V.; Bishop, Catherine M.

2014-07-01

The microstructures of two as-cast heats of HP alloy stainless steels modified with niobium and titanium were examined with particular attention paid to the interdendritic niobium-titanium-rich carbides formed during solidification of these alloys. Generally, these precipitates obtain a blocky morphology in the as-cast condition. However, the (NbTi)C precipitates may obtain a nodular morphology. To provide further insight to the origin of the two different morphologies obtained by the (NbTi)C precipitates in the HP-NbTi alloy, the microstructure and crystallography of each have been studied in detail using scanning electron microscopy, transmission electron microscopy, various electron diffraction methods (EBSD, SAD, and CBED), and energy-dispersive X-ray spectroscopy.

Study of Deformation Phenomena in TRIP/TWIP Steels by Acoustic Emission and Scanning Electron Microscopy

NASA Astrophysics Data System (ADS)

Linderov, M. L.; Segel, C.; Weidner, A.; Biermann, H.; Vinogradov, A. Yu.

2018-04-01

Modern metastable steels with TRIP/TWIP effects have a unique set of physical-mechanical properties. They combine both high-strength and high-plasticity characteristics, which is governed by processes activated during deformation, namely, twinning, the formation of stacking faults, and martensitic transformations. To study the behavior of these phenomena in CrMnNi TRIP/TWIP steels and stainless CrNiMo steel, which does not have these effects in the temperature range under study, we used the method of acoustic emission and modern methods of signal processing, including the cluster analysis of spectral-density functions. The results of this study have been compared with a detailed microstructural analysis performed with a scanning electron microscope using electron backscatter diffraction (EBSD).

A phase quantification method based on EBSD data for a continuously cooled microalloyed steel

DOE Office of Scientific and Technical Information (OSTI.GOV)

Zhao, H.; Wynne, B.P.; Palmiere, E.J., E-mail: e.j

2017-01-15

Mechanical properties of steels depend on the phase constitutions of the final microstructures which can be related to the processing parameters. Therefore, accurate quantification of different phases is necessary to investigate the relationships between processing parameters, final microstructures and mechanical properties. Point counting on micrographs observed by optical or scanning electron microscopy is widely used as a phase quantification method, and different phases are discriminated according to their morphological characteristics. However, it is difficult to differentiate some of the phase constituents with similar morphology. Differently, for EBSD based phase quantification methods, besides morphological characteristics, other parameters derived from the orientationmore » information can also be used for discrimination. In this research, a phase quantification method based on EBSD data in the unit of grains was proposed to identify and quantify the complex phase constitutions of a microalloyed steel subjected to accelerated coolings. Characteristics of polygonal ferrite/quasi-polygonal ferrite, acicular ferrite and bainitic ferrite on grain averaged misorientation angles, aspect ratios, high angle grain boundary fractions and grain sizes were analysed and used to develop the identification criteria for each phase. Comparing the results obtained by this EBSD based method and point counting, it was found that this EBSD based method can provide accurate and reliable phase quantification results for microstructures with relatively slow cooling rates. - Highlights: •A phase quantification method based on EBSD data in the unit of grains was proposed. •The critical grain area above which GAM angles are valid parameters was obtained. •Grain size and grain boundary misorientation were used to identify acicular ferrite. •High cooling rates deteriorate the accuracy of this EBSD based method.« less

Deformation-related microstructures in magmatic zircon and implications for diffusion

NASA Astrophysics Data System (ADS)

Reddy, Steven Michael; Timms, Nicholas E.; Hamilton, Patrick Joseph; Smyth, Helen R.

2009-02-01

An undeformed glomeroporphyritic andesite from the Sunda Arc of Java, Indonesia, contains zoned plagioclase and amphibole glomerocrysts in a fine-grained groundmass and records a complex history of adcumulate formation and subsequent magmatic disaggregation. A suite of xenocrystic zircon records Proterozoic and Archaean dates whilst a discrete population of zoned, euhedral, igneous zircon yields a SHRIMP U-Pb crystallisation age of 9.3 ± 0.2 Ma. Quantitative microstructural analysis of zircon by electron backscatter diffraction (EBSD) shows no deformation in the inherited xenocrysts, but intragrain orientation variations of up to 30° in 80% of the young zircon population. These variations are typically accommodated by both progressive crystallographic bending and discrete low angle boundaries that overprint compositional growth zoning. Dispersion of crystallographic orientations are dominantly by rotation about an axis parallel to the zircon c-axis [001], which is coincident with the dominant orientation of misorientation axes of adjacent analysis points in EBSD maps. Less common <100> misorientation axes account for minor components of crystallographic dispersion. These observations are consistent with zircon deformation by dislocation creep and the formation of tilt and twist boundaries associated with the operation of <001>{100} and <100>{010} slip systems. The restriction of deformation microstructures to large glomerocrysts and the young magmatic zircon population, and the absence of deformation within the host igneous rock and inherited zircon grains, indicate that zircon deformation took place within a low-melt fraction (<5% melt), mid-lower crustal cumulate prior to fragmentation during magmatic disaggregation and entrainment of xenocrystic zircons during magmatic decompression. Tectonic stresses within the compressional Sunda Arc at the time of magmatism are considered to be the probable driver for low-strain deformation of the cumulate in the late stages of initial crystallisation. These results provide the first evidence of crystal plastic dislocation creep in zircon associated with magmatic crystallisation and indicate that the development of crystal-plastic microstructures in zircon is not restricted to high-strain rocks. Such microstructures have previously been shown to enhance bulk diffusion of trace elements (U, Th and REE) in zircon. The development of deformation microstructures, and therefore multiple diffusion pathways in zircon in the magmatic environment, has significant implications for the interpretation of geochemical data from igneous zircon and the trace element budgets of melts due to the potential enhancement of bulk diffusion and dissolution rates.

Stress evolution and associated microstructure during transient creep of olivine at 1000-1200 °C

NASA Astrophysics Data System (ADS)

Thieme, M.; Demouchy, S.; Mainprice, D.; Barou, F.; Cordier, P.

2018-05-01

We study the mechanical response and correlated microstructure of axial deformed fine-grained olivine aggregates as a function of incremental finite strains. Deformation experiments were conducted in uniaxial compression in an internally heated gas-medium deformation apparatus at temperatures of 1000 and 1200 °C, at strain rates of 10-6 s-1 to 10-5 s-1 and at confining pressure of 300 MPa. Sample volumes are around 1.2 cm3. Finite strains range from 0.1 to 8.6% and corresponding maximal (final) differential stresses range from 80 to 1073 MPa for deformation at 1000 °C and from 71 to 322 MPa for deformation at 1200 °C. At 1200 °C, samples approach steady state deformation after about 8% of strain. At 1000 °C, significant strain hardening leads to stresses exceeding the confining pressure by a factor of 3.5 with brittle deformation after 3% of strain. Deformed samples were characterized by electron backscatter diffraction (EBSD) and transmission electron microscopy (TEM). EBSD maps with step sizes as low as 50 nm were acquired without introducing analytical artifacts for the first time. The grain size of deformed samples ranges from 2.1 to 2.6 μm. Despite clear strain hardening, texture or microstructure do not change as a function of stress or finite strain. This observation is supported by a constant texture strength (J-index) and symmetry (BA-index), constant grain shape and aspect ratio, constant density of geometrically necessary dislocations, grain orientation spread, and constant subgrain boundary spacing and misorientation in between samples. TEM shows that all samples exhibit unambiguous dislocation activity but with a highly heterogeneous dislocation distribution. Olivine grains display evidence of [1 0 0] and [0 0 1] slip activity, but there is no evidence of interaction between the dislocations from the different slip systems. Several observations of grain boundaries acting as dislocation sources have been found. We find no confirmation of increasing dislocation densities as the cause for strain hardening during transient creep. This suggests other, yet not fully understood mechanisms affecting the strength of deformed olivine. These mechanisms could possibly involve grain boundaries. Such mechanisms are relevant for the deformation of uppermost mantle rocks, where the Si diffusion rate is too slow and dislocation glide must be accommodated in another way to fulfill the von Mises criterion.

Classification and assessment of retrieved electron density maps in coherent X-ray diffraction imaging using multivariate analysis.

PubMed

Sekiguchi, Yuki; Oroguchi, Tomotaka; Nakasako, Masayoshi

2016-01-01

Coherent X-ray diffraction imaging (CXDI) is one of the techniques used to visualize structures of non-crystalline particles of micrometer to submicrometer size from materials and biological science. In the structural analysis of CXDI, the electron density map of a sample particle can theoretically be reconstructed from a diffraction pattern by using phase-retrieval (PR) algorithms. However, in practice, the reconstruction is difficult because diffraction patterns are affected by Poisson noise and miss data in small-angle regions due to the beam stop and the saturation of detector pixels. In contrast to X-ray protein crystallography, in which the phases of diffracted waves are experimentally estimated, phase retrieval in CXDI relies entirely on the computational procedure driven by the PR algorithms. Thus, objective criteria and methods to assess the accuracy of retrieved electron density maps are necessary in addition to conventional parameters monitoring the convergence of PR calculations. Here, a data analysis scheme, named ASURA, is proposed which selects the most probable electron density maps from a set of maps retrieved from 1000 different random seeds for a diffraction pattern. Each electron density map composed of J pixels is expressed as a point in a J-dimensional space. Principal component analysis is applied to describe characteristics in the distribution of the maps in the J-dimensional space. When the distribution is characterized by a small number of principal components, the distribution is classified using the k-means clustering method. The classified maps are evaluated by several parameters to assess the quality of the maps. Using the proposed scheme, structure analysis of a diffraction pattern from a non-crystalline particle is conducted in two stages: estimation of the overall shape and determination of the fine structure inside the support shape. In each stage, the most accurate and probable density maps are objectively selected. The validity of the proposed scheme is examined by application to diffraction data that were obtained from an aggregate of metal particles and a biological specimen at the XFEL facility SACLA using custom-made diffraction apparatus.

Twinning and martensite in a 304 austenitic stainless steel

DOE Office of Scientific and Technical Information (OSTI.GOV)

Shen, Yongfeng; Li, Xi; Sun, Xin

2012-08-30

The microstructure characteristics and deformation behavior of 304L stainless steel during tensile deformation at two different strain rates have been investigated by means of interrupted tensile tests, electron-backscatter-diffraction (EBSD) and transmission electron microscopy (TEM) techniques. The volume fractions of transformed martensite and deformation twins at different stages of the deformation process were measured using X-ray diffraction method and TEM observations. It is found that the volume fraction of martensite monotonically increases with increasing strain but decreases with increasing strain rate. On the other hand, the volume fraction of twins increases with increasing strain for strain level less than 57%. Beyondmore » that, the volume fraction of twins decreases with increasing strain. Careful TEM observations show that stacking faults (SFs) and twins preferentially occur before the nucleation of martensite. Meanwhile, both {var_epsilon}-martensite and {alpha}{prime}-martensite are observed in the deformation microstructures, indicating the co-existence of stress induced- transformation and strain-induced-transformation. We also discussed the effects of twinning and martensite transformation on work-hardening as well as the relationship between stacking faults, twinning and martensite transformation.« less

Direct growth of freestanding GaN on C-face SiC by HVPE.

PubMed

Tian, Yuan; Shao, Yongliang; Wu, Yongzhong; Hao, Xiaopeng; Zhang, Lei; Dai, Yuanbin; Huo, Qin

2015-06-02

In this work, high quality GaN crystal was successfully grown on C-face 6H-SiC by HVPE using a two steps growth process. Due to the small interaction stress between the GaN and the SiC substrate, the GaN was self-separated from the SiC substrate even with a small thickness of about 100 μm. Moreover, the SiC substrate was excellent without damage after the whole process so that it can be repeatedly used in the GaN growth. Hot phosphoric acid etching (at 240 °C for 30 min) was employed to identify the polarity of the GaN layer. According to the etching results, the obtained layer was Ga-polar GaN. High-resolution X-ray diffraction (HRXRD) and electron backscatter diffraction (EBSD) were done to characterize the quality of the freestanding GaN. The Raman measurements showed that the freestanding GaN film grown on the C-face 6H-SiC was stress-free. The optical properties of the freestanding GaN layer were determined by photoluminescence (PL) spectra.

Strain softening during tension in cold drawn Cu–Ag alloys

DOE Office of Scientific and Technical Information (OSTI.GOV)

Chang, L.L., E-mail: lilichang@sdu.edu.cn; Wen, S.; Li, S.L.

2015-10-15

Experiments were conducted on Cu–0.1wt.%Ag alloys to evaluate the influence of producing procedures and annealing conditions on microstructure evolution and mechanical properties of Cu–Ag alloys. Optical microscopy (OM), electron back-scattered diffraction (EBSD), X-ray diffraction (XRD) and transmission electron microscopy (TEM) were used for microstructural evaluation and mechanical properties were characterized by tensile tests. The results indicated that hot-extruded Cu–Ag alloys had a typical dynamic recrystallized microstructure with equiaxed grains. Cold drawing at room temperature leaded to partial recrystallized microstructure with a mixture of coarse and fine grains. The dominate {001}<100 > cubic texture formed during hot extrusion was changed tomore » be {112}<111 > copper texture by cold drawing. Strain softening occurred during room temperature tension of cold drawn Cu–Ag alloys with an average grain size of 13–19.7 μm. - Highlights: • Strain softening occurred during tension of Cu–Ag alloys with coarse grain size. • Work hardening was observed in hot-extruded and annealed Cu–0.1wt.%Ag alloys. • Strain softening was ascribed to dynamic recovery and dynamic recrystallization.« less

Estimation of dislocations density and distribution of dislocations during ECAP-Conform process

NASA Astrophysics Data System (ADS)

Derakhshan, Jaber Fakhimi; Parsa, Mohammad Habibi; Ayati, Vahid; Jafarian, Hamidreza

2018-01-01

Dislocation density of coarse grain aluminum AA1100 alloy (140 µm) that was severely deformed by Equal Channel Angular Pressing-Conform (ECAP-Conform) are studied at various stages of the process by electron backscattering diffraction (EBSD) method. The geometrically necessary dislocations (GNDs) density and statistically stored dislocations (SSDs) densities were estimate. Then the total dislocations densities are calculated and the dislocation distributions are presented as the contour maps. Estimated average dislocations density for annealed of about 2×1012 m-2 increases to 4×1013 m-2 at the middle of the groove (135° from the entrance), and they reach to 6.4×1013 m-2 at the end of groove just before ECAP region. Calculated average dislocations density for one pass severely deformed Al sample reached to 6.2×1014 m-2. At micrometer scale the behavior of metals especially mechanical properties largely depend on the dislocation density and dislocation distribution. So, yield stresses at different conditions were estimated based on the calculated dislocation densities. Then estimated yield stresses were compared with experimental results and good agreements were found. Although grain size of material did not clearly change, yield stress shown intensive increase due to the development of cell structure. A considerable increase in dislocations density in this process is a good justification for forming subgrains and cell structures during process which it can be reason of increasing in yield stress.

Scanning electron microscopy of the surfaces of ion implanted SiC

NASA Astrophysics Data System (ADS)

Malherbe, Johan B.; van der Berg, N. G.; Kuhudzai, R. J.; Hlatshwayo, T. T.; Thabethe, T. T.; Odutemowo, O. S.; Theron, C. C.; Friedland, E.; Botha, A. J.; Wendler, E.

2015-07-01

This paper gives a brief review of radiation damage caused by particle (ions and neutrons) bombardment in SiC at different temperatures, and its annealing, with an expanded discussion on the effects occurring on the surface. The surface effects were observed using SEM (scanning electron microscopy) with an in-lens detector and EBSD (electron backscatter diffraction). Two substrates were used, viz. single crystalline 6H-SiC wafers and polycrystalline SiC, where the majority of the crystallites were 3C-SiC. The surface modification of the SiC samples by 360 keV ion bombardment was studied at temperatures below (i.e. room temperature), just at (i.e. 350 °C), or above (i.e. 600 °C) the critical temperature for amorphization of SiC. For bombardment at a temperature at about the critical temperature an extra step, viz. post-bombardment annealing, was needed to ascertain the microstructure of bombarded layer. Another aspect investigated was the effect of annealing of samples with an ion bombardment-induced amorphous layer on a 6H-SiC substrate. SEM could detect that this layer started to crystalize at 900 °C. The resulting topography exhibited a dependence on the ion species. EBSD showed that the crystallites forming in the amorphized layer were 3C-SiC and not 6H-SiC as the substrate. The investigations also pointed out the behaviour of the epitaxial regrowth of the amorphous layer from the 6H-SiC interface.

Analysis of the ductility dip cracking in the nickel-base alloy 617mod

NASA Astrophysics Data System (ADS)

Eilers, A.; Nellesen, J.; Zielke, R.; Tillmann, W.

2017-03-01

While testing steam leading power plant components made of the nickel-base alloy A617mod at elevated temperatures (700 °C), ductility dip cracking (DDC) was observed in welding seams and their surroundings. In order to clarify the mechanism of crack formation, investigations were carried out on welded specimens made of A617mod. Interrupted tensile tests were performed on tensile specimens taken from the area of the welding seam. To simulate the conditions, the tensile tests were conducted at a temperature of 700 °C and with a low strain rate. Local strain fields at grain boundaries and inside single grains were determined at different deformation states by means of two-dimensional digital image correlation (DIC). Besides the strain fields, local hardnesses (nanoindentation), energy dispersive X-Ray spectroscopy (EDX), and electron backscatter diffraction (EBSD) measurements were performed. Besides information concerning the grain orientation, the EBSD measurement provides information on the coincidence site lattice (CSL) at grain boundaries as well as the Schmid factor of single grains. All results of the analysis methods mentioned above were correlated and compared to each other and related to the crack formation. Among other things, correlations between strain fields and Schmid factors were determined. The investigations show that the following influences affect the crack formation: orientation of the grain boundaries to the direction of the loading, the orientation of the grains to each other (CSL), and grain boundary sliding.

The correlation of local deformation and stress-assisted local phase transformations in MMC foams

DOE Office of Scientific and Technical Information (OSTI.GOV)

Berek, H., E-mail: harry.berek@ikgb.tu-freiberg.de; Ballaschk, U.; Aneziris, C.G.

2015-09-15

Cellular structures are of growing interest for industry, and are of particular importance for lightweight applications. In this paper, a special case of metal matrix composite foams (MMCs) is investigated. The investigated foams are composed of austenitic steel exhibiting transformation induced plasticity (TRIP) and magnesia partially stabilized zirconia (Mg-PSZ). Both components exhibit martensitic phase transformation during deformation, thus generating the potential for improved mechanical properties such as strength, ductility, and energy absorption capability. The aim of these investigations was to show that stress-assisted phase transformations within the ceramic reinforcement correspond to strong local deformation, and to determine whether they canmore » trigger martensitic phase transformations in the steel matrix. To this end, in situ interrupted compression experiments were performed in an X-ray computed tomography device (XCT). By using a recently developed registration algorithm, local deformation could be calculated and regions of interest could be defined. Corresponding cross sections were prepared and used to analyze the local phase composition by electron backscatter diffraction (EBSD). The results show a strong correlation between local deformation and phase transformation. - Graphical abstract: Display Omitted - Highlights: • In situ compressive deformation on MMC foams was performed in an XCT. • Local deformation fields and their gradient amplitudes were estimated. • Cross sections were manufactured containing defined regions of interest. • Local EBSD phase analysis was performed. • Local deformation and local phase transformation are correlated.« less

Web survey of sleep problems associated with early-onset bipolar spectrum disorders.

PubMed

Lofthouse, Nicholas; Fristad, Mary; Splaingard, Mark; Kelleher, Kelly; Hayes, John; Resko, Susan

2008-05-01

As research on sleep difficulties associated with Early-Onset Bipolar Spectrum Disorders (EBSD) is limited, a web-based survey was developed to further explore these problems. 494 parents of 4-to-12 year-olds, identified by parents as being diagnosed with EBSD, completed a web survey about past and current EBSD-related sleep problems. The survey included Children's Sleep Habits Questionnaire (CSHQ) items and sleep problems from the International Classification of Sleep Disorders 2nd edition. Nearly all parents reported some type of past or current EBSD-sleep problem. Most occurred during a worst mood period, particularly with mixed manic-depressive symptoms. Symptoms caused impairments at home, school, or with peers in 96.9% of the sample and across all three contexts in 64.0% of children. Sleep problems were also noted after three-day weekends and Spring and Fall Daylight Savings time changes. Findings, study limitations, and implications for treatment and etiology are discussed.

Heteogeneities During Deformation of Polycrystalline Ice, Recent Advances in Cryo-EBSD Analyses

NASA Astrophysics Data System (ADS)

Journaux, B.; Montagnat, M.; Chauve, T.; Barou, F.; Tommasi, A.; Mainprice, D.

2017-12-01

Microstructural heterogeneities come into play at various scales during deformation of polycrystalline materials. In particular, intra-granular heterogeneities such as subgrain boundaries, and dislocations sub-structures play a crucial role during dynamic recrystallization (DRX) mechanisms. The latter are active in ice, minerals and metals deformed at medium to high temperature, and enable a relaxation of strain energy. They regroup nucleation of new grains and grain boundary migration, which can drastically modify the microstructure and texture (crystallographic preferred orientations) during deformation in natural conditions or in the laboratory. Since ice has a strong viscoplastic anisotropy (with dislocations gliding mostly on the basal planes of its hexagonal crystalline structure), texture play a crucial role in the response of ice deformed naturally at low strain-rate. Texture evolution along natural ice cores has been studied for a long time but the bases DRX mechanisms were, up to recently, only offered a simplistic characterization due to the lack of resolution of the classical optical based technics. Since a few years, Electron BackScattering Diffraction (EBSD) imaging has been adapted for ice study. In particular, the EBSD of Geosciences Montpellier offers an unique opportunity to explore large samples of ice (2x3 cm2), at a relatively high resolution (20 to 5 μm), and a very good indexation (> 90%). We will present an overview of the type of informations made available by this technique, from a set of torsion and compression laboratory tests performed on ice polycrystals. The strong intra-granular heterogeneities measured were Geometrically Necessary Dislocations (GNDs), analyzed by the mean of the Weighted Burgers Vectors (Wheeler et al. 2009, J. of Microscopy 233).Our results clearly point out the complexity of the mechanisms (especially nucleation), and question up to the classical paradigm of the non-existence of non-basal dislocations with a c-axis component in ice. We therefore highlight the necessity to implement viscoplastic laws that correctly integrate a minimum of this complexity in full-field or mean-field modeling approaches that aim at simulating the mechanical response and texture evolution of ice.

Grain Boundary Sliding (GBS) as a Plastic Instability Leading to Coeval Pseudotachylyte Development in Mylonites: an EBSD Study of the Seismic Cycle in Brittle-Ductile Transition Rocks of the South Mountains Core Complex, Arizona, USA

NASA Astrophysics Data System (ADS)

Miranda, E.; Stewart, C.

2017-12-01

Exposures of coeval pseudotachylytes and mylonites are relatively rare, but are crucial for understanding the seismic cycle in the vicinity of the brittle-ductile transition (BDT). We use both field observations and electron backscatter diffraction (EBSD) analysis to investigate the coeval pseudotachylytes and granodiorite mylonites exposed in the footwall of the South Mountains core complex, Arizona, to evaluate how strain is localized both prior to and during pseudotachylyte development at the BDT. In the field, we observe numerous pseudotachylyte veins oriented parallel to mylonitic foliation; the veins have synthetic shear sense with adjacent mylonites, and are < 2 cm thick, laterally discontinuous, and confined to a few m in structural thickness. EBSD analysis reveals that deformation is strongly partitioned into quartz in mylonites, where quartz shows subgrain rotation overprinted by bulging recrystallization microstructures and lattice preferred orientation (LPO) patterns indicative of dislocation creep. Foliation-parallel zones of finely recrystallized, (< 5 μm diameter) bulge-nucleated grains in the mylonites show four-grain junctions and randomized LPO patterns consistent with grain boundary sliding (GBS). Pseudotachylyte veins have elongate polycrystalline quartz survivor clasts that also exhibit GBS traits, suggesting that pseudotachylytes form within GBS zones in mylonites. We interpret the onset of GBS as a triggering mechanism for coeval pseudotachylyte development, where the accompanying decrease in effective viscosity and increase in strain rate initiated seismic slip and pseudotachylyte formation within GBS zones. Strain became localized within the pseudotachylyte until crystallization of melt impeded flow, inducing pseudotachylyte development in other GBS zones. We associate the pseudotachylyte veins and host mylonites with the coseismic and interseismic parts of the seismic cycle, respectively, where the abundance and lateral discontinuity of pseudotachylyte veins suggests repeated events. We speculate that periodic, GBS-initiated pseudotachylyte generation may correlate with intermediate slip rate seismic events in the vicinity of the BDT, suggesting that coeval pseudotachylytes and mylonites are evidence of a unique class of seismic event.

Microstructure and Sn crystal orientation evolution in Sn-3.5Ag lead-free solders in high temperature packaging applications

DOE Office of Scientific and Technical Information (OSTI.GOV)

Zhou, Bite; Muralidharan, Govindarajan; Kurumaddali, Nalini Kanth

2014-01-01

Understanding the reliability of eutectic Sn-3.5Ag lead-free solders in high temperature packaging applications is of significant interest in power electronics for the next generation electric grid. Large area (2.5mm 2.5mm) Sn-3.5Ag solder joints between silicon dies and direct bonded copper substrates were thermally cycled between 5 C and 200 C. Sn crystal orientation and microstructure evolution during thermal cycling were characterized by electron backscatter diffraction (EBSD) in scanning electron microscope (SEM). Comparisons are made between observed initial texture and microstructure and its evolution during thermal cycling. Gradual lattice rotation and grain boundary misorientation evolution suggested the continuous recrystallization mechanism. Recrystallizationmore » behavior was correlated with dislocation slip activities.« less

Short communication on Kinetics of grain growth and particle pinning in U-10 wt.% Mo

NASA Astrophysics Data System (ADS)

Frazier, William E.; Hu, Shenyang; Overman, Nicole; Lavender, Curt; Joshi, Vineet V.

2018-01-01

The alloy U-10 wt% Mo was annealed at temperatures ranging from 700 °C to 900 °C for periods lasting up to 24 h. Annealed microstructures were examined using Electron Backscattered Diffraction (EBSD) to obtain average grain sizes and grain size distributions. From the temporal evolution of the average grain size, the activation energy of grain growth was determined to be 172.4 ± 0.961 kJ/mol. Grain growth over the annealing period stagnated after a period of 1-4 h. This stagnation is apparently caused by the pinning effect of second-phase particles in the materials. Back-scattered electron imaging (BSE) was used to confirm that these particles do not appreciably coarsen or dissolve during annealing at the aforementioned temperatures.

Microstructural analysis of the thermal annealing of ice-Ih using EBSD

NASA Astrophysics Data System (ADS)

Hidas, Károly; Tommasi, Andréa; Mainprice, David; Chauve, Thomas; Barou, Fabrice; Montagnat, Maurine

2017-04-01

Rocks deformed in the middle crust and deeper in the Earth typically remain at high temperature for extended time spans after the cessation of deformation. This results in annealing of the deformation microstructure by a series of thermally activated, diffusion-based processes, namely: recovery and static recrystallization, which may also modify the crystal preferred orientation (CPO) or texture. Understanding the effects of annealing on the microstructure and CPO is therefore of utmost importance for the interpretation of the microstructures and for the estimation of the anisotropy of physical properties of lower crustal and mantle rocks. Ice-Ih -the typical form of water ice on the Earth's surface, with hexagonal crystal symmetry- deforms essentially by glide of dislocations on the basal plane [1], thus it has high viscoplastic anisotropy, which induces strong heterogeneity of stresses and strains at both the intra- and intergranular scales [2-3]. This behavior makes ice-Ih an excellent analog material for silicate minerals that compose the Earth. In situ observations of the evolution of the microstructures and CPO during annealing enable the study of the interplay between the various physical processes involved in annealing (recovery, nucleation, grain growth). They also allow the analysis of the impact of the preexisting deformation microstructures on the microstructural and CPO evolution during annealing. Here we studied the evolution of the microstructure of ice-Ih during static recrystallization by stepwise annealing experiments. We alternated thermal annealing and electron backscatter diffraction (EBSD) analyses on polycrystalline columnar ice-Ih pre-deformed in uniaxial compression at temperature of -7 °C to strains of 3.0-5.2. Annealing experiments were carried out at -5 °C and -2 °C up to a maximum of 3.25 days, typically in 5-6 steps. EBSD crystal orientation maps obtained after each annealing step permit the description of microstructural changes. Decrease in average intragranular misorientation at the sample scale and modification of the misorientation across subgrain boundaries provide evidence for recovery from the earliest stages of annealing. This evolution is similar for all studied samples irrespective of their initial strain or annealing temperature. After an incubation period up to 2 hours, recovery is accompanied by recrystallization (nucleation and grain boundary migration). Grain growth proceeds at the expense of domains with high intra-granular misorientations and its kinetics fits the parabolic growth law. Deformation-induced microstructures (tilt boundaries and kink bands) are stable features during early stages of static recrystallization and locally slow down grain boundary migration, pinning grain growth. REFERENCES 1. Duval, P., Ashby, M.F., Anderman, I., 1983. Rate-controlling processes in the creep of polycrystalline ice. Journal of Physical Chemistry 87, 4066-4074. 2. Grennerat, F., Montagnat, M., Castelnau, O., Vacher, P., Moulinec, H., Suquet, P., Duval, P., 2012. Experimental characterization of the intragranular strain field in columnar ice during transient creep. Acta Materialia 60, 3655-3666. 3. Chauve, T., Montagnat, M., Vacher, P., 2015. Strain field evolution during dynamic recrystallization nucleation: A case study on ice. Acta Materialia 101, 116-124. Funding: Research leading to these results was funded by the EU-FP7 Marie Curie postdoctoral grant PIEF-GA-2012-327226 to K.H.

EBSD in Antarctic and Greenland Ice

NASA Astrophysics Data System (ADS)

Weikusat, Ilka; Kuiper, Ernst-Jan; Pennock, Gill; Sepp, Kipfstuhl; Drury, Martyn

2017-04-01

Ice, particularly the extensive amounts found in the polar ice sheets, impacts directly on the global climate by changing the albedo and indirectly by supplying an enormous water reservoir that affects sea level change. The discharge of material into the oceans is partly controlled by the melt excess over snow accumulation, partly by the dynamic flow of ice. In addition to sliding over bedrock, an ice body deforms gravitationally under its own weight. In order to improve our description of this flow, ice microstructure studies are needed that elucidate the dominant deformation and recrystallization mechanisms involved. Deformation of hexagonal ice is highly anisotropic: ice is easily sheared in the basal plane and is about two orders of magnitude harder parallel to the c-axis. As dislocation creep is the dominant deformation mechanism in polar ice this strong anisotropy needs to be understood in terms of dislocation activity. The high anisotropy of the ice crystal is usually ascribed to a particular behaviour of dislocations in ice, namely the extension of dislocations into partials on the basal plane. Analysis of EBSD data can help our understanding of dislocation activity by characterizing subgrain boundary types thus providing a tool for comprehensive dislocation characterization in polar ice. Cryo-EBSD microstructure in combination with light microscopy measurements from ice core material from Antarctica (EPICA-DML deep ice core) and Greenland (NEEM deep ice core) are presented and interpreted regarding substructure identification and characterization. We examined one depth for each ice core (EDML: 656 m, NEEM: 719 m) to obtain the first comparison of slip system activity from the two ice sheets. The subgrain boundary to grain boundary threshold misorientation was taken to be 3-5° (Weikusat et al. 2011). EBSD analyses suggest that a large portion of edge dislocations with slip systems basal gliding on the basal plane were indeed involved in forming subgrain boundaries. However, an almost equal number of tilt subgrain boundaries were measured, involving dislocations gliding on non-basal planes (prism or prism slip). A few subgrain boundaries involving prism edge dislocation glide, as well as boundaries involving basal twist dislocation slip, were also identified. The finding that subgrain boundaries built up by dislocations gliding on non-basal planes are as frequent as those originating from basal plane slip is surprising and has impact on the discussion on rate-controlling processes for the ice flow descriptions of large ice masses with respect to sea-level evolution. Weikusat, I.; Miyamoto, A.; Faria, S. H.; Kipfstuhl, S.; Azuma, N. & Hondoh, T.: Subgrain boundaries in Antarctic ice quantified by X-ray Laue diffraction J. Glaciol., 2011, 57, 85-94

Relationship between crystallographic structure of the Ti{sub 2}O{sub 3}/MnS complex inclusion and microstructure in the heat-affected zone (HAZ) in steel processed by oxide metallurgy route and impact toughness

DOE Office of Scientific and Technical Information (OSTI.GOV)

Xiong, Zhihui; Liu, Shilong; Wang, Xuemin, E-mail: wxm@mater.ustb.edu.cn

2015-08-15

A new method based on electron back scattered diffraction (EBSD) is proposed to determine the structure of titanium oxide/MnS complex inclusion which induced the formation of intragranular acicular ferrite (IAF) in heat-affected zone (HAZ) in steel processed by oxide metallurgy route. It was found that the complex inclusion was Ti{sub 2}O{sub 3}/MnS, the orientation relationship between Ti{sub 2}O{sub 3} and MnS was also examined, and the crystallographic orientation relationship among IAF, Ti{sub 2}O{sub 3}/MnS complex inclusion, austenite, bainite formed at lower temperature is researched systematically. It was observed that MnS precipitated on Ti{sub 2}O{sub 3} at specific habit plane andmore » direction and MnS had a specific orientation relationship ((0001) Ti{sub 2}O{sub 3}//(111) MnS), <10–10> Ti{sub 2}O{sub 3}//<110> MnS) with respect to Ti{sub 2}O{sub 3}. Intragranular acicular ferrite (IAF) nucleated on MnS part of the Ti{sub 2}O{sub 3}/MnS complex inclusion had no specific orientation relationship with MnS. IAF and the surrounding bainite had different Bain groups, so that there was an increase in high angle boundaries, which was beneficial for the toughness of HAZ. - Highlights: • The inclusion of TiO{sub x}/MnS that induced IAF formation is identified to be Ti{sub 2}O{sub 3}/MnS. • The inclusion is identified based on electron back scattered diffraction (EBSD). • MnS and Ti{sub 2}O{sub 3} had specific orientation relationship of Ti{sub 2}O{sub 3}/MnS complex inclusion. • The IAFs formed on the same inclusion tend to be in one Bain group. • IAF and the surrounding bainite tend to be in different Bain groups.« less

Experiments and simulation for 6061-T6 aluminum alloy resistance spot welded lap joints

NASA Astrophysics Data System (ADS)

Florea, Radu Stefanel

This comprehensive study is the first to quantify the fatigue performance, failure loads, and microstructure of resistance spot welding (RSW) in 6061-T6 aluminum (Al) alloy according to welding parameters and process sensitivity. The extensive experimental, theoretical and simulated analyses will provide a framework to optimize the welding of lightweight structures for more fuel-efficient automotive and military applications. The research was executed in four primary components. The first section involved using electron back scatter diffraction (EBSD) scanning, tensile testing, laser beam profilometry (LBP) measurements, and optical microscopy(OM) images to experimentally investigate failure loads and deformation of the Al-alloy resistance spot welded joints. Three welding conditions, as well as nugget and microstructure characteristics, were quantified according to predefined process parameters. Quasi-static tensile tests were used to characterize the failure loads in specimens based upon these same process parameters. Profilometer results showed that increasing the applied welding current deepened the weld imprints. The EBSD scans revealed the strong dependency between the grain sizes and orientation function on the process parameters. For the second section, the fatigue behavior of the RSW'ed joints was experimentally investigated. The process optimization included consideration of the forces, currents, and times for both the main weld and post-heating. Load control cyclic tests were conducted on single weld lap-shear joint coupons to characterize the fatigue behavior in spot welded specimens. Results demonstrate that welding parameters do indeed significantly affect the microstructure and fatigue performance for these welds. The third section comprised residual strains of resistance spot welded joints measured in three different directions, denoted as in-plane longitudinal, in-plane transversal, and normal, and captured on the fusion zone, heat affected zone and base metal of the joints. Neutron diffraction results showed residual stresses in the weld are approximately 40% lower than the yield strength of the parent material, with maximum variation occurring in the vertical position of the specimen because of the orientation of electrode clamping forces that produce a non-uniform solidification pattern. In the final section a theoretical continuum modeling framework for 6061-T6 aluminum resistance spot welded joints is presented.

Quantifying the Variation in Shear Zone Character with Depth: a Case Study from the Simplon Shear Zone, Central Alps

NASA Astrophysics Data System (ADS)

Cawood, T. K.; Platt, J. P.

2017-12-01

A widely-accepted model for the rheology of crustal-scale shear zones states that they comprise distributed strain at depth, in wide, high-temperature shear zones, which narrow to more localized, high-strain zones at lower temperature and shallower crustal levels. We test and quantify this model by investigating how the width, stress, temperature and deformation mechanisms change with depth in the Simplon Shear Zone (SSZ). The SSZ marks a major tectonic boundary in the central Alps, where normal-sense motion and rapid exhumation of the footwall have preserved evidence of older, deeper deformation in rocks progressively further into the currently-exposed footwall. As such, microstructures further from the brittle fault (which represents the most localized, most recently-active part of the SSZ) represent earlier, higher- temperature deformation from deeper crustal levels, while rocks closer to the fault have been overprinted by successively later, cooler deformation at shallower depths. This study uses field mapping and microstructural studies to identify zones representing deformation at various crustal levels, and characterize each in terms of zone width (representing width of the shear zone at that time and depth) and dominant deformation mechanism. In addition, quartz- (by Electron Backscatter Diffraction, EBSD) and feldspar grain size (measured optically) piezometry are used to calculate the flow stress for each zone, while the Ti-in-quartz thermometer (TitaniQ) is used to calculate the corresponding temperature of deformation. We document the presence of a broad zone in which quartz is recrystallized by the Grain Boundary Migration (GBM) mechanism and feldspar by Subgrain Rotation (SGR), which represents the broad, deep zone of deformation occurring at relatively high temperatures and low stresses. In map view, this transitions to successively narrower zones, respectively characterized by quartz SGR and feldspar Bulge Nucleation (BLG); quartz BLG and brittle deformation of feldspar; and finally, a zone of generally brittle deformation. These zones represent deformation in progressively narrower regions at shallower depths, under lower temperatures and higher stresses.

Non-basal dislocations should be accounted for in simulating ice mass flow

NASA Astrophysics Data System (ADS)

Chauve, T.; Montagnat, M.; Piazolo, S.; Journaux, B.; Wheeler, J.; Barou, F.; Mainprice, D.; Tommasi, A.

2017-09-01

Prediction of ice mass flow and associated dynamics is pivotal at a time of climate change. Ice flow is dominantly accommodated by the motion of crystal defects - the dislocations. In the specific case of ice, their observation is not always accessible by means of the classical tools such as X-ray diffraction or transmission electron microscopy (TEM). Part of the dislocation population, the geometrically necessary dislocations (GNDs) can nevertheless be constrained using crystal orientation measurements via electron backscattering diffraction (EBSD) associated with appropriate analyses based on the Nye (1950) approach. The present study uses the Weighted Burgers Vectors, a reduced formulation of the Nye theory that enables the characterization of GNDs. Applied to ice, this method documents, for the first time, the presence of dislocations with non-basal [ c ] or < c + a > Burgers vectors. These [ c ] or < c + a > dislocations represent up to 35% of the GNDs observed in laboratory-deformed ice samples. Our findings offer a more complex and comprehensive picture of the key plasticity processes responsible for polycrystalline ice creep and provide better constraints on the constitutive mechanical laws implemented in ice sheet flow models used to predict the response of Earth ice masses to climate change.

Texture analysis at neutron diffractometer STRESS-SPEC

NASA Astrophysics Data System (ADS)

Brokmeier, H.-G.; Gan, W. M.; Randau, C.; Völler, M.; Rebelo-Kornmeier, J.; Hofmann, M.

2011-06-01

In response to the development of new materials and the application of materials and components in advanced technologies, non-destructive measurement methods of textures and residual stresses have gained worldwide significance in recent years. The materials science neutron diffractometer STRESS-SPEC at FRM II (Garching, Germany) is designed to be applied equally to texture and residual stress analyses by virtue of its very flexible configuration. Due to the high penetration capabilities of neutrons and the high neutron flux of STRESS-SPEC it allows a combined analysis of global texture, local texture, strain pole figure and FWHM pole figure in a wide variety of materials including metals, alloys, composites, ceramics and geological materials. Especially, the analysis of texture gradients in bulk materials using neutron diffraction has advantages over laboratory X-rays and EBSD for many scientific cases. Moreover, neutron diffraction is favourable for coarse-grained materials, where bulk information averaged over texture inhomogeneities is needed, and also stands out due to easy sample preparation. In future, the newly developed robot system for STRESS-SPEC will allow much more flexibility than an Eulerian cradle as on standard instruments. Five recent measurements are shown to demonstrate the wide range of possible texture applications at STRESS-SPEC diffractometer.

Transformation and Precipitation Kinetics in 30Cr10Ni Duplex Stainless Steel

NASA Astrophysics Data System (ADS)

Fazarinc, Matevz; Terčelj, Milan; Bombač, David; Kugler, Goran

2010-09-01

To improve the microstructure during casting, hot forming, and heat treatment of 30Cr10Ni duplex stainless steel, accurate data on the precipitation and transformation processes at high temperatures are needed. In this article, the precipitation and transformation processes at various aging times in the temperature range 873 K to 1573 K (600 °C to 1300 °C) were studied. The 30Cr10Ni ferrous alloy contains a relatively large amount of Cr, Ni, and C, which results in a complex microstructure. In addition to the ferrite, austenite, and sigma phase, the M23C6 and MC carbides were also observed in the microstructure. The precipitation of the sigma phase was observed after just 3 minutes of aging, and after 30 minutes of aging at approximately 1053 K (780 °C), its fraction exceeded 40 pct. An intensive austenite-to-ferrite transformation was observed above 1423 K (1150 °C). Optical microscopy, energy-dispersive X-ray spectroscopy (EDS), electron backscattered diffraction (EBSD), and X-ray diffraction (XRD), as well as micro-indentation hardness, hardness, impact toughness, and tensile tests, were carried out to evaluate the obtained microstructures of aged samples.

An electron back-scattered diffraction study on the microstructure evolution of severely deformed aluminum AI6061 alloy

NASA Astrophysics Data System (ADS)

Vaseghi, M.; Karimi Taheri, A.; Kim, H. S.

2014-08-01

In this paper dynamic strain ageing behavior in an Al-Mg-Si alloy related to equal channel angular pressing (ECAP) was investigated. In order to examine the combined plastic deformation and ageing effects on microstructure evolutions and strengthening characteristics, the Al6061 alloy were subjected to phi=90° ECAP die for up to 4 passes via route Bc at high temperatures. For investigating the effects of ageing temperature and strain rate in ECAP, Vickers hardness tests were performed. The combination of the ECAP process with dynamic ageing at higher temperatures resulted in a significant increase in hardness. The microstructural evolution of the samples was studied using electron back-scattering diffraction (EBSD). The grains of Al6061 aluminum alloy were refined significantly at 100 and 150 °C with greater pass numbers and the distributions of grain size tended to be more uniform with pass number increasing. Frequency of sub-boundaries and low angle grain boundaries (LAGBs) increased at initial stage of deformation, and sub-boundaries and LAGBs evolved into highangle grain boundaries (HAGBs) with further deformation, which resulted in the high frequency of HAGBs in the alloy after ECAP 4 passes.

Effect of Grain Boundary Misorientation on Electromigration in Lead-Free Solder Joints

NASA Astrophysics Data System (ADS)

Tasooji, Amaneh; Lara, Leticia; Lee, Kyuoh

2014-12-01

Reduction in microelectronic interconnect size gives rise to solder bumps consisting of few grains, approaching a single- or bicrystal grain morphology in C4 bumps. Single grain anisotropy, individual grain orientation, presence of easy diffusion paths along grain boundaries, and the increased current density in these small solder bumps aggravate electromigration. This reduces the reliability of the entire microelectronic system. This paper focuses on electromigration behavior in Pb-free solder, specifically the Sn-0.7 wt.%Cu alloy. We discuss the effects of texture, grain orientation, and grain boundary misorientation angle on electromigration (EM) and intermetallic compound formation in EM-tested C4 bumps. The detailed electron backscatter diffraction (EBSD) analysis used in this study reveals the greater influence of grain boundary misorientation on solder bump electromigration compared with the effect associated with individual grain orientation.

Data on processing of Ti-25Nb-25Zr β-titanium alloys via powder metallurgy route: Methodology, microstructure and mechanical properties.

PubMed

Ueda, D; Dirras, G; Hocini, A; Tingaud, D; Ameyama, K; Langlois, P; Vrel, D; Trzaska, Z

2018-04-01

The data presented in this article are related to the research article entitled "Cyclic Shear behavior of conventional and harmonic structure-designed Ti-25Nb-25Zr β-titanium alloy: Back-stress hardening and twinning inhibition" (Dirras et al., 2017) [1]. The datasheet describes the methods used to fabricate two β-titanium alloys having conventional microstructure and so-called harmonic structure (HS) design via a powder metallurgy route, namely the spark plasma sintering (SPS) route. The data show the as-processed unconsolidated powder microstructures as well as the post-SPS ones. The data illustrate the mechanical response under cyclic shear loading of consolidated alloy specimens. The data show how electron back scattering diffraction(EBSD) method is used to clearly identify induced deformation features in the case of the conventional alloy.

DOE Office of Scientific and Technical Information (OSTI.GOV)

Yi, Gaosong; Cullen, David A.; Littrell, Kenneth C.

For this research, long-term aged [343 K (70 °C) for 30 months and natural exposure for over 10 years] Al 5456 H116 samples were characterized using electron backscatter diffraction (EBSD), scanning transmission electron microscopy (STEM), state-of-the-art energy-dispersive X-ray spectroscopy (EDS) systems, and small-angle neutron scattering (SANS). ASTM G-67 mass loss tests of the sensitized Al 5456 alloy samples were conducted. Intragranular Mg-rich precipitates, such as Guinier–Preston (GP) zones, were confirmed in Al 5456 H116 aged at 343 K (70 °C) for 30 months, and the volume of these precipitates is 1.39 pct. β' phase is identified at the grain boundarymore » of a navy ship sample, while high-resolution STEM results reveal no intragranular precipitates. Intergranular corrosion (IGC) of Al 5456 was found to be related to the continuity of intergranular precipitates.« less

Characterization of Laves phase in Crofer 22 H stainless steel.

PubMed

Hsiao, Zheng-Wen; Kuhn, Bernd; Chen, Delphic; Singheiser, Lorenz; Kuo, Jui-Chao; Lin, Dong-Yih

2015-07-01

This study investigated the effect of annealing temperature on the precipitation behavior of Crofer(®) 22 H at 600°C, 700°C, and 800°C. The grain size distribution, precipitate phase identification, and microstructure were analyzed using electron backscatter diffraction (EBSD) and energy dispersive X-ray spectroscopy (EDS). The morphology of Laves phase (Fe,Cr,Si)(2)(Nb,W) precipitates having the Cr(2)Nb structure changed from strip-like to needle-shaped as the annealing temperature was increased. The precipitates of the Laves phase also shifted from the grain boundaries to the grain interiors when the temperature was increased. However, the average grain size (150 μm) of the ferritic matrix did not significantly change at 600°C, 700°C, and 800°C for 10 h. Copyright © 2015 Elsevier Ltd. All rights reserved.

A protocol for searching the most probable phase-retrieved maps in coherent X-ray diffraction imaging by exploiting the relationship between convergence of the retrieved phase and success of calculation.

PubMed

Sekiguchi, Yuki; Hashimoto, Saki; Kobayashi, Amane; Oroguchi, Tomotaka; Nakasako, Masayoshi

2017-09-01

Coherent X-ray diffraction imaging (CXDI) is a technique for visualizing the structures of non-crystalline particles with size in the submicrometer to micrometer range in material sciences and biology. In the structural analysis of CXDI, the electron density map of a specimen particle projected along the direction of the incident X-rays can be reconstructed only from the diffraction pattern by using phase-retrieval (PR) algorithms. However, in practice, the reconstruction, relying entirely on the computational procedure, sometimes fails because diffraction patterns miss the data in small-angle regions owing to the beam stop and saturation of the detector pixels, and are modified by Poisson noise in X-ray detection. To date, X-ray free-electron lasers have allowed us to collect a large number of diffraction patterns within a short period of time. Therefore, the reconstruction of correct electron density maps is the bottleneck for efficiently conducting structure analyses of non-crystalline particles. To automatically address the correctness of retrieved electron density maps, a data analysis protocol to extract the most probable electron density maps from a set of maps retrieved from 1000 different random seeds for a single diffraction pattern is proposed. Through monitoring the variations of the phase values during PR calculations, the tendency for the PR calculations to succeed when the retrieved phase sets converged on a certain value was found. On the other hand, if the phase set was in persistent variation, the PR calculation tended to fail to yield the correct electron density map. To quantify this tendency, here a figure of merit for the variation of the phase values during PR calculation is introduced. In addition, a PR protocol to evaluate the similarity between a map of the highest figure of merit and other independently reconstructed maps is proposed. The protocol is implemented and practically examined in the structure analyses for diffraction patterns from aggregates of gold colloidal particles. Furthermore, the feasibility of the protocol in the structure analysis of organelles from biological cells is examined.

Near-liquidus growth of feldspar spherulites in trachytic melts: 3D morphologies and implications in crystallization mechanisms

NASA Astrophysics Data System (ADS)

Arzilli, Fabio; Mancini, Lucia; Voltolini, Marco; Cicconi, Maria Rita; Mohammadi, Sara; Giuli, Gabriele; Mainprice, David; Paris, Eleonora; Barou, Fabrice; Carroll, Michael R.

2015-02-01

The nucleation and growth processes of spherulitic alkali feldspar have been investigated in this study through X-ray microtomography and electron backscatter diffraction (EBSD) data. Here we present the first data on Shape Preferred Orientation (SPO) and Crystal Preferred Orientation (CPO) of alkali feldspar within spherulites. The analysis of synchrotron X-ray microtomography and EBSD datasets allowed us to study the morphometric characteristics of spherulites in trachytic melts in quantitative fashion, highlighting the three-dimensional shape, preferred orientation, branching of lamellae and crystal twinning, providing insights about the nucleation mechanism involved in the crystallization of the spherulites. The nucleation starts with a heterogeneous nucleus (pre-existing crystal or bubble) and subsequently it evolves forming "bow tie" morphologies, reaching radially spherulitic shapes in few hours. Since each lamella within spherulite is also twinned, these synthetic spherulites cannot be considered as single nuclei but crystal aggregates originated by heterogeneous nucleation. A twin boundary may have a lower energy than general crystal-crystal boundaries and many of the twinned grains show evidence of strong local bending which, combined with twin plane, creates local sites for heterogeneous nucleation. This study shows that the growth rates of the lamellae (10- 6-10- 7 cm/s) in spherulites are either similar or slightly higher than that for single crystals by up to one order of magnitude. Furthermore, the highest volumetric growth rates (10- 11-10- 12 cm3/s) show that the alkali feldspar within spherulites can grow fast reaching a volumetric size of ~ 10 μm3 in 1 s.

Microstructural Quantification of Rapidly Solidified Undercooled D2 Tool Steel

NASA Astrophysics Data System (ADS)

Valloton, J.; Herlach, D. M.; Henein, H.; Sediako, D.

2017-10-01

Rapid solidification of D2 tool steel is investigated experimentally using electromagnetic levitation (EML) under terrestrial and reduced gravity conditions and impulse atomization (IA), a drop tube type of apparatus. IA produces powders 300 to 1400 μm in size. This allows the investigation of a large range of cooling rates ( 100 to 10,000 K/s) with a single experiment. On the other hand, EML allows direct measurements of the thermal history, including primary and eutectic nucleation undercoolings, for samples 6 to 7 mm in diameter. The final microstructures at room temperature consist of retained supersaturated austenite surrounded by eutectic of austenite and M7C3 carbides. Rapid solidification effectively suppresses the formation of ferrite in IA, while a small amount of ferrite is detected in EML samples. High primary phase undercoolings and high cooling rates tend to refine the microstructure, which results in a better dispersion of the eutectic carbides. Evaluation of the cell spacing in EML and IA samples shows that the scale of the final microstructure is mainly governed by coarsening. Electron backscattered diffraction (EBSD) analysis of IA samples reveals that IA powders are polycrystalline, regardless of the solidification conditions. EBSD on EML samples reveals strong differences between the microstructure of droplets solidified on the ground and in microgravity conditions. While the former ones are polycrystalline with many different grains, the EML sample solidified in microgravity shows a strong texture with few much larger grains having twinning relationships. This indicates that fluid flow has a strong influence on grain refinement in this system.

Seismic properties of the upper mantle beneath Lanzarote (Canary Islands): Model predictions based on texture measurements by EBSD

NASA Astrophysics Data System (ADS)

Vonlanthen, Pierre; Kunze, Karsten; Burlini, Luigi; Grobety, Bernard

2006-12-01

We present a petrophysical analysis of upper mantle xenoliths, collected in the Quaternary alkali basalt fields (Series III and IV) from the island of Lanzarote. The samples consist of eight harzburgite and four dunite nodules, 5 to 15 cm in size, and exhibit a typical protogranular to porphyroclastic texture. An anomalous foliation resulting from strong recovery processes is observed in half of the specimens. The lattice preferred orientations (LPO) of olivine, orthopyroxene and clinopyroxene were measured using electron backscatter diffraction (EBSD). In most samples, olivine exhibits LPOs intermediate between the typical single crystal texture and the [100] fiber texture. Occasionally, the [010] fiber texture was also observed. Simultaneous occurrence of both types of fiber textures suggests the existence of more than one deformation regime, probably dominated by a simple shear component under low strain rate and moderate to high temperature. Orthopyroxene and clinopyroxene display a weaker but significant texture. The LPO data were used to calculate the seismic properties of the xenoliths at PT conditions obtained from geothermobarometry, and were compared to field geophysical data reported from the literature. The velocity of P-waves (7.9 km/s) obtained for a direction corresponding to the existing seismic transect is in good agreement with the most recent geophysical interpretation. Our results are consistent with a roughly W-E oriented fastest P-wave propagation direction in the uppermost mantle beneath the Canary Islands, and with the lithosphere structure proposed by previous authors involving a crust-mantle boundary at around 18 km in depth, overlaid by intermediate material between 11 and 18 km.

Quartz c-axis orientation patterns in fracture cement as a measure of fracture opening rate and a validation tool for fracture pattern models

DOE PAGES

Ukar, Estibalitz; Laubach, Stephen E.; Marrett, Randall

2016-03-09

Here, we evaluate a published model for crystal growth patterns in quartz cement in sandstone fractures by comparing crystal fracture-spanning predictions to quartz c-axis orientation distributions measured by electron backscatter diffraction (EBSD) of spanning quartz deposits. Samples from eight subvertical opening-mode fractures in four sandstone formations, the Jurassic– Cretaceous Nikanassin Formation, northwestern Alberta Foothills (Canada), Cretaceous Mesaverde Group (USA; Cozzette Sandstone Member of the Iles Formation), Piceance Basin, Colorado (USA), and upper Jurassic–lower Cretaceous Cotton Valley Group (Taylor sandstone) and overlying Travis Peak Formation, east Texas, have similar quartzose composition and grain size but contain fractures with different temperature historiesmore » and opening rates based on fluid inclusion assemblages and burial history. Spherical statistical analysis shows that, in agreement with model predictions, bridging crystals have a preferred orientation with c-axis orientations at a high angle to fracture walls. The second form of validation is for spanning potential that depends on the size of cut substrate grains. Using measured cut substrate grain sizes and c-axis orientations of spanning bridges, we calculated the required orientation for the smallest cut grain to span the maximum gap size and the required orientation of the crystal with the least spanning potential to form overgrowths that span across maximum measured gap sizes. We find that within a 10° error all spanning crystals conform to model predictions. Using crystals with the lowest spanning potential based on crystallographic orientation (c-axis parallel to fracture wall) and a temperature range for fracture opening measured from fluid inclusion assemblages, we calculate maximum fracture opening rates that allow crystals to span. These rates are comparable to those derived independently from fracture temperature histories based on burial history and multiple sequential fluid inclusion assemblages. Results support the R. Lander and S. Laubach model, which predicts that for quartz deposited synchronously with fracture opening, spanning potential, or likelihood of quartz deposits that are thick enough to span between fracture walls, depends on temperature history, fracture opening rate, size of opening increments, and size, mineralogy, and crystallographic orientation of substrates in the fracture wall (transected grains). Results suggest that EBSD maps, which can be more rapidly acquired than measurement of tens to hundreds of fluid inclusion assemblages, can provide a useful measure of relative opening rates within populations of quartz-filled fractures formed under sedimentary basin conditions. Such data are useful for evaluating fracture pattern development models.« less

Quartz c-axis orientation patterns in fracture cement as a measure of fracture opening rate and a validation tool for fracture pattern models

DOE Office of Scientific and Technical Information (OSTI.GOV)

Ukar, Estibalitz; Laubach, Stephen E.; Marrett, Randall

Here, we evaluate a published model for crystal growth patterns in quartz cement in sandstone fractures by comparing crystal fracture-spanning predictions to quartz c-axis orientation distributions measured by electron backscatter diffraction (EBSD) of spanning quartz deposits. Samples from eight subvertical opening-mode fractures in four sandstone formations, the Jurassic– Cretaceous Nikanassin Formation, northwestern Alberta Foothills (Canada), Cretaceous Mesaverde Group (USA; Cozzette Sandstone Member of the Iles Formation), Piceance Basin, Colorado (USA), and upper Jurassic–lower Cretaceous Cotton Valley Group (Taylor sandstone) and overlying Travis Peak Formation, east Texas, have similar quartzose composition and grain size but contain fractures with different temperature historiesmore » and opening rates based on fluid inclusion assemblages and burial history. Spherical statistical analysis shows that, in agreement with model predictions, bridging crystals have a preferred orientation with c-axis orientations at a high angle to fracture walls. The second form of validation is for spanning potential that depends on the size of cut substrate grains. Using measured cut substrate grain sizes and c-axis orientations of spanning bridges, we calculated the required orientation for the smallest cut grain to span the maximum gap size and the required orientation of the crystal with the least spanning potential to form overgrowths that span across maximum measured gap sizes. We find that within a 10° error all spanning crystals conform to model predictions. Using crystals with the lowest spanning potential based on crystallographic orientation (c-axis parallel to fracture wall) and a temperature range for fracture opening measured from fluid inclusion assemblages, we calculate maximum fracture opening rates that allow crystals to span. These rates are comparable to those derived independently from fracture temperature histories based on burial history and multiple sequential fluid inclusion assemblages. Results support the R. Lander and S. Laubach model, which predicts that for quartz deposited synchronously with fracture opening, spanning potential, or likelihood of quartz deposits that are thick enough to span between fracture walls, depends on temperature history, fracture opening rate, size of opening increments, and size, mineralogy, and crystallographic orientation of substrates in the fracture wall (transected grains). Results suggest that EBSD maps, which can be more rapidly acquired than measurement of tens to hundreds of fluid inclusion assemblages, can provide a useful measure of relative opening rates within populations of quartz-filled fractures formed under sedimentary basin conditions. Such data are useful for evaluating fracture pattern development models.« less

Diffraction-based study of fatigue crack initiation and propagation in aerospace aluminum alloys

NASA Astrophysics Data System (ADS)

Gupta, Vipul K.

The crack initiation sites and microstructure-sensitive growth of small fatigue cracks are experimentally characterized in two precipitation-hardened aluminum alloys, 7075-T651 and 7050-T7451, stressed in ambient temperature moist-air (warm-humid) and -50°C dry N2 (cold-dry) environmental conditions. Backscattered electron imaging (BSE) and energy dispersive spectroscopy (EDS) of the fracture surfaces showed that Fe-Cu rich constituent particle clusters are the most common initiation sites within both alloys stressed in either environment. The crack growth within each alloy, on average, was observed to be slowed in the cold-dry environment than in the warm-humid environment, but only at longer crack lengths. Although no overwhelming effects of grain boundaries and grain orientations on small-crack growth were observed, crack growth data showed local fluctuations within individual grains. These observations are understood as crack propagation through the underlying substructure at the crack surface and frequent interaction with low/high-angle grain and subgrain boundaries, during cyclic loading, and, are further attributed to periodic changes in crack propagation path and multiple occurrences of crack-branching observed in the current study. SEM-based stereology in combination with electron backscattered diffraction (EBSD) established fatigue crack surface crystallography within the region from ˜1 to 50 mum of crack initiating particle clusters. Fatigue crack facets were parallel to a wide variety of crystallographic planes, with pole orientations distributed broadly across the irreducible stereographic triangle between the {001} and {101}-poles within both warm-humid and cold-dry environments. The results indicate environmentally affected fatigue cracking in both cases, given the similarity between the observed morphology and crystallography with that of a variety of aerospace aluminum alloys cracked in the presence of moist-air. There was no evidence of crystallographic {111} slip-plane cracking typical of the Stage I crack growth mode observed in single crystals and high purity polycrystals of face centered cubic metals, and which has presently been assumed for the present materials within fatigue crack initiation models. Rather, the facets tend to have near-Mode I spatial orientation, which is another indicator of the importance of environmentally affected fatigue damage. The results provide a physical basis to develop microstructurally-based next generation multi-stage fatigue (MSF) models that should include a new crack decohesion criteria based upon environmental fatigue cracking mechanisms. EBSD study of small-cracks in alloy 7050-T7451, stressed in warm-humid environment, showed that crack-path orientation changes and crack-branching occurred at both low/high-angle grain and subgrain boundaries. Single surface trace analysis suggests that the crack-path differs substantially from crystallographic slip-planes. EBSD-based observations of small-crack propagation through subgrain structure, either formed by cyclic plastic strain accumulation or pre-existing (typical of unrecrystallized grain structure in the present materials), suggest that subgrain structure plays a crucial role in small fatigue crack propagation. As mentioned earlier, local fluctuations in small-crack growth rates appear to be caused by frequent interaction with subgrain boundaries, and multiple occurrences of crack-branching and crack-path orientation changes at low/high-angle grain and subgrain boundaries. The aforementioned deviation from low-index {001}/{101}-planes and the occurrence of high-index cracking planes observed by EBSD/Stereology, in this study and others, are interpreted as trans-subgranular decohesion or inter-subgranular cracking, due to trapped hydrogen. In summary, the results provide a firmer experimental foundation for, and clearer understanding of, the mechanisms of environmental fatigue cracking of aluminum alloys, especially the role of inter-subgranular cracking, which had previously been advanced based upon fracture surface observations alone.

Plastic strain and grain size effects in the surface roughening of a model aluminum alloy

NASA Astrophysics Data System (ADS)

Moore, Eric Joseph

To address issues surrounding improved automotive fuel economy, an experiment was designed to study the effect of uniaxial plastic tensile deformation on surface roughness and on slip and grain rotation. Electron backscatter diffraction (EBSD) and scanning laser confocal microscopy (SLCM) were used to track grain size, crystallographic texture, and surface topography as a function of incremental true strain for a coarse-grained binary alloy that is a model for AA5xxx series aluminum alloys. One-millimeter thick sheets were heat treated at 425°C to remove previous rolling texture and to grow grains to sizes in the range ˜10-8000 mum. At five different strain levels, 13 sample regions, containing 43 grains, were identified in both EBSD and SLCM micrographs, and crystallographic texture and surface roughness were measured. After heat treatment, a strong cube texture matrix emerged, with bands of generally non-cube grains embedded parallel to the rolling direction (RD). To characterize roughness, height profiles from SLCM micrographs were extracted and a filtered Fourier transform approach was used to separate the profiles into intergranular (long wavelength) and intragranular (short wavelength) signatures. The commonly-used rms roughness parameter (Rq) characterized intragranular results. Two important parameters assess intergranular results in two grain size regimes: surface tilt angle (Deltatheta) and surface height discontinuity (DeltazH) between neighboring grains at a boundary. In general, the magnitude of Rq and Deltatheta increase monotonically with strain and indicate that intergranular roughness is the major contributor to overall surface roughness for true strains up to epsilon = 0.12. Surface height discontinuity DeltazH is defined due to exceptions in surface tilt angle analyses. The range of observed Deltatheta= 1-10° are consistent with the observed 3-12° rotation of individual grains as measured with EBSD. For some grain boundaries with Deltatheta< 4°, the surface height discontinuity DeltazH characterizes the response of adjacent grains in which one or more are large (˜1000-2000 mum), making a 3-12° rotation of the grain highly unlikely. This can be understood by postulating that the energy associated with rotating large grains would exceed the energy to shear along the boundary. Slip and grain boundary shearing are the active mechanisms in these instances.

The effect of grain size on aluminum anodes for Al-air batteries in alkaline electrolytes

NASA Astrophysics Data System (ADS)

Fan, Liang; Lu, Huimin

2015-06-01

Aluminum is an ideal material for metallic fuel cells. In this research, different grain sizes of aluminum anodes are prepared by equal channel angular pressing (ECAP) at room temperature. Microstructure of the anodes is examined by electron backscatter diffraction (EBSD) in scanning electron microscope (SEM). Hydrogen corrosion rates of the Al anodes in 4 mol L-1 NaOH are determined by hydrogen collection method. The electrochemical properties of the aluminum anodes are investigated in the same electrolyte using electrochemical impedance spectroscopy (EIS) and polarization curves. Battery performance is also tested by constant current discharge at different current densities. Results confirm that the electrochemical properties of the aluminum anodes are related to grain size. Finer grain size anode restrains hydrogen evolution, improves electrochemical activity and increases anodic utilization rate. The proposed method is shown to effectively improve the performance of Al-air batteries.

Microstructure effects on the recrystallization of low-symmetry alpha-uranium

DOE Office of Scientific and Technical Information (OSTI.GOV)

McCabe, Rodney James; Richards, Andrew Walter; Coughlin, Daniel Robert

2015-10-01

We employ electron backscatter diffraction (EBSD) to investigate microstructural evolution of uranium during recrystallization. To understand the relationship between microstructure and recrystallization, we use measures of intra-granular misorientation within grains and near grain boundaries in both deformed (non-recrystallized) uranium and recrystallizing uranium. The data show that the level of intra-granular misorientation depends on crystallographic orientation. However, contrary to expectation, this relationship does not significantly affect the recrystallization texture. Rather, the analysis suggests that recrystallization nucleation occurs along high angle grain boundaries in the deformed microstructure. Specifically, we show that the nucleation of recrystallized grains correlates well with the spatially heterogeneousmore » distribution of high angle boundaries. Due to the inhomogeneous distribution of high angle boundaries, the recrystallized microstructure after long times exhibits clustered distributions of small and large grains. Twin boundaries do not appear to act as recrystallization nucleation sites.« less

GaN epitaxial layers grown on multilayer graphene by MOCVD

NASA Astrophysics Data System (ADS)

Li, Tianbao; Liu, Chenyang; Zhang, Zhe; Yu, Bin; Dong, Hailiang; Jia, Wei; Jia, Zhigang; Yu, Chunyan; Gan, Lin; Xu, Bingshe

2018-04-01

In this study, GaN epitaxial layers were successfully deposited on a multilayer graphene (MLG) by using metal-organic chemical vapor deposition (MOCVD). Highly crystalline orientations of the GaN films were confirmed through electron backscatter diffraction (EBSD). An epitaxial relationship between GaN films and MLG is unambiguously established by transmission electron microscope (TEM) analysis. The Raman spectra was used to analyze the internal stress of GaN films, and the spectrum shows residual tensile stress in the GaN films. Moreover, the results of the TEM analysis and Raman spectra indicate that the high quality of the MLG substrate is maintained even after the growth of the GaN film. This high-quality MLG makes it possible to easily remove epitaxial layers from the supporting substrate by micro-mechanical exfoliation technology. This work can aid in the development of transferable devices using GaN films.

Characterization of Al-Mg Alloy Aged at Low Temperatures

DOE PAGES

Yi, Gaosong; Cullen, David A.; Littrell, Kenneth C.; ...

2017-02-06

For this research, long-term aged [343 K (70 °C) for 30 months and natural exposure for over 10 years] Al 5456 H116 samples were characterized using electron backscatter diffraction (EBSD), scanning transmission electron microscopy (STEM), state-of-the-art energy-dispersive X-ray spectroscopy (EDS) systems, and small-angle neutron scattering (SANS). ASTM G-67 mass loss tests of the sensitized Al 5456 alloy samples were conducted. Intragranular Mg-rich precipitates, such as Guinier–Preston (GP) zones, were confirmed in Al 5456 H116 aged at 343 K (70 °C) for 30 months, and the volume of these precipitates is 1.39 pct. β' phase is identified at the grain boundarymore » of a navy ship sample, while high-resolution STEM results reveal no intragranular precipitates. Intergranular corrosion (IGC) of Al 5456 was found to be related to the continuity of intergranular precipitates.« less

Numerical Simulation and Experimental Casting of Nickel-Based Single-Crystal Superalloys by HRS and LMC Directional Solidification Processes

NASA Astrophysics Data System (ADS)

Yan, Xuewei; Wang, Run'nan; Xu, Qingyan; Liu, Baicheng

2017-04-01

Mathematical models for dynamic heat radiation and convection boundary in directional solidification processes are established to simulate the temperature fields. Cellular automaton (CA) method and Kurz-Giovanola-Trivedi (KGT) growth model are used to describe nucleation and growth. Primary dendritic arm spacing (PDAS) and secondary dendritic arm spacing (SDAS) are calculated by the Ma-Sham (MS) and Furer-Wunderlin (FW) models respectively. The mushy zone shape is investigated based on the temperature fields, for both high-rate solidification (HRS) and liquid metal cooling (LMC) processes. The evolution of the microstructure and crystallographic orientation are analyzed by simulation and electron back-scattered diffraction (EBSD) technique, respectively. Comparison of the simulation results from PDAS and SDAS with experimental results reveals a good agreement with each other. The results show that LMC process can provide both dendritic refinement and superior performance for castings due to the increased cooling rate and thermal gradient.

Effects of Temperature and Pressure of Hot Isostatic Pressing on the Grain Structure of Powder Metallurgy Superalloy

PubMed Central

Tan, Liming; He, Guoai; Liu, Feng; Li, Yunping; Jiang, Liang

2018-01-01

The microstructure with homogeneously distributed grains and less prior particle boundary (PPB) precipitates is always desired for powder metallurgy superalloys after hot isostatic pressing (HIPping). In this work, we studied the effects of HIPping parameters, temperature and pressure on the grain structure in PM superalloy FGH96, by means of scanning electron microscope (SEM), electron backscatter diffraction (EBSD), transmission electron microscope (TEM) and Time-of-flight secondary ion spectrometry (ToF-SIMS). It was found that temperature and pressure played different roles in controlling PPB precipitation and grain structure during HIPping, the tendency of grain coarsening under high temperature could be inhibited by increasing HIPping pressure which facilitates the recrystallization. In general, relatively high temperature and pressure of HIPping were preferred to obtain an as-HIPped superalloy FGH96 with diminished PPB precipitation and homogeneously refined grains. PMID:29495312

Effects of Temperature and Pressure of Hot Isostatic Pressing on the Grain Structure of Powder Metallurgy Superalloy.

PubMed

Tan, Liming; He, Guoai; Liu, Feng; Li, Yunping; Jiang, Liang

2018-02-24

The microstructure with homogeneously distributed grains and less prior particle boundary (PPB) precipitates is always desired for powder metallurgy superalloys after hot isostatic pressing (HIPping). In this work, we studied the effects of HIPping parameters, temperature and pressure on the grain structure in PM superalloy FGH96, by means of scanning electron microscope (SEM), electron backscatter diffraction (EBSD), transmission electron microscope (TEM) and Time-of-flight secondary ion spectrometry (ToF-SIMS). It was found that temperature and pressure played different roles in controlling PPB precipitation and grain structure during HIPping, the tendency of grain coarsening under high temperature could be inhibited by increasing HIPping pressure which facilitates the recrystallization. In general, relatively high temperature and pressure of HIPping were preferred to obtain an as-HIPped superalloy FGH96 with diminished PPB precipitation and homogeneously refined grains.

Strain Measurements of Chondrules and Refraction Inclusion in Allende

NASA Technical Reports Server (NTRS)

Tait, Alastair W.; Fisher, Kent R.; Simon, Justin I.

2013-01-01

This study uses traditional strain measurement techniques, combined with X-ray computerized tomography (CT), to evaluate petrographic evidence in the Allende CV3 chondrite for preferred orientation and to measure strain in three dimensions. The existence of petrofabrics and lineations was first observed in carbonaceous meteorites in the 1960's. Yet, fifty years later only a few studies have reported that meteorites record such features. Impacts are often cited as the mechanism for this feature, although plastic deformation from overburden and nebular imbrication have also been proposed. Previous work conducted on the Leoville CV3 and the Parnallee LL3 chondrites, exhibited a minimum uniaxial shortening of 33% and 21%, respectively. Petrofabrics in Allende CV3 have been looked at before; previous workers using Electron Back Scatter Diffraction (EBSD) found a major-axis alignment of olivine inside dark inclusions and an "augen"-like preferred orientation of olivine grains around more competent chondrules

Quantification of Microstructure-Properties-Behavior Relations in Magnesium Alloys Using a Hybrid Approach

NASA Astrophysics Data System (ADS)

Hazeli, K.; Cuadra, J.; Vanniamparambil, P. A.; Carmi, R.; Kontsos, A.

This study presents a hybrid experimental mechanics approach combining multi-scale mechanical testing, in situ nondestructive evaluation and targeted microscopic quantification to identify and quantify critical micro structural parameters that affect properties and overall plasticity of Mg alloys. Room temperature monotonic and cyclic experiments monitored by Digital Image Correlation (DIC) coupled with Acoustic Emission (AE) of Mg Alloys of the AZ series were used for this investigation. Data obtained using the optico-acoustic nondestructive system revealed for the first time the direct connection between surface strain localization effects similar to Luder's bands and pronounced twin activity. Electron Back Scatter Diffraction (EBSD) measurements showed the profuse and spatially inhomogeneous nature of twinning at early stages of plasticity which is related with the onset of yielding and the macroscopic plateau region in the stress-strain curve. Furthermore, twinning/detwinning activity was identified in several grains of tested specimens and during characteristic points of fatigue cycles.

Bauschinger Effect and Back Stress in Gradient Cu-Ge Alloy

NASA Astrophysics Data System (ADS)

Hu, Xianzhi; Jin, Shenbao; Zhou, Hao; Yin, Zhe; Yang, Jian; Gong, Yulan; Zhu, Yuntian; Sha, Gang; Zhu, Xinkun

2017-09-01

Using surface mechanical attrition treatment (SMAT), a gradient structure composed of two gradient structure (GS) layers and a coarse grain (CG) layer was generated from a Cu-5.7 wt pct Ge alloy, significantly improving the yield strength of the sample. Unloading-reloading tests showed an unusual Bauschinger effect in these GS samples. The back stresses caused by the accumulated geometrically necessary dislocations (GNDs) on the GS/CG border increased with increasing strain. As found by electron backscatter diffraction (EBSD), the GNDs are mainly distributed in the gradient structured layer, and the density of the GNDs increase with increasing SMAT time. The effect of the back stress increased with increasing SMAT processing time due to the increase in the strain gradient. The pronounced Bauschinger effect in a GS sample can improve the resistance to forward plastic flow and finally contributes to the high strength of GS samples.

The Effects of Grain Boundaries on the Current Transport Properties in YBCO-Coated Conductors

NASA Astrophysics Data System (ADS)

Yang, Chao; Xia, Yudong; Xue, Yan; Zhang, Fei; Tao, Bowan; Xiong, Jie

2015-10-01

We report a detailed study of the grain orientations and grain boundary (GB) networks in Y2O3 films grown on Ni-5 at.%W substrates. Electron back scatter diffraction (EBSD) exhibited different GB misorientation angle distributions, strongly decided by Y2O3 films with different textures. The subsequent yttria-stabilized zirconia (YSZ) barrier and CeO2 cap layer were deposited on Y2O3 layers by radio frequency sputtering, and YBa2Cu3O7-δ (YBCO) films were deposited by pulsed laser deposition. For explicating the effects of the grain boundaries on the current carry capacity of YBCO films, a percolation model was proposed to calculate the critical current density ( J c) which depended on different GB misorientation angle distributions. The significantly higher J c for the sample with sharper texture is believed to be attributed to improved GB misorientation angle distributions.

DOE Office of Scientific and Technical Information (OSTI.GOV)

Clark, Samuel, E-mail: S.J.Clark@warwick.ac.uk; Janik, Vit, E-mail: V.Janik@warwick.ac.uk; Rijkenberg, Arjan, E-mail: arjan.rijkenberg@tatasteel.com

In-situ characterization techniques have been applied to elucidate the influence of γ/α transformation upon the extent of interphase precipitation in a low-carbon, vanadium-HSLA steel. Electron Back-scattered diffraction analyses of the γ/α orientation relationship with continuous cooling at 2 and 10 K/s suggest that the proportion of ferrite likely to hold interphase precipitation varies little with cooling rate. However, TEM analyses show that the interphase precipitation refines with increasing cooling rate in this cooling range. With cooling rates in excess of 20 K/s, interphase precipitation is increasingly suppressed due to the increasingly diffusional-displacive nature of the Widmanstätten γ/α transformation that ismore » activated. The present study illustrates that the extent and dimensions of interphase precipitation can be controlled through controlled cooling. - Highlights: • In-situ characterization of γ/α transformation • EBSD characterization of γ/α transformation orientation relationship • Extent of interphase precipitation can be controlled through controlled cooling.« less

Texture-Induced Anisotropy in an Inconel 718 Alloy Deposited Using Electron Beam Freeform Fabrication

NASA Technical Reports Server (NTRS)

Tayon, W.; Shenoy, R.; Bird, R.; Hafley, R.; Redding, M.

2014-01-01

A test block of Inconel (IN) 718 was fabricated using electron beam freeform fabrication (EBF(sup 3)) to examine how the EBF(sup 3) deposition process affects the microstructure, crystallographic texture, and mechanical properties of IN 718. Tests revealed significant anisotropy in the elastic modulus for the as-deposited IN 718. Subsequent tests were conducted on specimens subjected to a heat treatment designed to decrease the level of anisotropy. Electron backscatter diffraction (EBSD) was used to characterize crystallographic texture in the as-deposited and heat treated conditions. The anisotropy in the as-deposited condition was strongly affected by texture as evidenced by its dependence on orientation relative to the deposition direction. Heat treatment resulted in a significant improvement in modulus of the EBF(sup 3) product to a level nearly equivalent to that for wrought IN 718 with reduced anisotropy; reduction in texture through recrystallization; and production of a more homogeneous microstructure.

Highlighting material structure with transmission electron diffraction correlation coefficient maps.

PubMed

Kiss, Ákos K; Rauch, Edgar F; Lábár, János L

2016-04-01

Correlation coefficient maps are constructed by computing the differences between neighboring diffraction patterns collected in a transmission electron microscope in scanning mode. The maps are shown to highlight material structural features like grain boundaries, second phase particles or dislocations. The inclination of the inner crystal interfaces are directly deduced from the resulting contrast. Copyright © 2016 Elsevier B.V. All rights reserved.

Dark-field phase retrieval under the constraint of the Friedel symmetry in coherent X-ray diffraction imaging.

PubMed

Kobayashi, Amane; Sekiguchi, Yuki; Takayama, Yuki; Oroguchi, Tomotaka; Nakasako, Masayoshi

2014-11-17

Coherent X-ray diffraction imaging (CXDI) is a lensless imaging technique that is suitable for visualizing the structures of non-crystalline particles with micrometer to sub-micrometer dimensions from material science and biology. One of the difficulties inherent to CXDI structural analyses is the reconstruction of electron density maps of specimen particles from diffraction patterns because saturated detector pixels and a beam stopper result in missing data in small-angle regions. To overcome this difficulty, the dark-field phase-retrieval (DFPR) method has been proposed. The DFPR method reconstructs electron density maps from diffraction data, which are modified by multiplying Gaussian masks with an observed diffraction pattern in the high-angle regions. In this paper, we incorporated Friedel centrosymmetry for diffraction patterns into the DFPR method to provide a constraint for the phase-retrieval calculation. A set of model simulations demonstrated that this constraint dramatically improved the probability of reconstructing correct electron density maps from diffraction patterns that were missing data in the small-angle region. In addition, the DFPR method with the constraint was applied successfully to experimentally obtained diffraction patterns with significant quantities of missing data. We also discuss this method's limitations with respect to the level of Poisson noise in X-ray detection.

Automated grain mapping using wide angle convergent beam electron diffraction in transmission electron microscope for nanomaterials.

PubMed

Kumar, Vineet

2011-12-01

The grain size statistics, commonly derived from the grain map of a material sample, are important microstructure characteristics that greatly influence its properties. The grain map for nanomaterials is usually obtained manually by visual inspection of the transmission electron microscope (TEM) micrographs because automated methods do not perform satisfactorily. While the visual inspection method provides reliable results, it is a labor intensive process and is often prone to human errors. In this article, an automated grain mapping method is developed using TEM diffraction patterns. The presented method uses wide angle convergent beam diffraction in the TEM. The automated technique was applied on a platinum thin film sample to obtain the grain map and subsequently derive grain size statistics from it. The grain size statistics obtained with the automated method were found in good agreement with the visual inspection method.

[Micro-area characteristics of laminated chert in the volcanic rocks of Xionger Group of Ruyang area and its geological significances].

PubMed

Luo, An; Li, Hong-zhong; Zhao, Ming-zhen; Yang, Zhi-jun; Liang, Jin; He, Jun-guo

2014-12-01

The Xionger Group was originated from the volcanic eruption and sedimentation in Precambrian, whose sedimentary strata at the top were named Majiahe Formation. In the Majiahe Formation, there were hydrothermal chert widely distributed, which were exhibited to be interlayers in the volcanic rocks. The polarized microscope, X-ray diffraction (XRD), Raman and electron back scatter diffraction (EBSD) were conducted to study the characteristics in micro area of the jasperite samples, which were from the sedimentary interlayers in the volcanic rocks of Majiahe Formation in Xionger Group. As shown in the microphotographs and EBSD images, the quartz in the chert had small grain size, low degree of crystallinity and close packed structure, which quite agreed with the characteristics of hydrothermal sedimentary chert. In the chert of Xionger Group, there were clear banded (or lamellar) structures which were contributed by the diversities of the grain size and mineral composition. The different bands (or lamellars) had alternative appearance repeatedly, and denoted the diversities and periodic changes in the substance supply during the precipitation. According to the results of the XRD analysis, the majority minerals of the chert was low temperature quartz, whose lattice parameters were a=b=0.4913 nm, c=0.5405 nm and Z=3. As denoted in the EBSD image and result of Raman analysis, several impurity minerals were formed in the chert in different stages, whose geneses and formation time were quite different. The clay minerals and pyrite were scattered in distribution, and should be contributed by the original sedimentation. On contrary, the felsic minerals and mafic silicate minerals were originated from the sedimentation of tuffaceous substance during the volcanic eruption. The minerals of volcanic genesis had relatively larger grain size, and they deposited together with the hydrothermal sediments to form the bands (or lamellars) of coarse minerals. However, the hydrothermal sedimentation contributed to the bands (or lamellars) with minerals of much smaller grain size, which therefore resulted in diversities from the other bands (or lamellars). According to this, the repeated bands (or lamellars) denoted the volcanic activities were cyclic during the formation of the chert. What's more, the carbonate vein came from the precipitation of subsequent hydrothermal fluids in the fracture of the chert, which contributed to the changes (e. g. rising in crystallinity degree of silica and formation of micro-structure of new silicate) near the interface between chert and the carbonate vein. Although there were many impurity minerals with complex genesis, the relatively lower content of silica in the chert of Xionger Group was due to the volcanic mineral mainly. Since there were impurity minerals of volcanic genesis in relatively large amount, the content of silica in the chert of Xionger Group was hence relatively low. In this study, the Raman analysis was witnessed to be an effective way in the researches on the chert, and could open out the type of mineral, micro-structure and degrees of crystallinity (or order). These characteristics were well kept in the micro-area, and played significant roles to reflect and understand the formation mechanism and subsequent evolution of the chert.

Local nanoscale strain mapping of a metallic glass during in situ testing

NASA Astrophysics Data System (ADS)

Gammer, Christoph; Ophus, Colin; Pekin, Thomas C.; Eckert, Jürgen; Minor, Andrew M.

2018-04-01

The local elastic strains during tensile deformation in a CuZrAlAg metallic glass are obtained by fitting an elliptic shape function to the characteristic amorphous ring in electron diffraction patterns. Scanning nanobeam electron diffraction enables strain mapping with a resolution of a few nanometers. Here, a fast direct electron detector is used to acquire the diffraction patterns at a sufficient speed to map the local transient strain during continuous tensile loading in situ in the transmission electron microscope. The elastic strain in tensile direction was found to increase during loading. After catastrophic fracture, a residual elastic strain that relaxes over time was observed.

Sample Preparation Techniques for Grain Boundary Characterization of Annealed TRISO-Coated Particles

DOE Office of Scientific and Technical Information (OSTI.GOV)

Dunzik-Gougar, M. L.; van Rooyen, I. J.; Hill, C. M.

Crystallographic information about chemical vapor deposition layers of silicon carbide (SiC) is essential to understanding layer performance, especially when the layers are in non planar geometries, such as spherical. We performed electron Back Scatter Diffraction (EBSD) analysis of spherical SiC layers using a different approach to sample focus ion beam milling technique to avoid the negative impacts of traditional sample polishing and to address the need of very small samples of irradiated materials for analysis. Mechanical and chemical grinding and polishing of sample surfaces can introduce lattice strains and result in unequal removal of SiC and surrounding layers of differentmore » material due to the hardness differences of these materials. The nature of layer interfaces is thought to play a key role in performance of the SiC; therefore, analysis of representative samples at these interfacial areas is crucial. In work reported here, a focused ion beam (FIB) was employed in a novel manner to prepare a more representative sample for EBSD analysis from TRISO layers free of effects introduced by mechanical and chemical preparation methods. In addition, the difficulty of handling neutron irradiated microscopic samples such as those analyzed in this work has been simplified with pre tilted mounting stages. Our study showed that although the average grain size of samples may be similar, the grain boundary characteristics may differ significantly. It was also found that low angle grain boundaries, comprises 25% in the FIB-prepared sample vs only 1-2% in the polished sample measured in the same particle. From this study it was determined that results of FIB prepared sample will provide more repeatable results, as the role of sample preparation is eliminated.« less

Effects of two-step homogenization on precipitation behavior of Al{sub 3}Zr dispersoids and recrystallization resistance in 7150 aluminum alloy

DOE Office of Scientific and Technical Information (OSTI.GOV)

Guo, Zhanying; Key Laboratory for Anisotropy and Texture of Materials, Northeastern University, Shenyang 110819, China,; Zhao, Gang

2015-04-15

The effect of two-step homogenization treatments on the precipitation behavior of Al{sub 3}Zr dispersoids was investigated by transmission electron microscopy (TEM) in 7150 alloys. Two-step treatments with the first step in the temperature range of 300–400 °C followed by the second step at 470 °C were applied during homogenization. Compared with the conventional one-step homogenization, both a finer particle size and a higher number density of Al{sub 3}Zr dispersoids were obtained with two-step homogenization treatments. The most effective dispersoid distribution was attained using the first step held at 300 °C. In addition, the two-step homogenization minimized the precipitate free zonesmore » and greatly increased the number density of dispersoids near dendrite grain boundaries. The effect of two-step homogenization on recrystallization resistance of 7150 alloys with different Zr contents was quantitatively analyzed using the electron backscattered diffraction (EBSD) technique. It was found that the improved dispersoid distribution through the two-step treatment can effectively inhibit the recrystallization process during the post-deformation annealing for 7150 alloys containing 0.04–0.09 wt.% Zr, resulting in a remarkable reduction of the volume fraction and grain size of recrystallization grains. - Highlights: • Effect of two-step homogenization on Al{sub 3}Zr dispersoids was investigated by TEM. • Finer and higher number of dispersoids obtained with two-step homogenization • Minimized the precipitate free zones and improved the dispersoid distribution • Recrystallization resistance with varying Zr content was quantified by EBSD. • Effectively inhibit the recrystallization through two-step treatments in 7150 alloy.« less

Sample Preparation Techniques for Grain Boundary Characterization of Annealed TRISO-Coated Particles

DOE PAGES

Dunzik-Gougar, M. L.; van Rooyen, I. J.; Hill, C. M.; ...

2016-08-25

Crystallographic information about chemical vapor deposition layers of silicon carbide (SiC) is essential to understanding layer performance, especially when the layers are in non planar geometries, such as spherical. We performed electron Back Scatter Diffraction (EBSD) analysis of spherical SiC layers using a different approach to sample focus ion beam milling technique to avoid the negative impacts of traditional sample polishing and to address the need of very small samples of irradiated materials for analysis. Mechanical and chemical grinding and polishing of sample surfaces can introduce lattice strains and result in unequal removal of SiC and surrounding layers of differentmore » material due to the hardness differences of these materials. The nature of layer interfaces is thought to play a key role in performance of the SiC; therefore, analysis of representative samples at these interfacial areas is crucial. In work reported here, a focused ion beam (FIB) was employed in a novel manner to prepare a more representative sample for EBSD analysis from TRISO layers free of effects introduced by mechanical and chemical preparation methods. In addition, the difficulty of handling neutron irradiated microscopic samples such as those analyzed in this work has been simplified with pre tilted mounting stages. Our study showed that although the average grain size of samples may be similar, the grain boundary characteristics may differ significantly. It was also found that low angle grain boundaries, comprises 25% in the FIB-prepared sample vs only 1-2% in the polished sample measured in the same particle. From this study it was determined that results of FIB prepared sample will provide more repeatable results, as the role of sample preparation is eliminated.« less

Characterization of the multilayered shell of a limpet, Lottia kogamogai (Mollusca: Patellogastropoda), using SEM-EBSD and FIB-TEM techniques.

PubMed

Suzuki, Michio; Kameda, Jun; Sasaki, Takenori; Saruwatari, Kazuko; Nagasawa, Hiromichi; Kogure, Toshihiro

2010-08-01

The microstructure and its crystallographic aspect of the shell of a limpet, Lottiakogamogai, have been investigated, as the first step to clarify the mechanism of shell formation in limpet. The shell consists of five distinct layers stacked along the shell thickness direction. Transmission electron microscopy (TEM) with the focused ion beam (FIB) sample preparation technique was primarily adopted, as well as scanning electron microscopy (SEM) with electron back-scattered diffraction (EBSD). The five layers were termed as M+3, M+2, M+1, M, M-1 from the outside to the inside in previous works, where M means myostracum. The outmost M+3 layer consists of calcite with a "mosaic" structure; granular submicron sub-grains with small-angle grain boundaries often accompanying dislocation arrays. M+2 layer consists of flat prismatic aragonite crystals with a leaf-like cross section, stacked obliquely to the shell surface. It looks that the prismatic crystals are surrounded by organic sheets, forming a compartment structure. M+1 and M-1 layers adopt a crossed lamellar structure consisting of aragonite flat prisms with rectangular cross section. M layer has a prismatic structure of aragonite perpendicular to the shell surface and with irregular shaped cross sections. Distinct organic sheets were not observed between the crystals in M+1, M and M-1 layers. The {110} twins are common in all aragonite M+2, M+1, M and M-1 layers, with the twin boundaries parallel to the prisms. These results for the microstructure of each layer should be considered in the discussion of the formation mechanism of the limpet shell structure. Copyright 2010 Elsevier Inc. All rights reserved.

Microstructure evolution and dynamic recrystallization behavior of a powder metallurgy Ti-22Al-25Nb alloy during hot compression

DOE Office of Scientific and Technical Information (OSTI.GOV)

Jia, Jianbo

The flow behavior of a powder metallurgy (P/M) Ti-22Al-25Nb alloy during hot compression tests has been investigated at a strain rate of 0.01 s{sup −1} and a temperature range of 980–1100 °C up to various true strains from 0.1 to 0.9. The effects of deformation temperature and strain on microstructure characterization and nucleation mechanisms of dynamic recrystallization (DRX) were assessed by means of Optical microscope (OM), electron backscatter diffraction (EBSD) and transmission electron microscope (TEM) techniques, respectively. The results indicated that the process of DRX was promoted by increasing deformation temperature and strain. By regression analysis, a power exponent relationshipmore » between peak stresses and sizes of stable DRX grains was developed. In addition, it is suggested that the discontinuous dynamic recrystallization (DDRX) and continuous dynamic recrystallization (CDRX) controlled nucleation mechanisms for DRX grains operated simultaneously during the whole hot process, and which played the leading role varied with hot process parameters of temperature and strain. It was further demonstrated that the CDRX featured by progressive subgrain rotation was weakened by elevating deformation temperatures. - Highlights: •Flow behavior of a P/M Ti-22Al-25Nb is studied by hot compression tests. •Microstructure evolution of alloy is affected by deformation temperature and strain. •The relationship between peak stress and stable DRX grain size was developed. •The process of DRX was promoted by increasing deformation temperature and strain. •Nucleation mechanisms of DRX were identified by EBSD analysis and TEM observation.« less

The Effect of Sn Orientation on Intermetallic Compound Growth in Idealized Sn-Cu-Ag Interconnects

NASA Astrophysics Data System (ADS)

Kinney, Chris; Linares, Xioranny; Lee, Kyu-Oh; Morris, J. W.

2013-04-01

The work reported here explores the influence of crystal orientation on the growth of the interfacial intermetallic layer during electromigration in Cu||Sn||Cu solder joints. The samples were thin, planar Sn-Ag-Cu (SAC) solder layers between Cu bars subject to a uniaxial current. Electron backscatter diffraction (EBSD) was used to characterize the microstructure before and after testing. The most useful representation of the EBSD data identifies the Sn grain orientation by the angle between the Sn c-axis and the current direction. The tested samples included single-crystal joints with c-axis nearly parallel to the current ("green" samples) and with c-axis perpendicular to the current ("red" samples). At current density of 104 A/cm2 (steady-state temperature of ~150°C), an intermetallic layer grew at an observable rate in the "green" samples, but not in the "red" ones. A current density of 1.15 × 104 A/cm2 (temperature ~160°C) led to measurable intermetallic growth in both samples. The growth fronts were nearly planar and the growth rates constant (after an initial incubation period); the growth rates in the "green" samples were about 10× those in the "red" samples. The Cu concentrations were constant within the joints, showing that the intermetallic growth is dominated by the electromigration flux. The measured growth rates and literature values for the diffusion of Cu in Sn were used to extract values for the effective charge, z *, that governs the electromigration of Cu. The calculated value of z * is significantly larger for current perpendicular to the c-axis than along it.

Optimizing disk registration algorithms for nanobeam electron diffraction strain mapping

DOE PAGES

Pekin, Thomas C.; Gammer, Christoph; Ciston, Jim; ...

2017-01-28

Scanning nanobeam electron diffraction strain mapping is a technique by which the positions of diffracted disks sampled at the nanoscale over a crystalline sample can be used to reconstruct a strain map over a large area. However, it is important that the disk positions are measured accurately, as their positions relative to a reference are directly used to calculate strain. Here in this study, we compare several correlation methods using both simulated and experimental data in order to directly probe susceptibility to measurement error due to non-uniform diffracted disk illumination structure. We found that prefiltering the diffraction patterns with amore » Sobel filter before performing cross correlation or performing a square-root magnitude weighted phase correlation returned the best results when inner disk structure was present. Lastly, we have tested these methods both on simulated datasets, and experimental data from unstrained silicon as well as a twin grain boundary in 304 stainless steel.« less

The nucleation and growth mechanism of Ni-Sn eutectic in a single crystal superalloy

NASA Astrophysics Data System (ADS)

Jiang, Weiguo; Wang, Li; Li, Xiangwei; Lou, Langhong

2017-12-01

The microstructure of single crystal superalloy with and without tin layer on the surface of as-cast and heat-treatment state was investigated by optical microscope (OM) and scanning electron microscopy (SEM). The composition of different regions on the surface was tested by energy dispersive X-ray (EDS). The reaction intermetallic compound (IMC) formed in the heat treatment process was confirmed by X-ray diffraction (XRD). The orientations of different microstructure in samples as heat treatment state were determined by electron back-scattering diffraction (EBSD) method. The porosity location in the interdendritic region was observed by X-ray computed tomography (XCT). The experiment results showed that the remained Sn on the surface of the superalloy reacted with Ni, and then formed Ni3Sn4 in the as-cast state. Sn enriched by diffusion along the porosity located in the interdendritic region and γ + γ‧ (contain a little of Sn) eutectic and Ni3Sn2 formed in single crystal superalloy during heat treatment, and the recalescence behaviors were found. Ni3Sn2 nucleated independently in the cooled liquid at the front of (γ + γ‧) (Sn) eutectic. The nucleation and growth mechanism of the eutectic and Ni3Sn2 IMC during heat treatment was discussed in the present paper.

Comparison between different techniques applied to quartz CPO determination in granitoid mylonites

NASA Astrophysics Data System (ADS)

Fazio, Eugenio; Punturo, Rosalda; Cirrincione, Rosolino; Kern, Hartmut; Wenk, Hans-Rudolph; Pezzino, Antonino; Goswami, Shalini; Mamtani, Manish

2016-04-01

Since the second half of the last century, several techniques have been adopted to resolve the crystallographic preferred orientation (CPO) of major minerals constituting crustal and mantle rocks. To this aim, many efforts have been made to increase the accuracy of such analytical devices as well as to progressively reduce the time needed to perform microstructural analysis. It is worth noting that many of these microstructural studies deal with quartz CPO because of the wide occurrence of this mineral phase in crustal rocks as well as its quite simple chemical composition. In the present work, four different techniques were applied to define CPOs of dynamically recrystallized quartz domains from naturally deformed rocks collected from a ductile crustal scale shear zone in order to compare their advantages and limitation. The selected Alpine shear zone is located in the Aspromonte Massif (Calabrian Peloritani Orogen, southern Italy) representing granitoid lithotypes. The adopted methods span from "classical" universal stage (US), to image analysis technique (CIP), electron back-scattered diffraction (EBSD), and time of flight neutron diffraction (TOF). When compared, bulk texture pole figures obtained by means of these different techniques show a good correlation. Advances in analytical techniques used for microstructural investigations are outlined by discussing results of quartz CPO that are presented in this study.

Cube texture formation during the early stages of recrystallization of Al-1%wt.Mn and AA1050 aluminium alloys

NASA Astrophysics Data System (ADS)

Miszczyk, M. M.; Paul, H.

2015-08-01

The cube texture formation during primary recrystallization was analysed in plane strain deformed samples of a commercial AA1050 alloy and an Al-1%wt.Mn model alloy single crystal of the Goss{110}<001> orientation. The textures were measured with the use of X-ray diffraction and scanning electron microscopy equipped with an electron backscattered diffraction facility. After recrystallization of the Al-1%wt.Mn single crystal, the texture of the recrystallized grains was dominated by four variants of the S{123}<634> orientation. The cube grains were only sporadically detected by the SEM/EBSD system. Nevertheless, an increased density of <111> poles corresponding to the cube orientation was observed. The latter was connected with the superposition of four variants of the S{123}<634> orientation. This indicates that the cube texture after the recrystallization was a ‘compromise texture’. In the case of the recrystallized AA1050 alloy, the strong cube texture results from both the increased density of the particular <111> poles of the four variants of the S orientation and the ∼40°(∼< 111>)-type rotation. The first mechanism transforms the Sdef-oriented areas into Srex ones, whereas the second the near S-oriented, as-deformed areas into near cube-oriented grains.

Improvement of Strength-Toughness-Hardness Balance in Large Cross-Section 718H Pre-Hardened Mold Steel

PubMed Central

Liu, Hanghang; Fu, Paixian; Liu, Hongwei; Li, Dianzhong

2018-01-01

The strength-toughness combination and hardness uniformity in large cross-section 718H pre-hardened mold steel from a 20 ton ingot were investigated with three different heat treatments for industrial applications. The different microstructures, including tempered martensite, lower bainite, and retained austenite, were obtained at equivalent hardness. The microstructures were characterized by using metallographic observations, scanning electron microscopy (SEM), transmission electron microscopy (TEM), X-ray diffraction (XRD), and electron back-scattered diffraction (EBSD). The mechanical properties were compared by tensile, Charpy U-notch impact and hardness uniformity tests at room temperature. The results showed that the test steels after normalizing-quenching-tempering (N-QT) possessed the best strength-toughness combination and hardness uniformity compared with the conventional quenched-tempered (QT) steel. In addition, the test steel after austempering-tempering (A-T) demonstrated the worse hardness uniformity and lower yield strength while possessing relatively higher elongation (17%) compared with the samples after N-QT (14.5%) treatments. The better ductility of A-T steel mainly depended on the amount and morphology of retained austenite and thermal/deformation-induced twined martensite. This work elucidates the mechanisms of microstructure evolution during heat treatments and will highly improve the strength-toughness-hardness trade-off in large cross-section steels. PMID:29642642

Effect of cold deformation on the recrystallization behavior of FePd alloy at the ordering temperature using electron backscatter diffraction

DOE Office of Scientific and Technical Information (OSTI.GOV)

Lin, Hung-Pin; Chen, Yen-Chun; Chen, Delphic

2014-08-15

In this study, the evolution of the recrystallization texture and microstructure was investigated after annealing of 50% and 90% cold-rolled FePd alloy at 530 °C. The FePd alloy was produced by vacuum arc melting in an atmosphere of 97% Ar and 3% H{sub 2}. The specimens were cold rolled to achieve 50% and 90% reduction in thickness. Electron backscatter diffraction measurements were performed on the rolling direction–normal direction section. With increased deformation from 50% to 90%, recrystallized texture transition occurs. For the 50% cold-rolled alloy, the preferred orientation is (0 1 0) [11 0 1], which is close to themore » cubic orientation after 400 h of annealing. For the 90% cold-rolled alloy, the orientation changes to (0 5 4) [22–4 5] after 16 h of annealing. - Highlights: • Texture and microstructure in cold-rolled FePd alloy was investigated during annealing using EBSD. • The recrystallized texture of 50% cold-rolled FePd is (0 1 0) [11 0 1] at 530 °C for 400 hours. • The recrystallized texture of 90% cold-rolled FePd is changed to (0 5 4) [22–4 5] at 530 °C after 16 hours.« less

Microstructure and Texture Development during Cold Rolling in UNS S32205 and UNS S32760 Duplex Stainless Steels

NASA Astrophysics Data System (ADS)

Kumar, Amit; Khatirkar, Rajesh Kisni; Chalapathi, Darshan; Kumar, Gulshan; Suwas, Satyam

2017-05-01

In the present study, microstructure and texture evolution during cold rolling in UNS S32205 and UNS S32760 duplex stainless steel was investigated. Both steels were unidirectionally cold rolled up to 80 pct thickness reduction. Scanning electron microscopy and electron backscattered diffraction (EBSD) were used for microstructural characterization, while X-ray diffraction (XRD) was used for the measurement of bulk texture. Strain-induced martensite (SIM) was identified and quantified with the help of magnetic measurements (B-H curve and magnetization saturation). With the increase in plastic strain, the grains became morphologically elongated along the rolling direction with the reduction in average band thickness and band spacing. SIM increased with the increase in deformation and was found to be a function of strain and the SFE of austenite. The increase in SIM was much more pronounced in UNS S32205 steel as compared to UNS S32760 steel. After cold rolling, strong α-fiber (RD//<110>) texture was developed in ferrite, while brass texture was dominant in austenite for both steels. The strength of texture components and fibers was stronger in UNS S32760 steel. Another significant feature was the development of weak γ-fiber (ND//<111>) in UNS S32760 steel at intermediate deformation.

Effect of screw threading dislocations and inverse domain boundaries in GaN on the shape of reciprocal-space maps.

PubMed

Barchuk, Mykhailo; Motylenko, Mykhaylo; Lukin, Gleb; Pätzold, Olf; Rafaja, David

2017-04-01

The microstructure of polar GaN layers, grown by upgraded high-temperature vapour phase epitaxy on [001]-oriented sapphire substrates, was studied by means of high-resolution X-ray diffraction and transmission electron microscopy. Systematic differences between reciprocal-space maps measured by X-ray diffraction and those which were simulated for different densities of threading dislocations revealed that threading dislocations are not the only microstructure defect in these GaN layers. Conventional dark-field transmission electron microscopy and convergent-beam electron diffraction detected vertical inversion domains as an additional microstructure feature. On a series of polar GaN layers with different proportions of threading dislocations and inversion domain boundaries, this contribution illustrates the capability and limitations of coplanar reciprocal-space mapping by X-ray diffraction to distinguish between these microstructure features.

Unraveling Recrystallization Mechanisms Governing Texture Development from Rare Earth Element Additions to Magnesium

NASA Astrophysics Data System (ADS)

Imandoust, Aidin

The origin of texture components associated with rare-earth (RE) element additions in wrought magnesium (Mg) alloys is a long-standing problem in magnesium technology. The objective of this research is to identify the mechanisms accountable for rare-earth texture during dynamic recrystallization (DRX). Towards this end, we designed binary Mg-Cerium and Mg-Gadolinium alloys along with complex alloy compositions containing zinc, yttrium and Mischmetal. Binary alloys along with pure Mg were designed to individually investigate their effects on texture evolutions, while complex compositions are designed to develop randomized texture, and be used in automotive and aerospace applications. We selected indirect extrusion to thermo-mechanically process our materials. Different extrusion ratios and speeds were designed to produce partially and fully recrystallized microstructures, allowing us to analyze DRX from its early stages to completion. X-ray diffraction, electron backscattered diffraction (EBSD) and transmission electron microscopy (TEM) were used to conduct microstructure and texture analyses. Our analyses revealed that rare-earth elements in zinc-containing magnesium alloys promote discontinuous dynamic recrystallization at the grain boundaries. During nucleation, the effect of rare earth elements on orientation selection was explained by the concomitant actions of multiple Taylor axes in the same grain. Isotropic grain growth was observed due to rare earth elements segregating to grain boundaries, which lead to texture randomization. The nucleation in binary Mg-RE alloys took place by continuous formation of necklace structures. Stochastic relaxation of basal and non-basal dislocations into low-angle grain boundaries produced chains of embryos with nearly random orientations. Schmid factor analysis showed a lower net activation of dislocations in RE textured grains compared to ones on the other side of the stereographic triangle. Lower dislocation densities within RE grains favored their growth by setting the boundary migration direction toward grains with higher dislocation density, thereby decreasing the system energy. We investigated the influence of RE elements on extension twinning induced hardening. RE addition enhanced tensile twinning induced hardening significantly. EBSD analysis illustrated that tensile twins cross low angle grain boundaries in Mg-RE alloys, which produced large twins and facilitated transmutation of basal to prismatic dislocations. Higher activity of pyramidal II dislocations in Mg-RE alloys resulted in higher twinning induced hardening.

Quartz preferred orientation in naturally deformed mylonitic rocks (Montalto shear zone-Italy): a comparison of results by different techniques, their advantages and limitations

NASA Astrophysics Data System (ADS)

Fazio, Eugenio; Punturo, Rosalda; Cirrincione, Rosolino; Kern, Hartmut; Pezzino, Antonino; Wenk, Hans-Rudolf; Goswami, Shalini; Mamtani, Manish A.

2017-10-01

In the geologic record, the quartz c-axis patterns are widely adopted in the investigation of crystallographic preferred orientations (CPO) of naturally deformed rocks. To this aim, in the present work, four different methods for measuring quartz c-axis orientations in naturally sheared rocks were applied and compared: the classical universal stage technique, the computer-integrated polarization microscopy method (CIP), the time-of-flight (TOF) neutron diffraction analysis , and the electron backscatter diffraction (EBSD). Microstructural analysis and CPO patterns of quartz, together with the ones obtained for feldspars and micas in mylonitic granitoid rocks, have been then considered to solve structural and geological questions related to the Montalto crustal scale shear zone (Calabria, southern Italy). Results obtained by applying the different techniques are discussed, and the advantages as well as limitations of each method are highlighted. Importantly, our findings suggest that patterns obtained by means of different techniques are quite similar. In particular, for such mylonites, a subsimple shear (40% simple shear vs 60% pure shear) by shape analysis of porphyroclasts was inferred. A general tendency of an asymmetric c-maximum near to the Z direction (normal to foliation) suggesting dominant basal slip, consistent with fabric patterns related to dynamically recrystallization under greenschist facies, is recognized. Rhombohedral slip was likely active as documented by pole figures of positive and negative rhombs (TOF), which reveal also potential mechanical Dauphiné twinning. Results showed that the most complete CPO characterization on deformed rocks is given by the TOF (from which also other quartz crystallographic axes can be obtained as well as various mineral phases may be investigated). However, this use is restricted by the fact that (a) there are very few TOF facilities around the world and (b) there is loss of any domainal reference, since TOF is a bulk type analysis. EBSD is a widely used technique, which allows an excellent microstructural control of the user covering a good amount of investigated grains. CIP and US are not expensive techniques with respect the other kind of investigations and even if they might be considered obsolete and/or time-consuming, they have the advantage to provide a fine and grain by grain "first round" inspection on the investigated rock fabric.

The Influence on Microstructure and Microtexture on Fatigue Crack Initiation and Growth in Alpha + Beta Titanium

DTIC Science & Technology

2011-10-01

crack growth, microstructure, EBSD, fractography 16. SECURITY CLASSIFICATION OF: 17. LIMITATION OF ABSTRACT: SAR NUMBER OF PAGES 6 19a...differences in thermomechanical processing routes have been correlated with variations in fatigue life through the use of quantitative fractography ...Keywords: fatigue, crack initiation, crack growth, microstructure, EBSD, fractography 1. Introduction Two-phase titanium alloys have the unique

Synchrotron X-ray reciprocal-space mapping, topography and diffraction resolution studies of macromolecular crystal quality.

PubMed

Boggon, T J; Helliwell, J R; Judge, R A; Olczak, A; Siddons, D P; Snell, E H; Stojanoff, V

2000-07-01

A comprehensive study of microgravity and ground-grown chicken egg-white lysozyme crystals is presented using synchrotron X-ray reciprocal-space mapping, topography techniques and diffraction resolution. Microgravity crystals displayed reduced intrinsic mosaicities on average, but no differences in terms of strain over their ground-grown counterparts. Topographic analysis revealed that in the microgravity case the majority of the crystal was contributing to the peak of the reflection at the appropriate Bragg angle. In the ground-control case only a small volume of the crystal contributed to the intensity at the diffraction peak. The techniques prove to be highly complementary, with the reciprocal-space mapping providing a quantitative measure of the crystal mosaicity and strain (or variation in lattice spacing) and the topography providing a qualitative overall assessment of the crystal in terms of its X-ray diffraction properties. Structural data collection was also carried out at the synchrotron.

Synchrotron X-Ray Reciprocal Space Mapping, Topography and Diffraction Resolution Studies of Macromolecular Crystal Quality

NASA Technical Reports Server (NTRS)

Boggon, T. J.; Helliwell, J. R.; Judge, Russell A.; Siddons, D. P.; Snell, Edward H.; Stojanoff, V.

2000-01-01

A comprehensive study of microgravity and ground grown chicken egg white lysozyme crystals is presented using synchrotron X-ray reciprocal space mapping, topography techniques and diffraction resolution. Microgravity crystals displayed, on average, reduced intrinsic mosaicities but no differences in terms of stress over their earth grown counterparts. Topographic analysis revealed that in the microgravity case the majority of the crystal was contributing to the peak of the reflection at the appropriate Bragg angle. In the earth case at the diffraction peak only a small volume of the crystal contributed to the intensity. The techniques prove to be highly complementary with the reciprocal space mapping providing a quantitative measure of the crystal mosaicity and stress (or variation in lattice spacing) and topography providing a qualitative overall assessment of the crystal in terms of its X-ray diffraction properties. Structural data collection was also carried out both at the synchrotron and in the laboratory.

Anisotropy of magnetic susceptibility versus lattice- and shape-preferred orientation in the Lac Tio hemo-ilmenite ore body (Grenville province, Quebec)

NASA Astrophysics Data System (ADS)

Bolle, Olivier; Charlier, Bernard; Bascou, Jérôme; Diot, Hervé; McEnroe, Suzanne A.

2014-08-01

The Lac Tio hemo-ilmenite ore body crops out in the outer portion of the 1.06 Ga Lac Allard anorthosite, a member of the Havre-Saint-Pierre anorthosite suite from the Grenville province of North America. It is made up of ilmenitite (commonly with more than 95% hemo-ilmenite) associated with noritic lithologies and anorthosite. The present study compares the magnetic fabric of the ore body, as deduced from anisotropy of magnetic susceptibility (AMS) measurements, with the crystallographic and shape fabrics, obtained from lattice-preferred orientation (LPO) and shape-preferred orientation (SPO) measurements made using electron backscattered diffraction (EBSD) and 3D image analysis, respectively. Room-temperature hysteresis measurements, thermomagnetic curves and values of the bulk magnetic susceptibility reveal a magnetic mineralogy dominated by a mixed contribution of hemo-ilmenite and magnetite. The hemo-ilmenite grains display a LPO characterized by a strong preferred orientation of the basal (0001) plane of ilmenite along which hematite was exsolved. This LPO and the magnetic fabric fit well (angle between the crystallographic c-axis and the axis of minimum susceptibility ≤ ca. 15° for most samples), and the latter is thus strongly influenced by the hemo-ilmenite magneto-crystalline anisotropy. A magnetite SPO, concordant with the hemo-ilmenite LPO, may also influence and even dominate the magnetic fabric. The rock shape fabric is coaxial with the magnetic fabric that can thus be used to perform detailed structural mapping. Interpretation of the magnetic fabric and field structural data suggests that the Lac Tio ore body would be a sag point at the margin of the Lac Allard anorthosite, deformed by ballooning during the final stage of diapiric emplacement of the anorthosite body.

Microstructure and texture evolution in cold-rolled and annealed alloy MA-956

NASA Astrophysics Data System (ADS)

Hosoda, Takashi

The microstructural and texture development with thermomechanical processing, performed through a combination of cold-rolling and annealing, in MA-956 plate consisting of a layered and inhomogeneous microstructure was systematically assessed. The alloy contained in mass percent, 20 Cr, 4.8 Al, 0.4 Ti, 0.4 Y2O3, and the balance iron. The starting material was as-hot-rolled plate, 9.7 mm thick. The as-hot-rolled plate was subjected to 40%, 60%, and 80% cold-rolling reduction and subsequently annealed at 1000, 1200, or 1380. Assessment of microstructural and texture developments before and after cold-rolling and annealing was performed using light optical microscopy (LOM), Vickers hardness testing, and electron backscatter diffraction (EBSD). Locally introduced misorientations by cold-rolling in each region were evaluated by Kernel Average Misorientation (KAM) maps. The as-hot-rolled condition contained a layered and inhomogeneous microstructure consisting of thin and coarse elongated grains, and aggregated regions which consisted of fine grains and sub-grains with {100} texture parallel to the longitudinal direction. The microstructure of the 40% cold-rolled condition contained deformation bands, and the 60% and 80% cold-rolled conditions also contained highly deformed regions where the deformation bands were intricately tangled. A predominant orientation of (001) parallel to the rolling direction was developed during cold-rolling, becoming more prominent with increasing reduction. The magnitudes of KAM angles varied through the thickness depending on the initial microstructures. Recrystallization occurred in regions where high KAM angles were dense after annealing and nucleation sites were the aggregation regions, deformation bands, and highly deformed regions. The shape and size of the recrystallized grains varied depending on the nucleation sites.

Deciphering the Possible Role of Strain Path on the Evolution of Microstructure, Texture, and Magnetic Properties in a Fe-Cr-Ni Alloy

NASA Astrophysics Data System (ADS)

Kumar, Amit; Khatirkar, Rajesh Kisni; Gupta, Aman; Shekhawat, Satish K.; Suwas, Satyam

2018-06-01

In the present work, the influence of strain path on the evolution of microstructure, crystallographic texture, and magnetic properties of a two-phase Fe-Cr-Ni alloy was investigated. The Fe-Cr-Ni alloy had nearly equal proportion of austenite and ferrite and was cold rolled up to a true strain of 1.6 (thickness reduction) using two different strain paths—unidirectional rolling and multi-step cross rolling. The microstructures were characterized by scanning electron microscopy (SEM) and electron backscattered diffraction (EBSD), while crystallographic textures were determined using X-ray diffraction. For magnetic characterization, B-H loops and M-H curves were measured and magnetic force microscopy was performed. After unidirectional rolling, ferrite showed the presence of strong α-fiber (rolling direction, RD//<110>) and austenite showed strong brass type texture (consisting of Brass (Bs) ({110}<112>), Goss ({110}<001>), and S ({123}<634>)). After multi-step cross rolling, strong rotated cube ({100}<110>) was developed in ferrite, while austenite showed ND (normal direction) rotated brass ( 10 deg) texture. The strain-induced martensite (SIM) was found to be higher in unidirectionally rolled samples than multi-step cross-rolled samples. The coherently diffracting domain size, micro-strain, coercivity, and core loss also showed a strong correlation with strain and strain path. More strain was partitioned into austenite than ferrite during deformation (unidirectional as well as cross rolling). Further, the strain partitioning (in both austenite and ferrite) was found to be higher in unidirectionally rolled samples.

The evolution of the deformation substructure in a Ni-Co-Cr equiatomic solid solution alloy

DOE PAGES

Miao, Jiashi; Slone, C. E.; Smith, T. M.; ...

2017-05-15

The equiatomic NiCoCr alloy exhibits an excellent combination of strength and ductility, even greater than the FeNiCrCoMn high entropy alloy, and also displays a simultaneous increase in strength and ductility with decreasing the testing temperature. To systemically investigate the origin of the exceptional properties of NiCoCr alloy, which are related to the evolution of the deformation substructure with strain, interrupted tensile testing was conducted on the equiatomic NiCoCr single-phase solid solution alloy at both cryogenic and room temperatures at five different plastic strain levels of 1.5%, 6.5%, 29%, 50% and 70%. The evolution of deformation substructure was examined using electronmore » backscatter diffraction (EBSD), transmission Kikuchi diffraction (TKD), conventional transmission electron microscopy (CTEM), diffraction contrast imaging using STEM (DCI-STEM) and atomic resolution scanning transmission electron microscopy. While the deformation substructure mainly consisted of planar dislocation slip and the dissociation of dislocations into stacking faults at small strain levels (≤6.5%), at larger strain levels, additional substructures including nanotwins and a new phase with hexagonal close packed (HCP) lamellae also appeared. The volume fraction of the HCP lamellae increases with increasing deformation, especially at cryogenic temperature. First principles calculations at 0 K indicate that the HCP phase is indeed energetically favorable relative to FCC for this composition. In conclusion, the effects of the nanotwin and HCP lamellar structures on hardening rate and ductility at both cryogenic and room temperature are qualitatively discussed.« less

BHQ revisited (1) - Looking at grain size

NASA Astrophysics Data System (ADS)

Heilbronner, Renée; Kilian, Rüdiger; Tullis, Jan

2016-04-01

Black Hills Quartzite (BHQ) has been used extensively in experimental rock deformation for numerous studies. Coaxial and general shear experiments have been carried out, for example, to define the dislocation creep regimes of quartz (Hirth & Tullis, 1992), to determine the effect of annealing (Heilbronner & Tullis, 2002) or to study the development of texture and microstructure with strain (Heilbronner & Tullis, 2006). BHQ was also used to determine the widely used quartz piezometer by Stipp & Tullis (2003). Among the microstructure analyses that were performed in those original papers, grain size was usually determined using CIP misorientation images. However, the CIP method (= computer-integrated polarization microscopy, details in Heilbronner and Barrett, 2014) is only capable of detecting the c-axis orientation of optically uniaxial materials and hence is only capable of detecting grain boundaries between grains that differ in c-axis orientation. One of the puzzling results we found (Heilbronner & Tullis, 2006) was that the recrystallized grain size seemed to depend on the crystallographic preferred orientation of the domain. In other words the grain size did not only depend on the flow stress but also on the orientation of the c-axis w/r to the shear direction. At the time, no EBSD analysis (electron back scatter diffraction) was carried out and hence the full crystallographic orientation was not known. In principle it is therefore possible that we missed some grain boundaries (between grains with parallel c-axes) and miscalculated our grain sizes. In the context of recent shear experiments on quartz gouge at the brittle-viscous transition (see Richter et al., this conference), where EBSD is used to measure the recrystallized grain size, we wanted to re-measure the CIP grain sizes of our 2006 samples (deformed in regime 1, 2 and 3 of dislocation) in exactly the same way. In two companion posters we use EBSD orientation imaging to repeat, refine and expand the microstructure and texture analysis of Heilbronner & Tullis (2006). Here, in poster (1), we focus on the recrystallized grain size with the aim of (a) comparing CIP- and EBSD derived grain size measurements, (b) of comparing the recrystallized grain size of coaxially deformed and sheared BHQ and (c) in order to confirm that the quartz piezometer indeed depends on texture, and (d) to test if it also depends on the type of deformation (irrotational versus rotational deformation). References cited: Heilbronner, R., and S.D. Barrett (2014) Image Analysis in Earth Sciences, Springer. Heilbronner, R., and J. Tullis (2002), The effect of static annealing on micro- structure and crystallographic preferred orientations of quartzites experimentally deformed in axial compression and shear, Geol. Soc. Spec. Publ., 200, 191 - 218. Heilbronner, R., and J. Tullis (2006), Evolution of c axis pole figures and grain size during dynamic recrystallization: Results from experimentally sheared quartzite. JGR, 111, B10202, doi:10.1029/2005JB004194, 2006 Hirth, G., and J. Tullis (1992), Dislocation creep regimes in quartz aggregates, JSG, 14, 145-159. Stipp, M., and J. Tullis (2003), The recrystallized grain size piezometer for quartz, Geophys. Res. Lett., 30(21), 2088, doi:10.1029/2003GL018444.

Structure-Property Relationships of Solid State Additive Manufactured Aluminum Alloy 2219 and Inconel 625

NASA Astrophysics Data System (ADS)

Rivera Almeyda, Oscar G.

In this investigation, the processing-structure-property relations are correlated for solid state additively manufactured (SSAM) Inconel 625 (IN 625) and a SSAM aluminum alloy 2219 (AA2219). This is the first research of these materials processed by a new SSAM method called additive friction stir (AFS). The AFS process results in a refined grain structure by extruding solid rod through a rotating tool generating heat and severe plastic deformation. In the case of the AFS IN625, the IN625 alloy is known for exhibiting oxidation resistance and temperature mechanical stability, including strength and ductility. This study is the first to investigate the beneficial grain refinement and densification produced by AFS in IN625 that results in advantageous mechanical properties (YS, UTS, epsilonf) at both quasi-static and high strain rate. Electron Backscatter Diffraction (EBSD) observed dynamic recrystallization and grain refinement during the layer deposition in the AFS specimens, where the results identified fine equiaxed grain structures formed by dynamic recrystallization (DRX) with even finer grain structures forming at the layer interfaces. The EBSD quantified grains as fine as 0.27 microns in these interface regions while the average grain size was approximately 1 micron. Additionally, this is the first study to report on the strain rate dependence of AFS IN625 through quasi-static (QS) (0.001/s) and high strain rate (HR) (1500/s) tensile experiments using a servo hydraulic frame and a direct tension-Kolsky bar, respectively, which captured both yield and ultimate tensile strengths increasing as strain rate increased. Fractography performed on specimens showed a ductile fracture surface on both QS, and HR. Alternatively, the other AFS material system investigated in this study, AA2219, is mostly used for aerospace applications, specifically for rocket fuel tanks. EBSD was performed in the cross-section of the AA2219, also exhibiting DRX with equiaxed microstructure in the three directions and an average grain size of 2.5 microns. EBSD PFs showed that the material has a strong torsional fiber A texture in the top of the build, and this texture gets weaker in the middle and bottom sections. TEM showed that there are no theta' precipitates in the as-deposited cross-section, therefore no precipitation strengthening should be expected. Strain rate and stress state dependence was study, and in both tension and compression, with an increase in strain rate, the YS increase and the UTS decreased. Ductile fracture surface was observed on specimens tested to failure in both QS and HR. The AFS AA2219 processing-structure-property relations are being studied in this investigation to address the stress-state and strain rate dependence of AFS AA2219 with an internal sate variable (ISV) plasticity-damage model to capture the different yield stress, work hardening and failure strain in the AFS AA2219 for high fidelity modeling of AFS components. The ISV plasticity model successfully captured the material behavior in tension, compression, tension-followed-by-compression and compression-followed-by-tension experiments. Furthermore, the damage parameters of the model were calibrated using the final void density measured from the fracture surfaces.

Disequilibrium growth of olivine in mafic magmas revealed by phosphorus zoning patterns of olivine from mafic-ultramafic intrusions

NASA Astrophysics Data System (ADS)

Xing, Chang-Ming; Wang, Christina Yan; Tan, Wei

2017-12-01

Olivine from mafic-ultramafic intrusions rarely displays growth zoning in major and some minor elements, such as Fe, Mg and Ni, due to fast diffusion of these elements at high temperatures. These elements in olivine are thus not useful in deciphering magma chamber processes, such as magma convection, multiple injection and mixing. High-resolution X-ray elemental intensity mapping reveals distinct P zoning patterns of olivine from two mafic-ultramafic intrusions in SW China. Polyhedral olivine grains from lherzolite and dunite of the Abulangdang intrusion show P-rich dendrites similar to those observed in volcanic rocks. Rounded olivine grains from net-textured Fe-Ti oxide ores of the Baima layered intrusion have irregular P-rich patches/bands crosscut and interlocked by P-poor olivine domains. P-rich patches/bands contain 250 to 612 ppm P, much higher than P-poor olivine domains with 123 to 230 ppm P. In electron backscattered diffraction (EBSD) maps, P-rich patches/bands within a single olivine grain have the same crystallographic orientation, indicating that they were remnants of the same crystal. Thus, both P-rich patches/bands and P-poor olivine domains in the same grain show a disequilibrium texture and clearly record two-stage growth. The P-rich patches/bands are likely the remnants of a polyhedral olivine crystal that formed in the first stage, whereas the P-poor olivine domains containing rounded Ti-rich magnetite and Fe-rich melt inclusions may have formed from an Fe-rich ambient melt in the second stage. The complex P zoning of olivine can be attributed to the dissolution of early polyhedral olivine and re-precipitation from the Fe-rich ambient melt. The early polyhedral olivine was in chemical disequilibrium with the ambient melt that may have been developed by silicate liquid immiscibility in a crystal mush. Our study implies that olivine crystals in igneous cumulates with an equilibrium appearance may have experienced disequilibrium growth processes during slow cooling. Therefore, the crystallization sequence of mafic magmas based on textural relationships should be treated with caution.

Development of olivine crystallographic preferred orientation in response to strain-induced fabric geometry

NASA Astrophysics Data System (ADS)

Chatzaras, Vasileios; Kruckenberg, Seth C.; Cohen, Shaina M.; Medaris, L. Gordon, Jr.; Withers, Anthony C.; Bagley, Brian

2016-04-01

The effect of finite strain ellipsoid geometry on crystallographic preferred orientation (CPO) is well known for crustal minerals (e.g., quartz, calcite, biotite, and hornblende). In the upper mantle, however, it remains poorly constrained how strain and fabric may affect olivine CPO. We present data from a suite of 40 spinel peridotite xenoliths from Marie Byrd Land (west Antarctica), which support an interpretation that fabric geometry rather than deformation conditions control the development of olivine CPO. We use X-ray computed tomography (XRCT) to quantitatively determine spinel fabric (orientation and geometry). Olivine CPOs, determined by Electron Backscattered Diffraction (EBSD), are plotted with respect to the XRCT-derived spinel foliation and lineation; this approach allows for the accurate, and unbiased, identification of CPO symmetries and types in mantle xenoliths. The combined XRCT and EBSD data show that the xenoliths are characterized by a range of fabric geometries (from oblate to prolate) and olivine CPO patterns; we recognize the A-type, axial-[010], axial-[100], and B-type patterns. The mantle xenoliths equilibrated at temperatures 779-1198 oC, as determined by 2-Px geothermometry. Using a geotherm consistent with the stability of spinel in all xenoliths, the range of equilibration temperatures occurs at depths between 39 and 72 km. Olivine recrystallized grain size piezometry reveals differential stresses ranging 2-60 MPa. Analysis of low-angle misorientation axes show a wide range in the distribution of rotation axes, with dominant {0kl}[100] slip. We use Fourier Transform Infrared (FTIR) spectroscopy to estimate the water content in the xenolith with the B-type CPO pattern. FTIR analysis shows that the equilibrium H concentration in olivine is low (4-13 ppm H2O). Combining these data, we observe that olivine CPO symmetry is controlled neither by the deformation conditions (stress, temperature, pressure, water content) for the range of conditions estimated in the Marie Byrd Land xenoliths, nor by the activation of the slip systems predicted by deformation experiments. Rather, our data show that olivine CPO is controlled by transitions in strain-induced fabric geometry. Microstructures and deformation mechanism maps suggest that deformation is dominated by dislocation-accommodated grain boundary sliding. We propose that slip of olivine glide planes and rotation of olivine grains occur so as to accommodate the imposed material flow, which is guided by the 3D strain-induced fabric geometry. As a result of this process, the axial-[010] and B-type patterns form in relation to oblate fabric ellipsoids, the A-type pattern forms in a range of fabric ellipsoids, and the axial-[100] pattern is associated with prolate fabric ellipsoids. We therefore suggest that the well-known process of strain geometry-induced development of CPO is also applicable to upper mantle rocks.

Comprehensive analysis of TEM methods for LiFePO4/FePO4 phase mapping: spectroscopic techniques (EFTEM, STEM-EELS) and STEM diffraction techniques (ACOM-TEM).

PubMed

Mu, X; Kobler, A; Wang, D; Chakravadhanula, V S K; Schlabach, S; Szabó, D V; Norby, P; Kübel, C

2016-11-01

Transmission electron microscopy (TEM) has been used intensively in investigating battery materials, e.g. to obtain phase maps of partially (dis)charged (lithium) iron phosphate (LFP/FP), which is one of the most promising cathode material for next generation lithium ion (Li-ion) batteries. Due to the weak interaction between Li atoms and fast electrons, mapping of the Li distribution is not straightforward. In this work, we revisited the issue of TEM measurements of Li distribution maps for LFP/FP. Different TEM techniques, including spectroscopic techniques (energy filtered (EF)TEM in the energy range from low-loss to core-loss) and a STEM diffraction technique (automated crystal orientation mapping (ACOM)), were applied to map the lithiation of the same location in the same sample. This enabled a direct comparison of the results. The maps obtained by all methods showed excellent agreement with each other. Because of the strong difference in the imaging mechanisms, it proves the reliability of both the spectroscopic and STEM diffraction phase mapping. A comprehensive comparison of all methods is given in terms of information content, dose level, acquisition time and signal quality. The latter three are crucial for the design of in-situ experiments with beam sensitive Li-ion battery materials. Furthermore, we demonstrated the power of STEM diffraction (ACOM-STEM) providing additional crystallographic information, which can be analyzed to gain a deeper understanding of the LFP/FP interface properties such as statistical information on phase boundary orientation and misorientation between domains. Copyright © 2016 Elsevier B.V. All rights reserved.

Dynamic spatial filtering using a digital micromirror device for high-speed optical diffraction tomography.

PubMed

Jin, Di; Zhou, Renjie; Yaqoob, Zahid; So, Peter T C

2018-01-08

Optical diffraction tomography (ODT) is an emerging microscopy technique for three-dimensional (3D) refractive index (RI) mapping of transparent specimens. Recently, the digital micromirror device (DMD) based scheme for angle-controlled plane wave illumination has been proposed to improve the imaging speed and stability of ODT. However, undesired diffraction noise always exists in the reported DMD-based illumination scheme, which leads to a limited contrast ratio of the measurement fringe and hence inaccurate RI mapping. Here we present a novel spatial filtering method, based on a second DMD, to dynamically remove the diffraction noise. The reported results illustrate significantly enhanced image quality of the obtained interferograms and the subsequently derived phase maps. And moreover, with this method, we demonstrate mapping of 3D RI distribution of polystyrene beads as well as biological cells with high accuracy. Importantly, with the proper hardware configuration, our method does not compromise the 3D imaging speed advantage promised by the DMD-based illumination scheme. Specifically, we have been able to successfully obtain interferograms at over 1 kHz speed, which is critical for potential high-throughput label-free 3D image cytometry applications.

Microstructural Analysis of Ti-6Al-4V Components Made by Electron Beam Additive Manufacturing

NASA Astrophysics Data System (ADS)

Coleman, Rashadd L.

Electron Beam Additive Manufacturing (EBAM) is a relatively new additive manufacturing (AM) technology that uses a high-energy electron beam to melt and fuse powders to build full-density parts in a layer by layer fashion. EBAM can fabricate metallic components, particularly, of complex shapes, in an efficient and cost-effective manner compared to conventional manufacturing means. EBAM is an enabling technology for rapid manufacturing (RM) of metallic components, and thus, can efficiently integrate the design and manufacturing of aerospace components. However, EBAM for aerospace-related applications remain limited because the effect of the EBAM process on part characteristics is not fully understood. In this study, various techniques including microhardness, optical microscopy (OM), X-ray diffraction (XRD), Scanning Electron Microscopy (SEM), and electron backscatter diffraction (EBSD) were used to characterize Ti-6Al-4V components processed using EBAM. The results were compared to Ti-6Al-4V components processed using conventional techniques. In this study it is shown that EBAM built Ti-64 components have increased hardness, elastic modulus, and yield strength compared to wrought Ti-6Al-4V. Further, it is also shown in this study that the horizontal build EBAM Ti-6Al-4V has increased hardness, elastic modulus, and yield strength compared to vertical build EBAM due to a preferential growth of the beta phase.

SEM and TEM characterization of microstructure of stainless steel composites reinforced with TiB{sub 2}

DOE Office of Scientific and Technical Information (OSTI.GOV)

Sulima, Iwona, E-mail: isulima@up.krakow.pl

Steel-8TiB{sub 2} composites were produced by two new sintering techniques, i.e. Spark Plasma Sintering (SPS) and High Pressure-High Temperature (HP-HT) sintering. This study discusses the impact of these sintering methods on the microstructure of steel composites reinforced with TiB{sub 2} particles. Scanning electron microscopy (SEM), wavelength dispersive spectroscopy (WDS), X-ray diffraction, electron backscatter diffraction (EBSD) and transmission electron microscopy (TEM) were used to analyze the microstructure evolution in steel matrix composites. The results of microscopic examinations revealed a close relationship between the composite microstructure and the methods and conditions of sintering. Substantial differences were observed in the grain size ofmore » materials sintered by HP-HT and SPS. It has been demonstrated that the composites sintered by HP-HT tend to form a chromium-iron-nickel phase in the steel matrix. In contrast, the microstructure of the composites sintered by SPS is characterized by the presence of complex borides and chromium-iron phase. - Highlights: •The steel-8TiB{sub 2} composites were fabricated by Spark Plasma Sintering (SPS) and High Pressure-High Temperature (HP-HT). •Sintering techniques has an important effect on changes in the microstructure of steel-8TiB{sub 2} composites. •New phases of different size and morphology were identified.« less

Crystallisation of Ba1-xSrxZn2Si2O7 from BaO/SrO/ZnO/SiO2 glass with different ZrO2 and TiO2 concentrations

NASA Astrophysics Data System (ADS)

Vladislavova, Liliya; Kracker, Michael; Zscheckel, Tilman; Thieme, Christian; Rüssel, Christian

2018-04-01

The effect of different nucleation agents such as ZrO2 and TiO2 was investigated for a first time with respect to their crystallisation behaviour in the glass system BaO-SrO-ZnO-SiO2. In all studied glasses, a Ba1-xSrxZn2Si2O7 (0.1 ≤ x ≤ 0.9) solid solution crystallized. This phase was first described in 2015 to possess a similar structure as the high temperature phase of BaZn2Si2O7 and a thermal expansion close to zero or even negative. It may find applications e.g. as cook panels, telescope mirrors, and furnace windows. Kinetic parameters of the crystallisation process were determined by supplying different heating rates in a differential scanning calorimeter (DSC). The results were evaluated using the equations of Ozawa and Kissinger with respect to the activation energies. Furthermore, the Ozawa method was used for the determination of Avrami parameters, which provides further information on the nucleation and crystallisation processes. Scanning electron microscopy including electron backscatter diffraction (EBSD) was used to characterise the microstructure, to determine the crystallite size and the crystal orientation. For the characterisation of the occurring crystalline phases, X-ray diffraction was used.

DOE Office of Scientific and Technical Information (OSTI.GOV)

Liu, Jiyuan; Zhang, Zicheng, E-mail: zhangzicheng2004@126.com; Manabe, Ken-ichi

Transformation-induced plasticity aided seamless steel tube comprising of ferrite, bainite, and metastable austenite was processed through forging, piercing, cold-drawing, and two-stage heat treatment. T-shape hydroforming is a classic forming method for experimental research and practical production. The current work studied austenite-to-martensite transformation and microcrack initiation and propagation of the tube during T-shape hydroforming using electron backscattering diffraction, scanning electron microscopy, and transmission electron microscopy. The strain distribution in the bcc-phase and fcc-phase was studied by evaluating changes in the average local misorientation. Compared to the compressive stress, metastable austenite with similar strain surrounding or inside the grains transformed easier undermore » tensile loading conditions. The inclusions were responsible for microcrack initiation. The propagation of the cracks is hindered by martensite/austenite constituent due to transformation induced plasticity effect. The volume fraction of untransformed retained austenite decreased with increase in strain implying transformation-induced plasticity effect. - Highlights: • Hydroformed tubes processed via TRIP concept • EBSD provided estimate of micro local strain. • Retained austenite hinders propagation of microcracks.« less

Study of the influence of the parameters of an experiment on the simulation of pole figures of polycrystalline materials using electron microscopy

DOE Office of Scientific and Technical Information (OSTI.GOV)

Antonova, A. O., E-mail: aoantonova@mail.ru; Savyolova, T. I.

2016-05-15

A two-dimensional mathematical model of a polycrystalline sample and an experiment on electron backscattering diffraction (EBSD) is considered. The measurement parameters are taken to be the scanning step and threshold grain-boundary angle. Discrete pole figures for materials with hexagonal symmetry have been calculated based on the results of the model experiment. Discrete and smoothed (by the kernel method) pole figures of the model sample and the samples in the model experiment are compared using homogeneity criterion χ{sup 2}, an estimate of the pole figure maximum and its coordinate, a deviation of the pole figures of the model in the experimentmore » from the sample in the space of L{sub 1} measurable functions, and the RP-criterion for estimating the pole figure errors. Is is shown that the problem of calculating pole figures is ill-posed and their determination with respect to measurement parameters is not reliable.« less

Evaluation of consolidation method on mechanical and structural properties of ODS RAF steel

NASA Astrophysics Data System (ADS)

Frelek-Kozak, M.; Kurpaska, L.; Wyszkowska, E.; Jagielski, J.; Jozwik, I.; Chmielewski, M.

2018-07-01

In the present work, the effects of the fabrication method on mechanical and structural properties of 12%Cr, 2%W, 0.25%Ti, 0.25%Y2O3 steels were investigated. Materials obtained by Spark Plasma Sintering (SPS), Hot Isostatic Pressing (HIP) and Hot Extrusion (HE) methods were studied. The microstructure was characterized by using Scanning Electron Microscopy (SEM) and Electron Backscatter Diffraction analysis (EBSD). Mechanical properties of the studied samples were evaluated by using Vickers micro hardness HV0.1, Small Punch Test (SPT) and nanoindentation (NI) methods. The analysis revealed that samples manufactured via HIP and SPS processes exhibit very similar properties, whereas SPS method produces material with slightly lower hardness. In addition, significantly lower mechanical properties of the specimens after HE process were observed. The study described in this article addresses also the problems of mechanical parameters measured in micro- and nano-scale experiments and aims to identify possible pitfalls related to the use of various manufacturing technologies.

Characterization of phase properties and deformation in ferritic-austenitic duplex stainless steels by nanoindentation and finite element method

DOE PAGES

Schwarm, Samuel C.; Kolli, R. Prakash; Aydogan, Eda; ...

2016-11-03

The phase properties and deformation behavior of the δ–ferrite and γ–austenite phases of CF–3 and CF–8 cast duplex stainless steels were characterized by nanoindentation and microstructure-based finite element method (FEM) models. We evaluated the elastic modulus of each phase and the results indicate that the mean elastic modulus of the δ–ferrite phase is greater than that of the γ–austenite phase, and the mean nanoindentation hardness values of each phase are approximately the same. Furthermore, the elastic FEM model results illustrate that greater von Mises stresses are located within the δ–ferrite phase, while greater von Mises strains are located in themore » γ–austenite phase in response to elastic deformation. The elastic moduli calculated by FEM agree closely with those measured by tensile testing. Finally, the plastically deformed specimens exhibit an increase in misorientation, deformed grains, and subgrain structure formation as measured by electron backscatter diffraction (EBSD).« less

Characterization of phase properties and deformation in ferritic-austenitic duplex stainless steels by nanoindentation and finite element method

DOE Office of Scientific and Technical Information (OSTI.GOV)

Schwarm, Samuel C.; Kolli, R. Prakash; Aydogan, Eda

The phase properties and deformation behavior of the δ–ferrite and γ–austenite phases of CF–3 and CF–8 cast duplex stainless steels were characterized by nanoindentation and microstructure-based finite element method (FEM) models. We evaluated the elastic modulus of each phase and the results indicate that the mean elastic modulus of the δ–ferrite phase is greater than that of the γ–austenite phase, and the mean nanoindentation hardness values of each phase are approximately the same. Furthermore, the elastic FEM model results illustrate that greater von Mises stresses are located within the δ–ferrite phase, while greater von Mises strains are located in themore » γ–austenite phase in response to elastic deformation. The elastic moduli calculated by FEM agree closely with those measured by tensile testing. Finally, the plastically deformed specimens exhibit an increase in misorientation, deformed grains, and subgrain structure formation as measured by electron backscatter diffraction (EBSD).« less

Effects of Zr Addition on Strengthening Mechanisms of Al-Alloyed High-Cr ODS Steels.

PubMed

Ren, Jian; Yu, Liming; Liu, Yongchang; Liu, Chenxi; Li, Huijun; Wu, Jiefeng

2018-01-12

Oxide dispersion strengthened (ODS) steels with different contents of zirconium (denoted as 16Cr ODS, 16Cr-0.3Zr ODS and 16Cr-0.6Zr ODS) were fabricated to investigate the effects of Zr on strengthening mechanism of Al-alloyed 16Cr ODS steel. Electron backscatter diffraction (EBSD) results show that the mean grain size of ODS steels could be decreased by Zr addition. Transmission electron microscope (TEM) results indicate that Zr addition could increase the number density but decrease the mean diameter and inter-particle spacing of oxide particles. Furthermore, it is also found that in addition to Y-Al-O nanoparticles, Y-Zr-O oxides with finer size were observed in 16Cr-0.3Zr ODS and 16Cr-0.6Zr ODS steels. These changes in microstructure significantly increase the yield strength (YS) and ultimate tensile strength (UTS) of ODS steels through mechanisms of grain boundary strengthening and dispersion strengthening.

Effects of Zr Addition on Strengthening Mechanisms of Al-Alloyed High-Cr ODS Steels

PubMed Central

Ren, Jian; Yu, Liming; Liu, Yongchang; Liu, Chenxi; Li, Huijun; Wu, Jiefeng

2018-01-01

Oxide dispersion strengthened (ODS) steels with different contents of zirconium (denoted as 16Cr ODS, 16Cr-0.3Zr ODS and 16Cr-0.6Zr ODS) were fabricated to investigate the effects of Zr on strengthening mechanism of Al-alloyed 16Cr ODS steel. Electron backscatter diffraction (EBSD) results show that the mean grain size of ODS steels could be decreased by Zr addition. Transmission electron microscope (TEM) results indicate that Zr addition could increase the number density but decrease the mean diameter and inter-particle spacing of oxide particles. Furthermore, it is also found that in addition to Y-Al-O nanoparticles, Y-Zr-O oxides with finer size were observed in 16Cr-0.3Zr ODS and 16Cr-0.6Zr ODS steels. These changes in microstructure significantly increase the yield strength (YS) and ultimate tensile strength (UTS) of ODS steels through mechanisms of grain boundary strengthening and dispersion strengthening. PMID:29329260

Individual analysis of inter and intragrain defects in electrically characterized polycrystalline silicon nanowire TFTs by multicomponent dark-field imaging based on nanobeam electron diffraction two-dimensional mapping

NASA Astrophysics Data System (ADS)

Asano, Takanori; Takaishi, Riichiro; Oda, Minoru; Sakuma, Kiwamu; Saitoh, Masumi; Tanaka, Hiroki

2018-04-01

We visualize the grain structures for individual nanosized thin film transistors (TFTs), which are electrically characterized, with an improved data processing technique for the dark-field image reconstruction of nanobeam electron diffraction maps. Our individual crystal analysis gives the one-to-one correspondence of TFTs with different grain boundary structures, such as random and coherent boundaries, to the characteristic degradations of ON-current and threshold voltage. Furthermore, the local crystalline uniformity inside a single grain is detected as the difference in diffraction intensity distribution.

DOE Office of Scientific and Technical Information (OSTI.GOV)

Kantor, M. M., E-mail: Kantor@imet.ac.ru; Vorkachev, K. G., E-mail: KGV@imet.ac.ru

The efficiency of different techniques application for the investigation of orientation inhomogeneities in polycrystalline materials was studied using FEG SEM-FIB dual beam station equipped with EBSD. It is shown that for the visualization of pearlitic ferrite fragments it is more appropriate to acquire the images in secondary electrons induced by Ga ions. At the same time for the visualization of nano-sized particles it is more prospective to use images in forward scatter electrons in combination with IQ maps. It is established that pearlitic ferrite fragments are not flat. Complicated spatial configuration of orientation inhomogeneities in pearlitic ferrite is shown bymore » means of 3-d reconstruction. The features of ferrites aggregation are revealed depending on pearlitic ferrite fragmentation criterion. The existence of long-range misorientations in the aggregation area of proeutectoid and pearlitic ferrites is shown.« less

Using in-situ diffraction, elastic plastic self-consistent models and microstructural analysis to interpret the low strain behavior of olivine polycrystals in the D-DIA apparatus

NASA Astrophysics Data System (ADS)

Burnley, P. C.; Kaboli, S.

2016-12-01

The textbook stress strain curve has an elastic response followed by a yield point and then plastic flow. Typically in rock deformation experiments the observed `elastic' behavior deviates from the Young's modulus because the mechanical response of the loading frame and friction in the sample assembly and between moving parts of the loading frame cannot be easily corrected for. Stress strain curves generated in a D-DIA apparatus used in conjunction with synchrotron x-rays should not have these problems because the sample length is measured directly by radiography and the stress in the sample is measured from the sample itself by x-ray diffraction. However, the sample's `elastic behavior', in many instances, still deviates from what is expected. For example, in constant strain rate experiments on both polycrystalline San Carlos olivine and fayalite olivine conducted at a variety of temperatures (25 - 1200 C) and pressures (4 and 7 GPa) although we are able to use elastic plastic self-consistent (EPSC) models to describe the plastic behavior of the olivine we are not able to fit the initial elastic behavior for all but the lowest temperature experiments. To a first approximation it appears that samples are generally more compliant than their elastic properties would predict and that the degree of softening is temperature dependent. For D-DIA experiments which have been conducted at strain rates of 10-5 /sec, there are not enough data points to really clarify what is happening in the elastic portion of the experiment. Therefore, we conducted a suite of low strain experiments at 5 x 10-6/sec at temperatures ranging from 400 C to 1200 C. For each experiment we fit the diffraction data using EPSC models. We will present the results from our diffraction analysis as well as detailed microstructural analysis of the experimental samples using electron backscatter diffraction (EBSD) and electron channeling contrast imaging (ECCI). The relative degree of relaxation observed for each grain population in the diffraction data as well as to the predictions of the EPSC model combined with the microstructural data, will be used create a more comprehensive picture of how individual grains and various grain populations contribute to the low strain mechanical behavior of the polycrystal.

Diffraction gratings used as identifying markers

DOEpatents

Deason, V.A.; Ward, M.B.

1991-03-26

A finely detailed diffraction grating is applied to an object as an identifier or tag which is unambiguous, difficult to duplicate, or remove and transfer to another item, and can be read and compared with prior readings with relative ease. The exact pattern of the diffraction grating is mapped by diffraction moire techniques and recorded for comparison with future readings of the same grating. 7 figures.

DOE Office of Scientific and Technical Information (OSTI.GOV)

Macente, A.; Fusseis, F.; Menegon, L.

Reaction and deformation microfabrics provide key information to understand the thermodynamic and kinetic controls of tectono-metamorphic processes, however they are usually analysed in two dimensions, omitting important information regarding the third spatial dimension. We applied synchrotron-based X-ray microtomography to document the evolution of a pristine olivine gabbro into a deformed omphacite-garnet eclogite in four dimensions, where the 4th dimension is represented by the degree of strain. In the investigated samples, which cover a strain gradient into a shear zone from the Western Gneiss Region (Norway), we focused on the spatial transformation of garnet coronas into elongated clusters of garnets withmore » increasing strain. Our microtomographic data allowed quantification of garnet volume, shape and spatial arrangement evolution with increasing strain. We combined microtomographic observations with light microscope- and backscatter electron images as well as electron microprobe- (EMPA) and electron backscatter diffraction (EBSD) analysis to correlate mineral composition and orientation data with the X-ray absorption signal of the same mineral grains. With increasing deformation, the garnet volume almost triples. In the low strain domain, garnets form a well interconnected large garnet aggregate that develops throughout the entire Page 1 of 52 sample. We also observed that garnet coronas in the gabbros never completely encapsulate olivine grains. In the most highly deformed eclogites, the oblate shapes of garnet clusters reflect a deformational origin of the microfabrics. We interpret the aligned garnet aggregates to direct synkinematic fluid flow and consequently influence the transport of dissolved chemical components. EBSD analyses reveal that garnet show a near-random crystal preferred orientation that testifies no evidence for crystal plasticity. There is, however evidence for minor fracturing, neo-nucleation and overgrowth. Microprobe chemical analysis revealed that garnet compositions progressively equilibrate to eclogite facies, becoming more almandine-rich. We interpret these observations as pointing to a mechanical disintegration of the garnet coronas during strain localisation, and their rearrangement into individual garnet clusters through a combination of garnet coalescence and overgrowth while the rock was deforming.« less

High-Temperature Microindentation Tests on Olivine and Clinopyroxene

NASA Astrophysics Data System (ADS)

Dorner, D.; Schellewald, M.; Stöckhert, B.

2001-12-01

The perspectives of microindentation techniques for the investigation of the mechanical behaviour of minerals at high temperatures are explored. The technique offers the following advantages: (1) natural specimens with small grain size can be used, (2) preparation is simple, (3) a reasonable number of experiments can be performed within a short period of time. The strength of single crystals as a function of orientation and the activated glide systems are studied using scanning electron microscopy (SEM) combined with electron backscatter diffraction (EBSD) facilities. Furthermore, the effects of compositional variations on the flow strength of solid solutions are explored. The indentation hardness tests are performed on selected grains within natural polycrystalline aggregates. The surface of the specimen is polished mechanically and chemically. The orientation of the crystals is determined using EBSD. The indentation tests are performed with a diamond pyramid (Vickers indenter) at temperatures of 25 ° C to 900 ° C. Loading is done with a constant displacement rate up to a force of 0.5 N, followed by a creep period of 10 s at constant load. SEM is used to measure the size of the indents and to examine their morphology in detail. The microhardness obtained for olivine depends on crystal and indenter orientation and decreases slightly with temperature. Slip steps are observed on the surface around the indents. Their orientation with respect to the crystal orientation indicates that the predominant glide system activated in the indentation process is \\{110\\}[001]. The Schmid factors for this glide system correlate with the observed orientation dependence of the hardness. Indentation hardness of clinopyroxene solid solutions depends on composition with jadeite being stronger than diopside. This is inverse to what is expected for dislocation creep. The high yield stresses inferred from the hardness data and the weak dependence of hardness on temperature are consistent with plasticity being the deformation regime explored in indentation hardness tests.

Origin and timing of Dauphiné twins in quartz cement in fractured sandstones from diagenetic environments: Insight from fluid inclusions

NASA Astrophysics Data System (ADS)

Fall, András; Ukar, Estibalitz; Laubach, Stephen E.

2016-09-01

Electron backscattered diffraction techniques (EBSD) show that Dauphiné twins in quartz are widespread in many tectonometamorphic environments. Our study documents that under diagenetic temperatures (< 200 °C) and burial depths < 5 km Dauphiné twins are common in isolated fracture quartz deposits spanning between fracture walls (i.e., quartz bridges) in low-porosity quartz-cemented sandstones. Using examples from East Texas and Colorado cores, we show that twins are associated with crack-seal microstructure and fluid inclusions. Fracture wall-parallel and wall-normal inclusion trails contain coexisting aqueous and hydrocarbon gas inclusions, so homogenization temperatures of aqueous inclusions record true trapping temperatures. Inclusions in alignments normal to fracture walls are large and irregularly shaped compared to those aligned parallel to walls, but both show similar liquid-to-vapor ratios. Stacking transmitted light images with scanning electron microscope cathodoluminescence (SEM-CL) and EBSD images demonstrates that Dauphiné twin boundaries are localized along wall-normal inclusion trails. Trapping temperatures for wall-normal inclusion trails are usually higher than those aligned parallel to the fracture wall. Wall-normal fluid inclusion assemblage temperatures typically match the highest temperatures of wall-parallel assemblages trapped during sequential widening, but not necessarily the most recent. In context of burial histories for these samples, this temperature pattern implies that wall-normal assemblages form at discrete times during or after crack-seal fracture widening. Localization in isolated, potentially high-stress quartz deposits in fractures is compatible with a mechanical origin for these Dauphiné twins. Punctuated temperature values and discrepant sizes and shapes of inclusions in wall-normal trails implies that twinning is a by-product of the formation of the wall-normal inclusion assemblages. The association of Dauphiné twins and fluid inclusion assemblages from which temperature and possibly timing can be inferred provides a way to research timing as well as magnitude of paleostress in some diagenetic settings.

Orientation and phase mapping in the transmission electron microscope using precession-assisted diffraction spot recognition: state-of-the-art results.

PubMed

Viladot, D; Véron, M; Gemmi, M; Peiró, F; Portillo, J; Estradé, S; Mendoza, J; Llorca-Isern, N; Nicolopoulos, S

2013-10-01

A recently developed technique based on the transmission electron microscope, which makes use of electron beam precession together with spot diffraction pattern recognition now offers the possibility to acquire reliable orientation/phase maps with a spatial resolution down to 2 nm on a field emission gun transmission electron microscope. The technique may be described as precession-assisted crystal orientation mapping in the transmission electron microscope, precession-assisted crystal orientation mapping technique-transmission electron microscope, also known by its product name, ASTAR, and consists in scanning the precessed electron beam in nanoprobe mode over the specimen area, thus producing a collection of precession electron diffraction spot patterns, to be thereafter indexed automatically through template matching. We present a review on several application examples relative to the characterization of microstructure/microtexture of nanocrystalline metals, ceramics, nanoparticles, minerals and organics. The strengths and limitations of the technique are also discussed using several application examples. ©2013 The Authors. Journal of Microscopy published by John Wiley & Sons Ltd on behalf of Royal Microscopical Society.

Ultrafast molecular processes mapped by femtosecond x-ray diffraction

NASA Astrophysics Data System (ADS)

Elsaesser, Thomas

2012-02-01

X-ray diffraction with a femtosecond time resolution allows for mapping photoinduced structural dynamics on the length scale of a chemical bond and in the time domain of atomic and molecular motion. In a pump-probe approach, a femtosecond excitation pulse induces structural changes which are probed by diffracting a femtosecond hard x-ray pulse from the excited sample. The transient angular positions and intensities of diffraction peaks give insight into the momentary atomic or molecular positions and into the distribution of electronic charge density. The simultaneous measurement of changes on different diffraction peaks is essential for determining atom positions and charge density maps with high accuracy. Recent progress in the generation of ultrashort hard x-ray pulses (Cu Kα, wavelength λ=0.154 nm) in laser-driven plasma sources has led to the implementation of the powder diffraction and the rotating crystal method with a time resolution of 100 fs. In this contribution, we report new results from powder diffraction studies of molecular materials. A first series of experiments gives evidence of a so far unknown concerted transfer of electrons and protons in ammonium sulfate [(NH4)2SO4], a centrosymmetric structure. Charge transfer from the sulfate groups results in the sub-100 fs generation of a confined electron channel along the c-axis of the unit cell which is stabilized by transferring protons from the adjacent ammonium groups into the channel. Time-dependent charge density maps display a periodic modulation of the channel's charge density by low-frequency lattice motions with a concerted electron and proton motion between the channel and the initial proton binding site. A second study addresses atomic rearrangements and charge dislocations in the non-centrosymmetric potassium dihydrogen phosphate [KH2PO4, KDP]. Photoexcitation generates coherent low-frequency motions along the LO and TO phonon coordinates, leaving the average atomic positions unchanged. The time-dependent maps of electron density demonstrate a concomitant oscillatory relocation of electronic charge with a spatial amplitude of the order of a chemical bond length, two orders of magnitude larger than the vibrational amplitudes. The coherent phonon motions drive the charge relocation, similar to a soft mode driven phase transition between the ferro- and paraelectric phase of KDP.

Tomographic diffractive microscopy with a wavefront sensor.

PubMed

Ruan, Y; Bon, P; Mudry, E; Maire, G; Chaumet, P C; Giovannini, H; Belkebir, K; Talneau, A; Wattellier, B; Monneret, S; Sentenac, A

2012-05-15

Tomographic diffractive microscopy is a recent imaging technique that reconstructs quantitatively the three-dimensional permittivity map of a sample with a resolution better than that of conventional wide-field microscopy. Its main drawbacks lie in the complexity of the setup and in the slowness of the image recording as both the amplitude and the phase of the field scattered by the sample need to be measured for hundreds of successive illumination angles. In this Letter, we show that, using a wavefront sensor, tomographic diffractive microscopy can be implemented easily on a conventional microscope. Moreover, the number of illuminations can be dramatically decreased if a constrained reconstruction algorithm is used to recover the sample map of permittivity.

Color image cryptosystem using Fresnel diffraction and phase modulation in an expanded fractional Fourier transform domain

NASA Astrophysics Data System (ADS)

Chen, Hang; Liu, Zhengjun; Chen, Qi; Blondel, Walter; Varis, Pierre

2018-05-01

In this letter, what we believe is a new technique for optical color image encryption by using Fresnel diffraction and a phase modulation in an extended fractional Fourier transform domain is proposed. Different from the RGB component separation based method, the color image is converted into one component by improved Chirikov mapping. The encryption system is addressed with Fresnel diffraction and phase modulation. A pair of lenses is placed into the fractional Fourier transform system for the modulation of beam propagation. The structure parameters of the optical system and parameters in Chirikov mapping serve as extra keys. Some numerical simulations are given to test the validity of the proposed cryptosystem.

Effects of processing history on the evolution of surface damage layer and dislocation substructure in large grain niobium cavities

DOE PAGES

Kang, D.; Bieler, T. R.; Compton, C.

2015-12-16

Large grain niobium (Nb) is being investigated for fabricating superconducting radiofrequency cavities as an alternative to the traditional approach using fine grain polycrystalline Nb sheets. Past studies have identified a surface damage layer on fine grain cavities due to deep drawing and demonstrated the necessity for chemical etching on the surface. However, the origin of and depth of the damage layer are not well understood, and similar exploration on large grain cavities is lacking. In this work, electron backscatter diffraction (EBSD) was used to examine the cross sections at the equator and iris of a half cell deep drawn frommore » a large grain Nb ingot slice. The results indicate that the damage (identified by a high density of geometrically necessary dislocations) depends on crystal orientations, is different at the equator and iris, and is present through the full thickness of a half cell in some places. After electron backscatter diffraction, the specimens were heat treated at 800 °C or 1000 °C for two hours, and the same areas were reexamined. A more dramatic decrease in dislocation content was observed at the iris than the equator, where some regions exhibited no change. The specimens were then etched and examined again, to determine if the subsurface region behaved differently than the surface. As a result, little change in the dislocation substructure was observed, suggesting that the large grain microstructure is retained with a normal furnace anneal.« less

Non-destructive detection of cross-sectional strain and defect structure in an individual Ag five-fold twinned nanowire by 3D electron diffraction mapping.

PubMed

Fu, Xin; Yuan, Jun

2017-07-24

Coherent x-ray diffraction investigations on Ag five-fold twinned nanowires (FTNWs) have drawn controversial conclusions concerning whether the intrinsic 7.35° angular gap could be compensated homogeneously through phase transformation or inhomogeneously by forming disclination strain field. In those studies, the x-ray techniques only provided an ensemble average of the structural information from all the Ag nanowires. Here, using three-dimensional (3D) electron diffraction mapping approach, we non-destructively explore the cross-sectional strain and the related strain-relief defect structures of an individual Ag FTNW with diameter about 30 nm. The quantitative analysis of the fine structure of intensity distribution combining with kinematic electron diffraction simulation confirms that for such a Ag FTNW, the intrinsic 7.35° angular deficiency results in an inhomogeneous strain field within each single crystalline segment consistent with the disclination model of stress-relief. Moreover, the five crystalline segments are found to be strained differently. Modeling analysis in combination with system energy calculation further indicates that the elastic strain energy within some crystalline segments, could be partially relieved by the creation of stacking fault layers near the twin boundaries. Our study demonstrates that 3D electron diffraction mapping is a powerful tool for the cross-sectional strain analysis of complex 1D nanostructures.

Material characterization using ultrasound tomography

NASA Astrophysics Data System (ADS)

Falardeau, Timothe; Belanger, Pierre

2018-04-01

Characterization of material properties can be performed using a wide array of methods e.g. X-ray diffraction or tensile testing. Each method leads to a limited set of material properties. This paper is interested in using ultrasound tomography to map speed of sound inside a material sample. The velocity inside the sample is directly related to its elastic properties. Recent develop-ments in ultrasound diffraction tomography have enabled velocity mapping of high velocity contrast objects using a combination of bent-ray time-of-flight tomography and diffraction tomography. In this study, ultrasound diffraction tomography was investigated using simulations in human bone phantoms. A finite element model was developed to assess the influence of the frequency, the number of transduction positions and the distance from the sample as well as to adapt the imaging algorithm. The average velocity in both regions of the bone phantoms were within 5% of the true value.

Risk and benefit of diffraction in Energy Dispersive X-ray fluorescence mapping

NASA Astrophysics Data System (ADS)

Nikonow, Wilhelm; Rammlmair, Dieter

2016-11-01

Energy dispersive X-ray fluorescence mapping (μ-EDXRF) is a fast and non-destructive method for chemical quantification and therefore used in many scientific fields. The combination of spatial and chemical information is highly valuable for understanding geological processes. Problems occur with crystalline samples due to diffraction, which appears according to Bragg's law, depending on the energy of the X-ray beam, the incident angle and the crystal parameters. In the spectra these peaks can overlap with element peaks suggesting higher element concentrations. The aim of this study is to investigate the effect of diffraction, the possibility of diffraction removal and potential geoscientific applications for X-ray mapping. In this work the μ-EDXRF M4 Tornado from Bruker was operated with a Rh-tube and polychromatic beam with two SDD detectors mounted each at ± 90° to the tube. Due to the polychromatic beam the Bragg condition fits for several mineral lattice planes. Since diffraction depends on the angle, it is shown that a novel correction approach can be applied by measuring from two different angles and calculating the minimum spectrum of both detectors gaining a better limit of quantification for this method. Furthermore, it is possible to use the diffraction information for separation of differently oriented crystallites within a monomineralic aggregate and obtain parameters like particle size distribution for the sample, as it is done by thin section image analysis in cross-polarized light. Only with μ-EDXRF this can be made on larger samples without preparation of thin sections.

X-Ray Diffraction Wafer Mapping Method for Rhombohedral Super-Hetero-Epitaxy

NASA Technical Reports Server (NTRS)

Park, Yoonjoon; Choi, Sang Hyouk; King, Glen C.; Elliott, James R.; Dimarcantonio, Albert L.

2010-01-01

A new X-ray diffraction (XRD) method is provided to acquire XY mapping of the distribution of single crystals, poly-crystals, and twin defects across an entire wafer of rhombohedral super-hetero-epitaxial semiconductor material. In one embodiment, the method is performed with a point or line X-ray source with an X-ray incidence angle approximating a normal angle close to 90 deg, and in which the beam mask is preferably replaced with a crossed slit. While the wafer moves in the X and Y direction, a narrowly defined X-ray source illuminates the sample and the diffracted X-ray beam is monitored by the detector at a predefined angle. Preferably, the untilted, asymmetric scans are of {440} peaks, for twin defect characterization.

Formation of wadsleyite in a shock experiment - implications for the duration of shock events in meteorite parent bodies

NASA Astrophysics Data System (ADS)

Tschauner, O.; Asimow, P. D.; Ahrens, T. J.; Kostandova, N.; Sinogeikin, S.

2007-12-01

We report the first observation of the high-pressure silicate phase wadsleyite in the recovery products of a shock experiment. Wadsleyite was detected by micro-X ray diffraction and EBSD. Wadsleyite grew from melt which formed by chemical reaction of periclase and silica during shock. Our findings show that the growth rate of high pressure silicate phases in shock-generated melts can be of the order of m/s and is probably not diffusion controlled. Our finding has important implications for the time scale of shock events recorded by meteorites and indicates that the presence of high pressure silicates found in shocked meteorites does not necessarily imply large impactor sizes. This work was supported by the NNSA Cooperative Agreement DOE-FC88-01NV14049 and NASA/Goddard grants under awards NNG04GP57G and NNG04GI07G. Use of the HPCAT facility was supported by DOE-BES, DOE-NNSA, NSF, DOD -TACOM, and the W.M. Keck Foundation. APS is supported by DOE-BES under Contract No. W-31-109-Eng-38.

Effect of Nb on Delayed Fracture Resistance of Ultra-High Strength Martensitic Steels

NASA Astrophysics Data System (ADS)

Song, Rongjie; Fonstein, Nina; Pottore, Narayan; Jun, Hyun Jo; Bhattacharya, Debanshu; Jansto, Steve

Ultra-high strength steels are materials of considerable interest for automotive and structural applications and are increasingly being used in those areas. Higher strength, however, makes steels more prone to hydrogen embrittlement (HE). The effects of Nb and other alloying elements on the hydrogen-induced delayed fracture resistance of cold rolled martensitic steels with ultra-high strength 2000 MPa were studied using an acid immersion test, thermal desorption analysis (TDA) and measuring of permeation. The microstructure was characterized by high resolution field emission Scanning Electron Microscopy (SEM) with Electron Backscattered Diffraction (EBSD) and Transmission Electron Microscopy (TEM). It was shown that the combined addition of Nb significantly improved the delayed fracture resistance of investigated steel. The addition of Nb to alloyed martensitic steels resulted in very apparent grain refinement of the prior austenite grain size. The Nb microalloyed steel contained a lower diffusible hydrogen content during thermal desorption analysis as compared to the base steel and had a higher trapped hydrogen amount after charging. The reason that Nb improved the delayed fracture resistance of steels can be attributed mostly to both hydrogen trapping and grain refinement.

In-situ laser ultrasonic measurement of the hcp to bcc transformation in commercially pure titanium

DOE Office of Scientific and Technical Information (OSTI.GOV)

Shinbine, A., E-mail: alyssa.shinbine@gmail.com; Garcin, T.; Sinclair, C.

2016-07-15

Using a novel in-situ laser ultrasonic technique, the evolution of longitudinal velocity was used to measure the α − β transformation during cyclic heating and cooling in commercially pure titanium. In order to quantify the transformation kinetics, it is shown that changes in texture can not be ignored. This is particularly important in the case of titanium where significant grain growth occurs in the β-phase leading to the ultrasonic wave sampling a decreasing number of grains on each thermal treatment cycle. Electron backscatter diffraction measurements made postmortem in the region where the ultrasonic pulse traveled were used to obtain anmore » estimate of such local texture and grain size changes. An analysis technique for including the anisotropy of wave velocity depending on local texture is presented and shown to give self consistent results for the transformation kinetics. - Highlights: • Laser ultrasound and EBSD interpret the hcp/bcc phase transformation in cp-Ti. • Grain growth and texture produced variation in velocity during similar treatments. • Texture was deconvoluted from phase addition to obtain transformation kinetics.« less

Characterization and modeling of mechanical behavior of single crystal titanium deformed by split-Hopkinson pressure bar

DOE PAGES

Morrow, B. M.; Lebensohn, R. A.; Trujillo, C. P.; ...

2016-03-28

Single crystal titanium samples were dynamically loaded using split-Hopkinson pressure bar (SHPB) and the resulting microstructures were examined. Characterization of the twins and dislocations present in the microstructure was conducted to understand the pathway for observed mechanical behavior. Electron backscatter diffraction (EBSD) was used to measure textures and quantify twinning. Microstructures were profusely twinned after loading, and twin variants and corresponding textures were different as a function of initial orientation. Focused ion beam (FIB) foils were created to analyze dislocation content using transmission electron microscopy (TEM). Large amounts of dislocations were present, indicating that plasticity was achieved through slip andmore » twinning together. Viscoplastic self-consistent (VPSC) modeling was used to confirm the complex order of operations during deformation. The activation of different mechanisms was highly dependent upon crystal orientation. For [0001] and View the MathML source[101¯1]-oriented crystals, compressive twinning was observed, followed by secondary tensile twinning. Furthermore, dislocations though prevalent in the microstructure, contributed to final texture far less than twinning.« less

Understanding the Effect of Grain Boundary Character on Dynamic Recrystallization in Stainless Steel 316L

NASA Astrophysics Data System (ADS)

Beck, Megan; Morse, Michael; Corolewski, Caleb; Fritchman, Koyuki; Stifter, Chris; Poole, Callum; Hurley, Michael; Frary, Megan

2017-08-01

Dynamic recrystallization (DRX) occurs during high-temperature deformation in metals and alloys with low to medium stacking fault energies. Previous simulations and experimental research have shown the effect of temperature and grain size on DRX behavior, but not the effect of the grain boundary character distribution. To investigate the effects of the distribution of grain boundary types, experimental testing was performed on stainless steel 316L specimens with different initial special boundary fractions (SBF). This work was completed in conjunction with computer simulations that used a modified Monte Carlo method which allowed for the addition of anisotropic grain boundary energies using orientation data from electron backscatter diffraction (EBSD). The correlation of the experimental and simulation work allows for a better understanding of how the input parameters in the simulations correspond to what occurs experimentally. Results from both simulations and experiments showed that a higher fraction of so-called "special" boundaries ( e.g., Σ3 twin boundaries) delayed the onset of recrystallization to larger strains and that it is energetically favorable for nuclei to form on triple junctions without these so-called "special" boundaries.

Grain Cluster Microstructure and Grain Boundary Character Distribution in Alloy 690

NASA Astrophysics Data System (ADS)

Xia, Shuang; Zhou, Bangxin; Chen, Wenjue

2009-12-01

The effects of thermal-mechanical processing (TMP) on microstructure evolution during recrystallization and grain boundary character distribution (GBCD) in aged Alloy 690 were investigated by the electron backscatter diffraction (EBSD) technique and optical microscopy. The original grain boundaries of the deformed microstructure did not play an important role in the manipulation of the proportion of the Σ3 n ( n = 1, 2, 3…) type boundaries. Instead, the grain cluster formed by multiple twinning starting from a single nucleus during recrystallization was the key microstructural feature affecting the GBCD. All of the grains in this kind of cluster had Σ3 n mutual misorientations regardless of whether they were adjacent. A large grain cluster containing 91 grains was found in the sample after a small-strain (5 pct) and a high-temperature (1100 °C) recrystallization anneal, and twin relationships up to the ninth generation (Σ39) were found in this cluster. The ratio of cluster size over grain size (including all types of boundaries as defining individual grains) dictated the proportion of Σ3 n boundaries.

TEM investigations on twin boundary structures of feathery crystals in aluminum alloys during Bridgman solidification

NASA Astrophysics Data System (ADS)

Yang, Luyan; Li, Shuangming; Fan, Kai; Li, Yang; Zhong, Hong; Fu, Hengzhi

2018-06-01

Feathery crystals are an ensemble of twinned dendrites, and are characterized by a unique twin boundary (TB) structure in the solidification pattern of aluminum alloys. In this work, the high-density twinned dendrites of Al-4.5 wt% Cu alloys, produced during the Bridgman solidification, have been studied using electron backscattered diffraction (EBSD) and high-resolution transmission electron microscopy (HRTEM). The experimental results showed that, after systematically decreasing the growth rate from 3000 μm/s to 1 μm/s, the TBs remained stable, while the solute field around the TBs changed significantly. According to the HRTEM results, successive stacking faults were occurred near the TBs at 1 μm/s, while slight distortion was observed around the TBs at 3000 μm/s. The composition analysis revealed an obvious solute enrichment near the TBs. Furthermore, the solute gradient profile within the TBs became smoother with the decrease in the growth speed. This is due to the more sufficient solid-state back diffusion occurring perpendicular to the twin plane after the solidification.

Effect of composition on the tensile properties and fracture toughness of A7N01S-T5 aluminum alloys welded joints

NASA Astrophysics Data System (ADS)

Liu, Yali; Gou, Guoqing; Chen, Jia; Chen, Hui; Wang, Wanjng; Li, Xiaodong; Che, Xiaoli; Wang, Yirong

2017-07-01

In this paper, welded joints of four types of A7N01S-T5 aluminum alloy with different chemical compositions were investigated. The welding process was under 70% environmental humidity conditions at 10∘C with single-pulse GMAW welding technology. The strength and fracture toughness of the four types of samples were tested, and the microstructures were investigated by micro-X-ray fluorescence (SR-LXRF) technology and backscattered electron diffraction (EBSD) technology. The results showed that the #2 alloy that is composed of Zn: 4.59 wt.%, Mg: 1.56 wt.% Mn: 0.22 wt.%, Cr: 0.14 wt.%, Zr: 0.01 wt.% and Ti: 0.027 wt.% had the best combination of tensile strength and elongation, with the values of 302.35 MPa and 3.74%, respectively. The better result for the combination of the strength and elongation was mainly determined by the volume fraction and size. The fine grain size and compositions played important roles to obtain high fracture toughness.

Synthesis and characterization of Ti-27.5Nb alloy made by CLAD® additive manufacturing process for biomedical applications.

PubMed

Fischer, M; Laheurte, P; Acquier, P; Joguet, D; Peltier, L; Petithory, T; Anselme, K; Mille, P

2017-06-01

Biocompatible beta-titanium alloys such as Ti-27.5(at.%)Nb are good candidates for implantology and arthroplasty applications as their particular mechanical properties, including low Young's modulus, could significantly reduce the stress-shielding phenomenon usually occurring after surgery. The CLAD® process is a powder blown additive manufacturing process that allows the manufacture of patient specific (i.e. custom) implants. Thus, the use of Ti-27.5(at.%)Nb alloy formed by CLAD® process for biomedical applications as a mean to increase cytocompatibility and mechanical biocompatibility was investigated in this study. The microstructural properties of the CLAD-deposited alloy were studied with optical microscopy and electron back-scattered diffraction (EBSD) analysis. The conservation of the mechanical properties of the Ti-27.5Nb material after the transformation steps (ingot-powder atomisation-CLAD) were verified with tensile tests and appear to remain close to those of reference material. Cytocompatibility of the material and subsequent cell viability tests showed that no cytotoxic elements are released in the medium and that viable cells proliferated well. Copyright © 2017 Elsevier B.V. All rights reserved.

Correlation of Fracture Behavior With Microstructure in Friction Stir Welded, and Spin Formed AI-Li 2195 Domes

NASA Technical Reports Server (NTRS)

Tayon, Wesley A.; Domack, Marcia S.; Hales, Stephen J.

2012-01-01

Single-piece, spin-formed domes manufactured from friction stir welded (FSW) plates of Al-Li alloy 2195 have the potential to reduce the cost of fabricating cryogenic propellant tanks. Mechanical properties in the completed domes can be related directly to the final material condition and the microstructures developed. However, these new fabrication techniques have resulted in unexpected material challenges, such as abnormal grain growth in the weld nugget and the propensity for fracture in the adjacent thermo-mechanically affected zone (TMAZ). In this study, the microstructure and texture transformations within the TMAZ are related to fracture location in the vicinity of the weldment. The texture variations in the TMAZ are caused primarily by the varying amounts of shear deformation introduced during the FSW process. Grain morphology and microtexture characteristics are examined as a function of location in the TMAZ via electron backscatter diffraction (EBSD). A strong correlation between fracture location and the presence of texture banding in the TMAZ is observed. The fracture path tends to follow a distinct region of low Taylor Factor (TF) grains.

Investigation of the material flow and texture evolution in friction-stir welded aluminum alloy

NASA Astrophysics Data System (ADS)

Kang, Suk Hoon; Han, Heung Nam; Oh, Kyu Hwan; Cho, Jae-Hyung; Lee, Chang Gil; Kim, Sung-Joon

2009-12-01

The material flow and crystallographic orientation in aluminum alloy sheets joined by friction stir welding (FSW) were investigated by electron back scattered diffraction (EBSD). The microstructure and microtexture of the material near the stir zone was found to be influenced by the rotational behavior of the tool pin. It was found that, during FSW, the forward movement of the tool pin resulted in loose contact between the tool pin and the receding material at the advancing side. This material behavior inside the joined aluminum plates was also observed by an X-ray micrograph by inlaying a gold marker into the plates. As the advancing speed of the tool increases at a given rotation speed, the loose contact region widens. As the microtexture of the material near the stir zone is very close to the simple shear texture on the basis of the frame of the tool pin in the normal and tangent directions, the amount of incompletely rotated material due to the loose contact could be estimated from the tilt angle of the shear texture in the pole figure around the key hole.

In situ micro-compression testing of He2+ ion irradiated titanium aluminide

NASA Astrophysics Data System (ADS)

Wei, Tao; Xu, Alan; Zhu, Hanliang; Ionescu, Mihail; Bhattacharyya, Dhriti

2017-10-01

A titanium aluminide (TiAl) alloy 45XD has been irradiated by a He ion beam with an energy of 5 MeV on a tandem accelerator at the Australian Nuclear Science and Technology Organization (ANSTO). The total fluence of He ions was 5 × 1017 ion cm-2. A 17 μm uniform damage region from the material surface with a helium concentration of about 5000 appm was achieved by using an energy degrading wheel in front of the TiAl target. The micro-size test specimens from the damage layer were fabricated using a focused ion beam & scanning electron microscope (FIB-SEM) system. The in situ SEM micromechanical compressive testing was carried out inside an SEM and the results indicated irradiation embrittlement in the helium affected region. Electron back scatter diffraction (EBSD) analysis has been applied to reveal the orientation of the lamellae in the TiAl specimens, and used to understand the deformation processes in the sample. The irradiation damage of gallium ion beam from FIB on the surface of TiAl sample was also investigated.

Correlation of Fracture Behavior with Microstructure in Friction Stir Welded, and Spin-Formed Al-Li 2195 Domes

NASA Astrophysics Data System (ADS)

Tayon, Wesley A.; Domack, Marcia S.; Hales, Stephen J.

Single-piece, spin-formed domes manufactured from friction stir welded (FSW) plates of Al-Li alloy 2195 have the potential to reduce the cost of fabricating cryogenic propellant tanks. Mechanical properties in the completed domes can be related directly to the final material condition and the microstructures developed. However, these new fabrication techniques have resulted in unexpected material challenges, such as abnormal grain growth in the weld nugget and the propensity for fracture in the adjacent thermo-mechanically affected zone (TMAZ). In this study, the microstructure and texture transformations within the TMAZ are related to fracture location in the vicinity of the weldment. The texture variations in the TMAZ are caused primarily by the varying amounts of shear deformation introduced during the FSW process. Grain morphology and microtexture characteristics are examined as a function of location in the TMAZ via electron backscatter diffraction (EBSD). A strong correlation between fracture location and the presence of texture banding in the TMAZ is observed. The fracture path tends to follow a distinct region of low Taylor Factor (TF) grains.

Nanoscale insights on one- and two-dimensional material structures

NASA Astrophysics Data System (ADS)

Floresca, Herman Carlo

The race for smaller, faster and more efficient devices has led researchers to explore the possibilities of utilizing nanostructures for scaling. These one-dimensional and two-dimensional materials have properties that are attractive for this purpose but are still not well controlled. Control comes with a complete understanding of the materials' electrical, thermal, optical and structural characteristics but is difficult to obtain due to their small scale. This work is intended to help researchers overcome the difficulty in studying nanostructures by providing techniques for analysis and insights of nanostructures that have not been previously available. Two nanostructures were studied: silicon nanowires and graphene. The nanowires were prepared for cross-section transmission electron microscopy (TEM) to discover the effects that controlled oxidation has on the dimensions and shape of the nanowires. Since cross-section TEM is not able to provide information about surface structure, a method for manipulating the wires with orientation control was developed. With this ability, all three orthogonal views of the nanowire were compiled for a comprehensive study on its structure in terms of shape and surface roughness. Graphene was used for a two-dimensional analytical technique that took advantage of customized computer programs for data acquisition, measurement and display. With the information provided, distinctions between grain boundary types in polycrystalline graphene were made and supported by statistical information from the software's output. It was also applied to a growth series of graphene samples in conjunction with scanning electron microscopy (SEM) images and electron backscatter diffraction (EBSD) maps. The results help point to origins of graphene's polycrystalline nature. This dissertation concludes with a thought towards the future by highlighting a method that can help analyze nanostructures, which may become incorporated into the structures of large devices. The fold-out method is a TEM sample preparation technique utilizing a focused ion beam (FIB) for site specific thinning across a large sample area. Its process is demonstrated along with advantages over conventional methods.

Modelling of deformation and recrystallisation microstructures in rocks and ice

NASA Astrophysics Data System (ADS)

Bons, Paul D.; Evans, Lynn A.; Gomez-Rivas, Enrique; Griera, Albert; Jessell, Mark W.; Lebensohn, Ricardo; Llorens, Maria-Gema; Peternell, Mark; Piazolo, Sandra; Weikusat, Ilka; Wilson, Chris J. L.

2015-04-01

Microstructures both record the deformation history of a rock and strongly control its mechanical properties. As microstructures in natural rocks only show the final "post-mortem" state, geologists have attempted to simulate the development of microstructures with experiments and later numerical models. Especially in-situ experiments have given enormous insight, as time-lapse movies could reveal the full history of a microstructure. Numerical modelling is an alternative approach to simulate and follow the change in microstructure with time, unconstrained by experimental limitations. Numerical models have been applied to a range of microstructural processes, such as grain growth, dynamic recrystallisation, porphyroblast rotation, vein growth, formation of mylonitic fabrics, etc. The numerical platform "Elle" (www.elle.ws) in particular has brought progress in the simulation of microstructural development as it is specifically designed to include the competition between simultaneously operating processes. Three developments significantly improve our capability to simulate microstructural evolution: (1) model input from the mapping of crystallographic orientation with EBSD or the automatic fabric analyser, (2) measurement of grain size and crystallographic preferred orientation evolution using neutron diffraction experiments and (3) the implementation of the full-field Fast Fourier Transform (FFT) solver for modelling anisotropic crystal-plastic deformation. The latter enables the detailed modelling of stress and strain as a function of local crystallographic orientation, which has a strong effect on strain localisation such as, for example, the formation of shear bands. These models can now be compared with the temporal evolution of crystallographic orientation distributions in in-situ experiments. In the last decade, the possibility to combine experiments with numerical simulations has allowed not only verification and refinement of the numerical simulation technique but also increased significantly the ability to predict and/or interpret natural microstructures. This contribution will present the most recent developments in in-situ and numerical modelling of deformation and recrystallisation microstructures in rocks and in ice.

Mineral texture based seismic properties of meta-sedimentary and meta-igneous rocks in the orogenic wedge of the Central Scandinavian Caledonides

NASA Astrophysics Data System (ADS)

Almqvist, B. S. G.; Czaplinska, D.; Piazolo, S.

2015-12-01

Progress in seismic methods offers the possibility to visualize in ever greater detail the structure and composition of middle to lower continental crust. Ideally, the seismic parameters, including compressional (Vp) and shear (Vs) wave velocities, anisotropy and Vp/Vs-ratio, allow the inference of detailed and quantitative information on the deformation conditions, chemical composition, temperature and the amount and geometry of fluids and melts in the crust. However, such inferences regarding the crust should be calibrated with known mineral and rock physical properties. Seismic properties calculated from the crystallographic preferred orientation (CPO) and laboratory measurements on representative core material allow us to quantify the interpretations from seismic data. The challenge of such calibrations lies in the non-unique interpretation of seismic data. A large catalogue of physical rock properties is therefore useful, with as many constraining geophysical parameters as possible (including anisotropy and Vp/Vs ratio). We present new CPO data and modelled seismic properties for amphibolite and greenschist grade rocks representing the orogenic wedge in the Central Scandinavian Caledonides. Samples were collected from outcrops in the field and from a 2.5 km long drill core, which penetrated an amphibolite-grade allochthonous unit composed of meta-sedimentary and meta-igneous rocks, as well as mica and chlorite-rich mylonites. The textural data was acquired using large area electron backscatter diffraction (EBSD) maps, and the chemical composition of minerals obtained by energy dispersive x-ray (EDS). Based on the texture data, we compare and evaluate some of the existing methods to calculate texture-based seismic properties of rocks. The suite of samples consists of weakly anisotropic rocks such as felsic gneiss and calc-silicates, and more anisotropic amphibolite, metagabbro, mica-schist. The newly acquired dataset provides a range of seismic properties that improves compositional and structural characterization of deformed middle and lower crust.

The relevance of grain dissection for grain size reduction in polar ice: insights from numerical models and ice core microstructure analysis

NASA Astrophysics Data System (ADS)

Steinbach, Florian; Kuiper, Ernst-Jan N.; Eichler, Jan; Bons, Paul D.; Drury, Martyn R.; Griera, Albert; Pennock, Gill M.; Weikusat, Ilka

2017-09-01

The flow of ice depends on the properties of the aggregate of individual ice crystals, such as grain size or lattice orientation distributions. Therefore, an understanding of the processes controlling ice micro-dynamics is needed to ultimately develop a physically based macroscopic ice flow law. We investigated the relevance of the process of grain dissection as a grain-size-modifying process in natural ice. For that purpose, we performed numerical multi-process microstructure modelling and analysed microstructure and crystallographic orientation maps from natural deep ice-core samples from the North Greenland Eemian Ice Drilling (NEEM) project. Full crystallographic orientations measured by electron backscatter diffraction (EBSD) have been used together with c-axis orientations using an optical technique (Fabric Analyser). Grain dissection is a feature of strain-induced grain boundary migration. During grain dissection, grain boundaries bulge into a neighbouring grain in an area of high dislocation energy and merge with the opposite grain boundary. This splits the high dislocation-energy grain into two parts, effectively decreasing the local grain size. Currently, grain size reduction in ice is thought to be achieved by either the progressive transformation from dislocation walls into new high-angle grain boundaries, called subgrain rotation or polygonisation, or bulging nucleation that is assisted by subgrain rotation. Both our time-resolved numerical modelling and NEEM ice core samples show that grain dissection is a common mechanism during ice deformation and can provide an efficient process to reduce grain sizes and counter-act dynamic grain-growth in addition to polygonisation or bulging nucleation. Thus, our results show that solely strain-induced boundary migration, in absence of subgrain rotation, can reduce grain sizes in polar ice, in particular if strain energy gradients are high. We describe the microstructural characteristics that can be used to identify grain dissection in natural microstructures.

Twin related domains in 3D microstructures of conventionally processed and grain boundary engineered materials

DOE PAGES

Lind, Jonathan; Li, Shiu Fai; Kumar, Mukul

2016-05-20

The concept of twin-limited microstructures has been explored in the literature as a crystallographically constrained grain boundary network connected via only coincident site lattice (CSL) boundaries. The advent of orientation imaging has made classification of twin-related domains (TRD) or any other orientation cluster experimentally accessible in 2D using EBSD. With the emergence of 3D orientation mapping, a comparison of TRDs in measured 3D microstructures is performed in this paper and compared against their 2D counterparts. The TRD analysis is performed on a conventionally processed (CP) and a grain boundary engineered (EM) high purity copper sample that have been subjected tomore » successive anneal procedures to promote grain growth. Finally, the EM sample shows extremely large TRDs which begin to approach that of a twin-limited microstructure, while the TRDs in the CP sample remain relatively small and remote.« less

Preliminary 3D In-situ measurements of the texture evolution of strained H2O ice during annealing using neutron Laue diffractometry

NASA Astrophysics Data System (ADS)

Journaux, Baptiste; Montagnat, Maurine; Chauve, Thomas; Ouladdiaf, Bachir; Allibon, John

2015-04-01

Dynamic recrystallization (DRX) strongly affects the evolution of microstructure (grain size and shape) and texture (crystal preferred orientation) in materials during deformation at high temperature. Since texturing leads to anisotropic physical properties, predicting the effect of DRX is essential for industrial applications, for interpreting geophysical data and modeling geodynamic flows, and predicting ice sheet flow and climate evolution. A large amount of literature is available related to metallurgy, geology or glaciology, but there remains overall fundamental questions about the relationship between nucleation, grain boundary migration and texture development at the microscopic scale. Previous measurements of DRX in ice were either conducted using 2D ex-situ techniques such as AITA [1,2] or Electron Backscattering Diffraction (EBSD) [3], or using 3D statistical ex-situ [4] or in-situ [5] techniques. Nevertheless, all these techniques failed to observe at the scale of nucleation processes during DRX in full 3D. Here we present a new approach using neutron Laue diffraction, which enable to perform 3D measurements of in-situ texture evolution of strained polycrystalline H2O ice (>2% at 266 K) during annealing at the microscopic scale. Thanks the CYCLOPS instrument [6] (Institut Laue Langevin Grenoble, France) and the intrinsic low background of this setup, preliminary observations enabled us to follow, in H2O ice, the evolution of serrated grain boundaries, and kink-band during annealing. Our observations show a significant evolution of the texture and internal misorientation over the course of few hours at an annealing temperature of 268.5 K. In the contrary, ice kink-band structures seem to be very stable over time at near melting temperatures. The same samples have been analyzed ex-situ using EBSD for comparison. These results represent a first step toward in-situ microscopic measurements of dynamic recrystallization processes in ice during strain. This experiment has been conducted in the frame of the ANR-funded DREAM project that focuses on the recrystallization processes in anisotropic materials. References [1] D. S. Russell-Head and C.J.L. Wilson., 2001, Journal of Glaciology, 24, 117-130. [2] Wilson, C.J.L., Peternell, M., Piazolo, S., Luzin, V., 2014, Journal of Structural Geology, Microdynamics of Ice, 61, 50-77. [3] M. Montagnat, T. Chauve, F. Barou, A. Tommasi, B. Beausir, C. Fressengeas., in prep. [4] T. H. Jacka and J. Li., 2000, In T. Hondoh, editor, Physics of Ice Core Records, pages 83-102. Hokkaido University Press, Sapporo. [5] S. Piazolo, C. J. L. Wilson, V. Luzin, C. Brouzet, and M. Peternell., 2013, Geochemistry, Geophysics, Geosystems, 14, 4185-4194. [6] B. Ouladdiaf et al., 2011, Journal of Applied Crystallography, 44, 392-397.

A novel multi-detection technique for three-dimensional reciprocal-space mapping in grazing-incidence X-ray diffraction.

PubMed

Schmidbauer, M; Schäfer, P; Besedin, S; Grigoriev, D; Köhler, R; Hanke, M

2008-11-01

A new scattering technique in grazing-incidence X-ray diffraction geometry is described which enables three-dimensional mapping of reciprocal space by a single rocking scan of the sample. This is achieved by using a two-dimensional detector. The new set-up is discussed in terms of angular resolution and dynamic range of scattered intensity. As an example the diffuse scattering from a strained multilayer of self-assembled (In,Ga)As quantum dots grown on GaAs substrate is presented.

The statistical kinematical theory of X-ray diffraction as applied to reciprocal-space mapping

PubMed

Nesterets; Punegov

2000-11-01

The statistical kinematical X-ray diffraction theory is developed to describe reciprocal-space maps (RSMs) from deformed crystals with defects of the structure. The general solutions for coherent and diffuse components of the scattered intensity in reciprocal space are derived. As an example, the explicit expressions for intensity distributions in the case of spherical defects and of a mosaic crystal were obtained. The theory takes into account the instrumental function of the triple-crystal diffractometer and can therefore be used for experimental data analysis.

Mapping of reciprocal space of La{sub 0.30}CoO{sub 2} in 3D: Analysis of superstructure diffractions and intergrowths with Co{sub 3}O{sub 4}

DOE Office of Scientific and Technical Information (OSTI.GOV)

Brázda, Petr, E-mail: brazda@fzu.cz; Palatinus, Lukáš; Klementová, Mariana

2015-07-15

We have used electron diffraction tomography and powder X-ray diffraction to elucidate the structural properties of layered cobaltate γ-La{sub 0.30}CoO{sub 2}. The structure consists of hexagonal sheets of edge-sharing CoO{sub 6} octahedra interleaved by lanthanum monolayers. The La{sup 3+} cations occupy only one third of available P2 sites, forming a 2-dimensional a√3×a√3 superstructure in a–b plane. The results show that there exists no order in the mutual relative shift between the neighbouring La interlayers within the a–b plane. This is manifested in the observed monotonous decrease of the diffracted intensity of the superstructure diffractions along c{sup ⁎} in both X-raymore » and electron diffraction data. The observed lack of stacking order differentiates the La{sub x}CoO{sub 2} from its Ca and Sr analogues where at least a partial stacking order of the cationic interlayers is manifested in experimental data published in literature. - Highlights: • We use electron diffraction tomography for reciprocal space mapping of La{sub 0.30}CoO{sub 2}. • We observed a complete disorder of the stacking of Lanthanum interlayers. • Co{sub 3}O{sub 4} intergrown with La{sub 0.30}CoO{sub 2} crystals brings about fake superstructure diffractions. • Twinning of Co{sub 3}O{sub 4} enhances the problem of fake superstructure diffractions.« less

Electron backscatter diffraction analysis of Nb3Al multifilamentary strands prepared by rapid heating, quenching and transformation annealing

NASA Astrophysics Data System (ADS)

Takeuchi, T.; Tsuchiya, K.; Saeda, M.; Banno, N.; Kikuchi, A.; Iijima, Y.

2010-12-01

To enhance the non-Cu critical current density Jc at 15 T and 4.2 K (1000 A mm - 2 at present) we have endeavoured to refine the grain size of rapid heating, quenching and transformation (RHQT)-processed Nb3Al. In the present study, the grain boundary structures of RHQT-processed Nb3Al were examined by electron backscatter diffraction (EBSD) because transgranular fracture prevents the observation of fractured cross sections of Nb3Al to statistically determine the grain size. The grain size distributions of body-centred-cubic supersaturated-solid-solution Nb(Al)ss and A15 Nb3Al filaments were measured for grains misoriented by more than 2°, 5° and 15°. A mixed grain structure, which consists of a few large grains (>25 µm) and many small grains (<1 µm), was observed for an Nb3Al filament that had been transformed from non-deformed Nb(Al)ss. Plastic deformation that had been made between the rapid heating and quenching steps and the transformation step apparently homogenized the grain size distribution and then reduced the average grain size. The misorientation angle distributions of Nb(Al)ss and Nb3Al were also measured and compared with each other. A clear relationship between the Jc and the inverse grain size was not confirmed for the RHQT Nb3Al conductors examined in the present study, which indicates the importance of making a filament compositionally homogeneous to obtain a high Jc.

Surface Crystallization of a MgO/Y2O3/SiO2/Al2O3/ZrO2 Glass: Growth of an Oriented β-Y2Si2O7 Layer and Epitaxial ZrO2

PubMed Central

Wisniewski, Wolfgang; Seidel, Sabrina; Patzig, Christian; Rüssel, Christian

2017-01-01

The crystallization behavior of a glass with the composition 54.7 SiO2·10.9 Al2O3·15.0 MgO·3.4 ZrO2·16.0 Y2O3 is studied using X-ray diffraction (XRD), scanning electron microscopy (SEM) including electron backscatter diffraction (EBSD) and (scanning) transmission electron microscopy [(S)TEM] including energy-dispersive X-ray spectrometry (EDXS). This glass shows the sole surface crystallization of four different yttrium silicates of the composition Y2Si2O7 (YS). The almost simultaneous but independent nucleation of α-, β-, δ-, and ε-YS at the surface is followed by growth into the bulk, where ε-YS quickly dominates a first crystallized layer. An accumulation of Mg at the growth front probably triggers a secondary nucleation of β-YS, which forms a thin compact layer before fragmenting into a highly oriented layer of fine grained crystals occupying the remaining bulk. The residual glass between the YS growth structures allows the crystallization of indialite, yttrium stabilized ZrO2 (Y-ZrO2) and very probably μ-cordierite during cooling. Hence, this glass basically shows the inverted order of crystallization observed in other magnesium yttrium alumosilicate glasses containing less Y2O3. An epitaxial relationship between Y-ZrO2 and ε-YS is proven and multiple twinning relationships occur in the YS phases. PMID:28281661

Effect of cold rolling on the microstructural evolution of new β-typed Ti–6Mo–6V–5Cr–3Sn–2.5Zr alloys

DOE Office of Scientific and Technical Information (OSTI.GOV)

Choi, Gwnaghyo; Lee, Kwangmin, E-mail: kmlee@jnu.a

A Ti–6Mo–6V–5Cr–3Sn–2.5Zr (wt.%) alloy was designed as a new metastable β-Ti alloy. The effect that cold rolling had on the microstructural evolution of the material was investigated via optical microscopy (OM), X-ray diffraction (XRD), electron back-scattered diffraction (EBSD) and transmission electron microscopy (TEM) measurements. A single β phase formed in the alloy after solution treatment at 780 °C for 30 min followed by water quenching. The solution-treated alloy was cold rolled with thickness reductions of 10%, 30%, 50% and 70%, and the hardness values increased as the thickness of the specimen decreased. The textures of the cold rolled specimen weremore » characterized according to the 〈110〉 partial parallel to the rolling direction as the rolling reduction increased. The crystallographic orientation showed principal α-fiber textures for (111)〈110〉 and (112)〈110〉. The cold deformation led to the appearance of martensite α″ phases, particularly stress-induced martensite (SIM) α″ phases. - Highlights: • Effect of cold rolling on new β-typed Ti-6Mo-6V-5Cr-3Sn-2.5Zr alloy was studied. • A single β phase was obtained after solution treatment at 780 °C for 30 min. • α-Fiber textures became dominated with the increase in cold rolling reduction. • A stress-induced α″ martensite was caused by cold rolling.« less

Thermoelectric properties of Co₄Sb₁₂ with Bi₂Te₃ nanoinclusions.

PubMed

Ghosh, Sanyukta; Bisht, Anuj; Karati, Anirudha; Rogl, Gerda; Rogl, Peter F; Murty, B S; Suwas, Satyam; Mallik, Ramesh Chandra

2018-01-08

The figure of merit (zT) of a thermoelectric material can be enhanced by incorporation of nanoinclusions into bulk material. The presence of bismuth telluride (Bi2Te3) nanoinclusions in Co4Sb12 leads to lower phonon thermal conductivity by introducing interfaces and defects; it enhances the average zT between 300-700 K. In the current study, Bi2Te3 nanoparticles were dispersed into bulk Co4Sb12 by ball-milling. The bulk was fabricated by spark plasma sintering (SPS). The presence of Bi2Te3 dispersion in Co4Sb12 was confirmed by X-ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM) and electron back scattered diffraction (EBSD) technique. Energy dispersive spectroscopy (EDS) showed antimony (Sb) as an impurity phase for higher contents of Bi2Te3 in the sample. The Seebeck coefficient (S) and electrical conductivity () were measured in the temperature range of 350 - 673 K. The negative value of S indicates that most of the charge carriers were electrons. A decrease in S and increase in with Bi2Te3 content are due to the increased carrier concentration, as confirmed by Hall measurement. The thermal conductivity, measured between 423 - 673 K, decreased due to the increased phonon scattering at interfaces. A maximum zT of 0.17 was achieved at 523 K and it did not vary much throughout the temperature range. The experimental results of composites were compared by using effective medium theories. © 2018 IOP Publishing Ltd.

Pyrite deformation and connections to gold mobility: insight from micro-structural analysis and trace element mapping

NASA Astrophysics Data System (ADS)

Dubosq, Renelle; Rogowitz, Anna; Lawley, Christopher; Schneider, David; Jackson, Simon

2017-04-01

Pyrite is an important and ubiquitous gold-bearing phase in many orogenic gold deposits making the study of its deformation behaviour under metamorphic conditions crucial to the understanding of gold (re)mobilization. However, pyrite deformation mechanisms and their influence on the retention or release of trace elements during deformation and metamorphism remain poorly understood. We propose a syn- to post-peak metamorphic and deformation driven gold upgrading model where gold is remobilized through deformation-induced diffusion pathways in the form of substructures in pyrite. The middle amphibolite facies assemblage (actinolite-biotite-plagioclase-almandine) of the Detour Lake deposit (Canada) makes it an ideal study area due to maximum temperatures reaching 550°C, exceeding the conditions for plastic deformation in pyrite (450°C). The world-class Detour Lake deposit, containing 16.4 Moz of Au at 1 g/t, is a Neoarchean orogenic gold ore body located in the northern Abitibi district within the Superior Province. The mine is situated along the high strain, sub-vertical ductile-brittle Sunday Lake Deformation Zone (SLDZ) parallel to the broadly E-W trending Abitibi greenstone belt. Herein we combine orientation contrast (OC) forescatter imaging, electron backscatter diffraction (EBSD) and 2D laser ablation inductively coupled plasma mass spectrometry (LA-ICP-MS) trace element pyrite mapping to evaluate the influence of pyrite brittle and plastic deformation on the release of trace elements during syn-metamorphic gold remobilization. Local misorientation patterns in pyrite exhibit parallel bands that can be described by continuous rotation around one of the <100> axes, whereas higher strain areas reveal more heterogeneous misorientation patterns and the development of low-angle grain boundaries with late fractures indicative of dislocation creep and strain hardening. These late fractures are an important micro-structural setting for gold and clusters of precious-metal mineral inclusions (telluride minerals). Minor recrystallization processes can also be observed along phase boundaries between pyrite and more competent amphibole crystals. LA-ICP-MS trace element maps document primary, syn-metamorphic oscillatory zoning of some chalcophile and siderophile elements during crystallization of pyrite porphyroblasts. These primary pyrite features are cut by late metal-rich fractures suggesting that remobilization of gold occurred with trace element enrichment of other chalcophile and siderophile elements (Cu, Pb, Zn, Ag, Bi, Te), which post-dates the main period of syn-metamorphic pyrite crystallization at the margins of pre- to syn-deformation, high-grade gold veins. Pyrite grain boundaries and subgrains are also base and precious metal rich, suggesting that late gold remobilization also occurred during pyrite recrystallization. Additional trace element mapping will help determine to what extent pyrite plastic deformation facilitates the diffusion of gold and other trace elements during gold precipitation and remobilization, which, in turn, will inform the source to sink pathways of ore deposition.

Flat ion milling: a powerful tool for preparation of cross-sections of lead-silver alloys.

PubMed

Brodusch, Nicolas; Boisvert, Sophie; Gauvin, Raynald

2013-06-01

While conventional mechanical and chemical polishing results in stress, deformation and polishing particles embedded on the surface, flat milling with Ar+ ions erodes the material with no mechanical artefacts. This flat milling process is presented as an alternative method to prepare a Pb-Ag alloy cross-section for scanning electron microscopy. The resulting surface is free of scratches with very little to no stress induced, so that electron diffraction and channelling contrast are possible. The results have shown that energy dispersive spectrometer (EDS) mapping, electron channelling contrast imaging and electron backscatter diffraction can be conducted with only one sample preparation step. Electron diffraction patterns acquired at 5 keV possessed very good pattern quality, highlighting an excellent surface condition. An orientation map was acquired at 20 keV with an indexing rate of 90.1%. An EDS map was performed at 5 keV, and Pb-Ag precipitates of sizes lower than 100 nm were observed. However, the drawback of the method is the generation of a noticeable surface topography resulting from the interaction of the ion beam with a polycrystalline and biphasic sample.

Optical diffraction tomography using a digital micromirror device for stable measurements of 4D refractive index tomography of cells

NASA Astrophysics Data System (ADS)

Shin, Seungwoo; Kim, Kyoohyun; Kim, Taeho; Yoon, Jonghee; Hong, Kihyun; Park, Jinah; Park, YongKeun

2016-03-01

Optical diffraction tomography (ODT) is an interferometric microscopy technique capable of measuring 3-D refractive index (RI) distribution of transparent samples. Multiple 2-D holograms of a sample illuminated with various angles are measured, from which 3-D RI map of the sample is reconstructed via the diffraction theory. ODT has been proved as a powerful tool for the study of biological cells, due to its non-invasiveness, label-free and quantitative imaging capability. Recently, our group has demonstrated that a digital micromirror device (DMD) can be exploited for fast and precise control of illumination beams for ODT. In this work, we systematically study the precision and stability of the ODT system equipped with a DMD and present measurements of 3-D and 4-D RI maps of various types of live cells including human red blood cells, white blood cells, hepatocytes, and HeLa cells. Furthermore, we also demonstrate the effective visualization of 3-D RI maps of live cells utilizing the measured information about the values and gradient of RI tomograms.

Nanoscale Fresnel coherent diffraction imaging tomography using ptychography.

PubMed

Peterson, I; Abbey, B; Putkunz, C T; Vine, D J; van Riessen, G A; Cadenazzi, G A; Balaur, E; Ryan, R; Quiney, H M; McNulty, I; Peele, A G; Nugent, K A

2012-10-22

We demonstrate Fresnel Coherent Diffractive Imaging (FCDI) tomography in the X-ray regime. The method uses an incident X-ray illumination with known curvature in combination with ptychography to overcome existing problems in diffraction imaging. The resulting tomographic reconstruction represents a 3D map of the specimen's complex refractive index at nano-scale resolution. We use this technique to image a lithographically fabricated glass capillary, in which features down to 70nm are clearly resolved.

Crystallographic Orientation Relationships (CORs) between rutile inclusions and garnet hosts: towards using COR frequencies as a petrogenetic indicator

NASA Astrophysics Data System (ADS)

Griffiths, Thomas; Habler, Gerlinde; Schantl, Philip; Abart, Rainer

2017-04-01

Crystallographic orientation relationships (CORs) between crystalline inclusions and their hosts are commonly used to support particular inclusion origins, but often interpretations are based on a small fraction of all inclusions in a system. The electron backscatter diffraction (EBSD) method allows collection of large COR datasets more quickly than other methods while maintaining high spatial resolution. Large datasets allow analysis of the relative frequencies of different CORs, and identification of 'statistical CORs', where certain limited degrees of freedom exist in the orientation relationship between two neighbour crystals (Griffiths et al. 2016). Statistical CORs exist in addition to completely fixed 'specific' CORs (previously the only type of COR considered). We present a comparison of three EBSD single point datasets (all N > 200 inclusions) of rutile inclusions in garnet hosts, covering three rock systems, each with a different geological history: 1) magmatic garnet in pegmatite from the Koralpe complex, Eastern Alps, formed at temperatures > 600°C and low pressures; 2) granulite facies garnet rims on ultra-high-pressure garnets from the Kimi complex, Rhodope Massif; and 3) a Moldanubian granulite from the southeastern Bohemian Massif, equilibrated at peak conditions of 1050°C and 1.6 GPa. The present study is unique because all datasets have been analysed using the same catalogue of potential CORs, therefore relative frequencies and other COR properties can be meaningfully compared. In every dataset > 94% of the inclusions analysed exhibit one of the CORs tested for. Certain CORs are consistently among the most common in all datasets. However, the relative abundances of these common CORs show large variations between datasets (varying from 8 to 42 % relative abundance in one case). Other CORs are consistently uncommon but nonetheless present in every dataset. Lastly, there are some CORs that are common in one of the datasets and rare in the remainder. These patterns suggest competing influences on relative COR frequencies. Certain CORs seem consistently favourable, perhaps pointing to very stable low energy configurations, whereas some CORs are favoured in only one system, perhaps due to particulars of the formation mechanism, kinetics or conditions. Variations in COR frequencies between datasets seem to correlate with the conditions of host-inclusion system evolution. The two datasets from granulite-facies metamorphic samples show more similarities to each other than to the pegmatite dataset, and the sample inferred to have experienced the highest temperatures (Moldanubian granulite) shows the lowest diversity of CORs, low frequencies of statistical CORs and the highest frequency of specific CORs. These results provide evidence that petrological information is being encoded in COR distributions. They make a strong case for further studies of the factors influencing COR development and for measurements of COR distributions in other systems and between different phases. Griffiths, T.A., Habler, G., Abart, R. (2016): Crystallographic orientation relationships in host-inclusion systems: New insights from large EBSD data sets. Amer. Miner., 101, 690-705.

Mapping the continuous reciprocal space intensity distribution of X-ray serial crystallography.

PubMed

Yefanov, Oleksandr; Gati, Cornelius; Bourenkov, Gleb; Kirian, Richard A; White, Thomas A; Spence, John C H; Chapman, Henry N; Barty, Anton

2014-07-17

Serial crystallography using X-ray free-electron lasers enables the collection of tens of thousands of measurements from an equal number of individual crystals, each of which can be smaller than 1 µm in size. This manuscript describes an alternative way of handling diffraction data recorded by serial femtosecond crystallography, by mapping the diffracted intensities into three-dimensional reciprocal space rather than integrating each image in two dimensions as in the classical approach. We call this procedure 'three-dimensional merging'. This procedure retains information about asymmetry in Bragg peaks and diffracted intensities between Bragg spots. This intensity distribution can be used to extract reflection intensities for structure determination and opens up novel avenues for post-refinement, while observed intensity between Bragg peaks and peak asymmetry are of potential use in novel direct phasing strategies.

Stress in recrystallized quartz by electron backscatter diffraction mapping

NASA Astrophysics Data System (ADS)

Llana-Fúnez, S.

2017-07-01

The long-term state of stress at middle and lower crustal depths can be estimated through the study of the microstructure of exhumed rocks from active and/or ancient shear zones. Constitutive equations for deformation mechanisms in experimentally deformed rocks relate differential stress to the size of recrystallized grains. Cross et al. (2017) take advantage of electron backscatter diffraction mapping to systematically separate new recrystallized grains from host grains on the basis of the measurable lattice distorsion within the grains. They produce the first calibrated piezometer for quartz with this technique, reproducing within error a previous calibration based on optical microscopy.

Cyclic Ductile-Brittle Deformation during Temperature Decrease in Quartz-Rich Mylonites: Insights from the Calamita Schists (Elba Island, Italy)

NASA Astrophysics Data System (ADS)

Papeschi, S.; Menegon, L. M.; Musumeci, G.

2017-12-01

The Calamita Schists are a metamorphic complex that experienced transient (< 1 Ma) upper Miocene HT/LP metamorphism related to the emplacement of the Porto Azzurro pluton at P<0.2 GPa. HT/LP metamorphism was coeval with regional scale contractional tectonics leading to the development of meter to decameter ductile east-verging high-strain domains marked by mylonitic fabric overprinted by non-Andersonian brittle faults. In order to investigate the switch in deformation mechanism during temperature decrease at constant pressure (P<0.2 GPa), a sample of mylonitic quartzite with S-C' fabric was examined by Electron Backscatter Diffraction (EBSD), optical microscopy and Scanning Electron Microscope (SEM). Mylonitic fabric is marked by synkinematic biotite + cordierite + andalusite + K-feldspar assemblage, which is progressively replaced by retrograde white mica + chlorite. Quartz microfabric is defined by coarse-grained (100-900 µm) quartz porphyroclasts wrapped by ribbons of dynamically recrystallized finer grains ( 50 µm) showing a strong CPO. This fabric is cross cut by conjugate and synthetic C'-shear bands localized in porphyroclasts and marked by recrystallized fine grains (5-50 µm). EBSD data indicate that prism was the dominant slip system during crystal plastic deformation and dynamic recrystallization in the polycrystalline ribbons. Subsequently, brittle deformation localized along intracrystalline bands (both in conjugate sets and parallel to C' shear bands) within quartz porphyroclasts. The bands evolved in localized cataclastic micro-shear zones and in shear fractures, which localized fluid infiltration and healing by solution precipitation. The quartz new grains filling the bands are preferentially oriented with their c-axis parallel to the shear band boundary. This work highlights that deformation in the Calamita Schists switched over time from high-temperature dynamic recrystallization, accommodated by prism slip to low grade brittle-ductile processes. At the brittle-ductile transition strain partitioning was controlled by grain size and fluid penetration and was characterized by cyclical ductile-brittle mechanisms. In particular brittle failure localized in coarse-grains acted as the precursor for ductile C' shear bands.

Phase identification in boron-containing powder metallurgy steel using EBSD in combination with EPMA

DOE Office of Scientific and Technical Information (OSTI.GOV)

Wu, Ming-Wei, E-mail: mwwu@ntut.edu.tw; Cai, Wen-Zhang

2016-03-15

Boron (B) is extensively used to induce liquid phase sintering (LPS) in powder metallurgy (PM) steels and thereby increase the densification. The alloying elements in B-containing PM steels affect the boride phase, stability of the boride, the temperature of liquid formation, and the progress of LPS. However, the boride phase has not been systematically identified yet. The main objective of this study was to clarify the influences of alloying elements, including C, Cr, and Ni, on the boride phases using electron backscatter diffraction (EBSD) in combination with electron probe microanalysis (EPMA). Network structures consisting of ferrite, Fe{sub 2}B boride, andmore » Fe{sub 3}C carbide were extensively observed in the Fe–0.4B–0.5C steel. The portions of Fe{sub 2}B were sufficiently larger than those of Fe{sub 3}C, and Fe{sub 3}C was mostly distributed at the interfaces between ferrite and Fe{sub 2}B. Adding 1.5 wt.% Cr or 1.8 wt.% Ni to Fe–0.4B–0.5C steel completely changes the Fe{sub 2}B and Fe{sub 3}C phases to a M{sub 3}(B,C) phase, where M represents the metallic elements, including Fe, Cr, Mo, and Ni. Furthermore, Cr, Mo, B, and C atoms tend to concentrate on the M{sub 3}(B,C) phase, but Ni atoms do not. - Highlights: • Network structures consisting of ferrite, Fe{sub 2}B boride, and Fe{sub 3}C carbide were extensively observed in the Fe–0.4B–0.5C steel. • Adding 1.5 wt.% Cr or 1.8 wt.% Ni to Fe–0.4B–0.5C steel completely transforms the Fe{sub 2}B and Fe{sub 3}C phases to a M{sub 3}(B,C) phase. • Cr, Mo, B, and C atoms tend to concentrate on the M{sub 3}(B,C) phase, but Ni atoms do not.« less

Study on the Toughness of X100 Pipeline Steel Heat Affected Zone

NASA Astrophysics Data System (ADS)

Li, Xueda; Shang, Chengjia; Ma, Xiaoping; Subramanian, S. V.

Microstructure-property correlation of heat affected zone (HAZ) in X100 longitudinal submerged arc welding (LSAW) real weld joint was studied in this paper. Coarse grained (CG) HAZ and intercritically reheated coarse grained (ICCG) HAZ were characterized by optical microscope (OM), electron backscattered diffraction (EBSD). The microstructure of CGHAZ is mostly composed of granular bainite with low density of high angle boundaries (HAB). Prior austenite grain size is 80μm. In ICCGHAZ, coarse prior austenite grains were decorated by coarse necklacing martensite-austenite (M-A) constituents. Different layers were observed within M-A constituent, which may be martensite and austenite layers. Charpy absorbed energy of two different HAZ regions (ICCGHAZ containing and non-containing regions) was recorded using instrumental Charpy impact test machine. The results showed that the existence of ICCGHAZ resulted in the sharp drop of Charpy absorbed energy from 180J to 50J, while the existence of only CGHAZ could still lead to good toughness. The fracture surface was 60% brittle in the absence of ICCGHAZ, and 100% brittle in the presence of ICCGHAZ in the impact tested samples. The underlying reason is the microstructure of ICCGHAZ consisted of granular bainite and upper bainite with necklace-type M-A constituent along the grain boundaries. Cleavage fracture initiated from M-A constituent, either through cracking of M-A or debonding from the matrix, was observed at the fracture surface of ICCGHAZ. The presence of necklace type M-A constituent in ICCGHAZ notably increases the susceptibility of cleavage microcrack nucleation. Furthermore, the study of secondary microcracks beneath the CGHAZ and the ICCGHAZ through EBSD suggested that the fracture mechanism changes from nucleation-controlled in the CGHAZ to propagation-controlled in the ICCGHAZ because of the presence of necklace-type M-A constituent in the ICCGHAZ region. Both fracture mechanism contribute to the poor toughness of the sample contained ICCGHAZ. In conclusion, big prior austenite grains with low density of HAB plus coarse necklacing M-A products along grain boundary is the dominant factor resulting in low toughness.

Thermal and collisional history of Tishomingo iron meteorite: More evidence for early disruption of differentiated planetesimals

NASA Astrophysics Data System (ADS)

Yang, Jijin; Goldstein, Joseph I.; Scott, Edward R. D.; Michael, Joseph R.; Kotula, Paul G.; Grimberg, Ansgar; Leya, Ingo

2014-01-01

Tishomingo is a chemically and structurally unique iron with 32.5 wt.% Ni that contains 20% residual taenite and 80% martensite plates, which formed on cooling to between -75 and -200 °C, probably the lowest temperature recorded by any meteorite. Our studies using transmission (TEM) and scanning electron microscopy (SEM), X-ray microanalysis (AEM) and electron backscatter diffraction (EBSD) show that martensite plates in Tishomingo formed in a single crystal of taenite and decomposed during reheating forming 10-100 nm taenite particles with ∼50 wt.% Ni, kamacite with ∼4 wt.%Ni, along with martensite or taenite with 32 wt.% Ni. EBSD data and experimental constraints show that Tishomingo was reheated to 320-400 °C for about a year transforming some martensite to kamacite and to taenite particles and some martensite directly to taenite without composition change. Fizzy-textured intergrowths of troilite, kamacite with 2.7 wt.% Ni and 2.6 wt.% Co, and taenite with 56 wt.% Ni and 0.15 wt.% Co formed by localized shock melting. A single impact probably melted the sub-mm sulfides, formed stishovite, and reheated and decomposed the martensite plates. Tishomingo and its near-twin Willow Grove, which has 28 wt.% Ni, differ from IAB-related irons like Santa Catharina and San Cristobal that contain 25-36 wt.% Ni, as they are highly depleted in moderately volatile siderophiles and enriched in Ir and other refractory elements. Tishomingo and Willow Grove therefore resemble IVB irons but are chemically distinct. The absence of cloudy taenite in these two irons shows that they cooled through 250 °C abnormally fast at >0.01 °C/yr. Thus this grouplet, like the IVA and IVB irons, suffered an early impact that disrupted their parent body when it was still hot. Our noble gas data show that Tishomingo was excavated from its parent body about 100 to 200 Myr ago and exposed to cosmic rays as a meteoroid with a radius of ∼50-85 cm.

Microstructure and seismic anisotropy of phyllite from Geumseongri Formation and Munjuri Formation in Korea

NASA Astrophysics Data System (ADS)

Han, S.; Jung, H.

2016-12-01

Mica is a mineral group that shows the strongest seismic anisotropy among the minerals comprising continental crust of the Earth. It is also noteworthy that alignment of mica can strongly affect magnitude and symmetry of seismic anisotropy if a seismic wave passes through a rock composed of mica more than 20-40%. Thus, it is highly necessary to analyze mica-rich rocks to investigate the origin of seismic anisotropy observed in continental crust. In this study, muscovite-quartz phyllites from Geumseongri and Munjuri Formation in Korea were analyzed using Electron Backscattered Diffraction (EBSD) to measure lattice preferred orientation (LPO) of minerals. The samples are mainly composed of muscovite, quartz, albite, chlorite, and biotite with minor calcite and rutile. The EBSD analysis showed that the muscovite [001] axis was strongly aligned normal to the foliation while both [100] and [010] axes were dispersed parallel to the foliation. Chlorite and biotite also exhibited similar LPO except for the chlorite [001] axis in the sample 2619, dispersed normal to the lineation. LPOs of quartz were weak in most samples. The albite (010) pole in the sample 2363M and (001) pole in the sample 2364Q were aligned normal to the foliation. Seismic anisotropy was calculated based on the LPO and modal composition of the specimens. The anisotropy of P-wave (Vp) for quartz was in the range of 4.3 - 9.3% and 3.3 - 6.7% for albite. The maximum shear wave anisotropy (AVs) was in the range of 5.3 - 11.2% for quartz and 3.9 - 5.4% for albite. The Vp anisotropy and maximum AVs anisotropy of mica were in the range of 19.3 - 53.4% and 11.6 - 62.9%, respectively, which are much larger than those of other minerals. As a result, The Vp and maximum AVs anisotropy for whole rock were in the range of 11.8 - 44% and 11.6 - 51.8%, respectively. These results show that modal composition and alignment of mica mainly control the magnitude and symmetry of seismic anisotropy.

Improved twin detection via tracking of individual Kikuchi band intensity of EBSD patterns.

PubMed

Rampton, Travis M; Wright, Stuart I; Miles, Michael P; Homer, Eric R; Wagoner, Robert H; Fullwood, David T

2018-02-01

Twin detection via EBSD can be particularly challenging due to the fine scale of certain twin types - for example, compression and double twins in Mg. Even when a grid of sufficient resolution is chosen to ensure scan points within the twins, the interaction volume of the electron beam often encapsulates a region that contains both the parent grain and the twin, confusing the twin identification process. The degradation of the EBSD pattern results in a lower image quality metric, which has long been used to imply potential twins. However, not all bands within the pattern are degraded equally. This paper exploits the fact that parent and twin lattices share common planes that lead to the quality of the associated bands not degrading; i.e. common planes that exist in both grains lead to bands of consistent intensity for scan points adjacent to twin boundaries. Hence, twin boundaries in a microstructure can be recognized, even when they are associated with thin twins. Proof of concept was performed on known twins in Inconel 600, Tantalum, and Magnesium AZ31. This method was then used to search for undetected twins in a Mg AZ31 structure, revealing nearly double the number of twins compared with those initially detected by standard procedures. Copyright © 2017 Elsevier B.V. All rights reserved.

Atomic-scale diffractive imaging of sub-cycle electron dynamics in condensed matter

PubMed Central

Yakovlev, Vladislav S.; Stockman, Mark I.; Krausz, Ferenc; Baum, Peter

2015-01-01

For interaction of light with condensed-matter systems, we show with simulations that ultrafast electron and X-ray diffraction can provide a time-dependent record of charge-density maps with sub-cycle and atomic-scale resolutions. Using graphene as an example material, we predict that diffraction can reveal localised atomic-scale origins of optical and electronic phenomena. In particular, we point out nontrivial relations between microscopic electric current and density in undoped graphene. PMID:26412407

Atomic-scale diffractive imaging of sub-cycle electron dynamics in condensed matter

DOE PAGES

Yakovlev, Vladislav S.; Stockman, Mark I.; Krausz, Ferenc; ...

2015-09-28

For interaction of light with condensed-matter systems, we show with simulations that ultrafast electron and X-ray diffraction can provide a time-dependent record of charge-density maps with sub-cycle and atomic-scale resolutions. Using graphene as an example material, we predict that diffraction can reveal localised atomic-scale origins of optical and electronic phenomena. Here, we point out nontrivial relations between microscopic electric current and density in undoped graphene.

Documenting Mica Microstructures in Mylonites of the Cossato-Mergozzo-Brissago Line, Northern Italy

NASA Astrophysics Data System (ADS)

Aslin, Joe; Mariani, Elisabetta; Wheeler, John

2016-04-01

The rheology of the Earth's crust is ultimately a function of the properties of its constituent minerals. Nowhere are the results of applied tectonic stresses within the Earth's crust more evident than along large scale fault zones and shear zones where strains become focussed producing localised deformation and displacement. These dynamic tectonic discontinuities are often dominated by fault rocks and mylonites that contain an abundance of phyllosilicates (such as micas) whose inherent weakness, relative to other silicate phases (Mariani et al. 2006), acts to concentrate deformation along these narrow regions. Experimental studies show that even in rocks where the concentration of weak phases, such as micas, is low, their effect on the strength and fabric of the rock is significant due to processes such as strain-induced interconnectivity (Holyoke & Tullis 2006). Once this interconnectivity has been established, very high strains can be accommodated within very narrow regions, termed shear bands or micro-shear zones. In this study, a combination of optical and scanning electron microscope (SEM) based techniques including electron backscatter diffraction (EBSD) have been used to observe and document features that are indicative of such processes within samples collected from the Cossato-Mergozzo-Brissago (CMB) shear zone in North Western Italy. This tectonic discontinuity is interpreted to be of Permian age and separates the metapelitic schists of the Kinzigite formation of the lower crustal Ivrea-Verbano zone from the mid-crustal schists and amphibolites of the Serie dei Laghi. Despite its present vertical attitude, the CMB line is believed to have formed as a gently inclined, mid-crustal shear zone during the early stages of post-Hercynian crustal stretching (Rutter et al. 2007). This has produced mylonites composed predominantly of quartz, feldspar and abundant phyllosilicates which serve as perfect natural examples on which to study the distribution of micas, their internal structure and the microstructures of other neighbouring phases in order to give insights into the mechanisms of deformation active within micas under conditions of large, predominantly simple shear strain. Future work will include detailed geological mapping of transects across the CMB line as well as the use of quantitative methods including EBSD to identify crystallographic preferred orientations of grains of mica, and other phases with higher strength, in order to better understand the deformation mechanisms of micas and the role they play in strain localisation and deformation within the crust. References Holyoke, C.W.I. & Tullis, J., 2006. Mechanisms of weak phase interconnection and the effects of phase strength contrast on fabric development. Journal of Structural Geology, 28(4), pp.621-640. Mariani, E., Brodie, K.H. & Rutter, E.H., 2006. Experimental deformation of muscovite shear zones at high temperatures under hydrothermal conditions and the strength of phyllosilicate-bearing faults in nature. Journal of Structural Geology, 28, pp.1569-1587. Rutter, E., Brodie, K., James, T. and Burlini, L., 2007. Large-scale folding in the upper part of the Ivrea-Verbano zone, NW Italy. Journal of Structural Geology, 29(1), pp.1-17.

Coherent diffraction imaging: consistency of the assembled three-dimensional distribution.

PubMed

Tegze, Miklós; Bortel, Gábor

2016-07-01

The short pulses of X-ray free-electron lasers can produce diffraction patterns with structural information before radiation damage destroys the particle. From the recorded diffraction patterns the structure of particles or molecules can be determined on the nano- or even atomic scale. In a coherent diffraction imaging experiment thousands of diffraction patterns of identical particles are recorded and assembled into a three-dimensional distribution which is subsequently used to solve the structure of the particle. It is essential to know, but not always obvious, that the assembled three-dimensional reciprocal-space intensity distribution is really consistent with the measured diffraction patterns. This paper shows that, with the use of correlation maps and a single parameter calculated from them, the consistency of the three-dimensional distribution can be reliably validated.

Trace elements in natural azurite pigments found in illuminated manuscript leaves investigated by synchrotron x-ray fluorescence and diffraction mapping

NASA Astrophysics Data System (ADS)

Smieska, Louisa M.; Mullett, Ruth; Ferri, Laurent; Woll, Arthur R.

2017-07-01

We present trace-element and composition analysis of azurite pigments in six illuminated manuscript leaves, dating from the thirteenth to sixteenth century, using synchrotron-based, large-area x-ray fluorescence (SR-XRF) and diffraction (SR-XRD) mapping. SR-XRF mapping reveals several trace elements correlated with azurite, including arsenic, zirconium, antimony, barium, and bismuth, that appear in multiple manuscripts but were not always detected by point XRF. Within some manuscript leaves, variations in the concentration of trace elements associated with azurite coincide with distinct regions of the illuminations, suggesting systematic differences in azurite preparation or purification. Variations of the trace element concentrations in azurite are greater among different manuscript leaves than the variations within each individual leaf, suggesting the possibility that such impurities reflect distinct mineralogical/geologic sources. SR-XRD maps collected simultaneously with the SR-XRF maps confirm the identification of azurite regions and are consistent with impurities found in natural mineral sources of azurite. In general, our results suggest the feasibility of using azurite trace element analysis for provenance studies of illuminated manuscript fragments, and demonstrate the value of XRF mapping in non-destructive determination of trace element concentrations within a single pigment.

X-ray absorption microtomography (microCT) and small beam diffraction mapping of sea urchin teeth.

PubMed

Stock, S R; Barss, J; Dahl, T; Veis, A; Almer, J D

2002-07-01

Two noninvasive X-ray techniques, laboratory X-ray absorption microtomography (microCT) and X-ray diffraction mapping, were used to study teeth of the sea urchin Lytechinus variegatus. MicroCT revealed low attenuation regions at near the tooth's stone part and along the carinar process-central prism boundary; this latter observation appears to be novel. The expected variation of Mg fraction x in the mineral phase (calcite, Ca(1-x)Mg(x)CO(3)) cannot account for all of the linear attenuation coefficient decrease in the two zones: this suggested that soft tissue is localized there. Transmission diffraction mapping (synchrotron X-radiation, 80.8 keV, 0.1 x 0.1mm(2) beam area, 0.1mm translation grid, image plate area detector) simultaneously probed variations in 3-D and showed that the crystal elements of the "T"-shaped tooth were very highly aligned. Diffraction patterns from the keel (adaxial web) and from the abaxial flange (containing primary plates and the stone part) differed markedly. The flange contained two populations of identically oriented crystal elements with lattice parameters corresponding to x=0.13 and x=0.32. The keel produced one set of diffraction spots corresponding to the lower x. The compositions were more or less equivalent to those determined by others for camarodont teeth, and the high Mg phase is expected to be disks of secondary mineral epitaxially related to the underlying primary mineral element. Lattice parameter gradients were not noted in the keel or flange. Taken together, the microCT and diffraction results indicated that there was a band of relatively high protein content, of up to approximately 0.25 volume fraction, in the central part of the flange and paralleling its adaxial and abaxial faces. X-ray microCT and microdiffraction data used in conjunction with protein distribution data will be crucial for understanding the properties of various biocomposites and their mechanical functions.

Microstructural Evolution at Micro/Meso-Scale in an Ultrafine-Grained Pure Aluminum Processed by Equal-Channel Angular Pressing with Subsequent Annealing Treatment.

PubMed

Xu, Jie; Li, Jianwei; Zhu, Xiaocheng; Fan, Guohua; Shan, Debin; Guo, Bin

2015-11-04

Micro-forming with ultrafine-grained (UFG) materials is a promising direction for the fabrication of micro-electro-mechanical systems (MEMS) components due to the improved formability, good surface quality, and excellent mechanical properties it provides. In this paper, micro-compression tests were performed using UFG pure aluminum processed by equal-channel angular pressing (ECAP) with subsequent annealing treatment. Microstructural evolution was investigated by electron back-scattered diffraction (EBSD) and transmission electron microscopy (TEM). The results show that microstructural evolutions during compression tests at the micro/meso-scale in UFG pure Al are absolutely different from the coarse-grained (CG) materials. A lot of low-angle grain boundaries (LAGBs) and recrystallized fine grains are formed inside of the original large grains in CG pure aluminum after micro-compression. By contrast, ultrafine grains are kept with few sub-grain boundaries inside the grains in UFG pure aluminum, which are similar to the original microstructure before micro-compression. The surface roughness and coordinated deformation ability can be signmicrostructure; micro/meso-forming; ultrafine grains; ECAP; aluminumificantly improved with UFG pure aluminum, which demonstrates that the UFG materials have a strong potential application in micro/meso-forming.

Effect of Nb addition on microstructure and corrosion resistance of novel stainless steels fabricated by direct laser metal deposition

NASA Astrophysics Data System (ADS)

Wu, S. Q.; Zhang, C. H.; Zhang, S.; Wang, Q.; Liu, Y.; Abdullah, Adil O.

2018-03-01

The study demonstrated the successful fabrication of novel stainless steels by direct laser metal deposition with the aim of investigating the impact of niobium content (Nb = 0, 0.25, 0.75, 1.25 wt%) on their microstructure and electrochemical properties. The microstructure and phase evolution of the as-built stainless steels were studied using scanning electron microscope (SEM) and electron back-scatter diffraction (EBSD). Corrosion behavior of the samples was evaluated using electrochemical workstation in 3.5 wt% NaCl. Experimental results have shown that the crystal structure of as-built stainless steels was BCC with a small trace of dispersive carbides and FCC phase. Grain refinement was observed with increasing niobium content. Large-angle boundaries were obtained in different Nb-containing samples with distribution from 50° to 60°. An increase in niobium content extremely improved the corrosion resistance of as-built stainless steels and the as-built samples with 1.25 wt% exhibited the best corrosion resistance among the tested samples as indicated by its lowest corrosion rate, which was an order of magnitude lower than that of Nb-free samples.

Microstructure Evolution during Dissimilar Friction Stir Welding of AA7003-T4 and AA6060-T4.

PubMed

Dong, Jialiang; Zhang, Datong; Zhang, Weiwen; Zhang, Wen; Qiu, Cheng

2018-02-27

In this work, the dissimilar joint of AA7003-T4 and 6060-T4 alloy has been produced by friction stir welding (FSW). The microstructure was examined by optical microscope (OM), electron back scattered diffraction (EBSD), transmission electron microscopy (TEM), and the mechanical properties of the joint were investigated. It is demonstrated that sound dissimilar joint can be produced through FSW. In the nugget; precipitations dissolve into the matrix and η' reprecipitate subsequently; and the elongated aluminum grains are replaced by fine and equiaxed grains due to dynamic recrystallization (DRX). In the heat affected zone (HAZ), coarse β' and η precipitates are formed and the aluminum grains are coarser as compared to the base materials. In the thermo-mechanical affected zone (TMAZ), equiaxed and elongated grains coexist due to incomplete DRX. The ultimate tensile strength of the dissimilar joint is 159.2 MPa and its elongation is 10.4%. The weak area exists in the HAZ of 6060 alloy, which is placed in the retreating side during FSW. The correlations between the microstucture and mechanical properties of the dissimilar joint are discussed.

Microstructure Evolution during Dissimilar Friction Stir Welding of AA7003-T4 and AA6060-T4

PubMed Central

Dong, Jialiang; Zhang, Datong; Zhang, Weiwen; Zhang, Wen; Qiu, Cheng

2018-01-01

In this work, the dissimilar joint of AA7003-T4 and 6060-T4 alloy has been produced by friction stir welding (FSW). The microstructure was examined by optical microscope (OM), electron back scattered diffraction (EBSD), transmission electron microscopy (TEM), and the mechanical properties of the joint were investigated. It is demonstrated that sound dissimilar joint can be produced through FSW. In the nugget; precipitations dissolve into the matrix and η′ reprecipitate subsequently; and the elongated aluminum grains are replaced by fine and equiaxed grains due to dynamic recrystallization (DRX). In the heat affected zone (HAZ), coarse β′ and η precipitates are formed and the aluminum grains are coarser as compared to the base materials. In the thermo-mechanical affected zone (TMAZ), equiaxed and elongated grains coexist due to incomplete DRX. The ultimate tensile strength of the dissimilar joint is 159.2 MPa and its elongation is 10.4%. The weak area exists in the HAZ of 6060 alloy, which is placed in the retreating side during FSW. The correlations between the microstucture and mechanical properties of the dissimilar joint are discussed. PMID:29495463

Characterization of Multilayered Multipass Friction Stir Weld on ASTM A572 G50 Steel

DOE PAGES

Lim, Yong Chae; Sanderson, Samuel; Mahoney, Murray; ...

2014-01-01

A multilayered multipass friction stir weld (MM-FSW) on ASTM A572 Grade 50 steel was characterized to understand its potential application for thick-section structures. The 15-mm-thick section was fabricated by stacking up three steel plates and then friction stir welding the plates together in a total of 5 passes. The unique butt/lap joint configuration encountered in the multilayer weld was examined to understand the effect of tool rotation direction on the joint quality especially the formation of hooking defect. Charpy V-notch impact toughness tests showed generally higher impact toughness energy for the stir zone than the base metal with a ductilemore » fracture mode. The microhardness value was measured from 195 to 220 HV in the stir zone, while the base metal showed an average value of 170 HV. The microstructure in the stir zone and the adjacent heat affected zone was quantified using Optical and Scanning Electron Microscopy (SEM) including Electron Backscatter Diffraction (EBSD). The increased toughness and hardness were correlated with the refined microstructure in stir zone, resulting from severe plastic deformation and subsequent dynamic recrystallization during friction stir welding.« less

Effect of heavy tempering on microstructure and yield strength of 28CrMo48VTiB martensitic steel

NASA Astrophysics Data System (ADS)

Sun, Yu; Gu, Shunjie; Wang, Qian; Wang, Huibin; Wang, Qingfeng; Zhang, Fucheng

2018-02-01

The 28CrMo48VTiB martensitic steel for sulfide stress cracking (SSC) resistance oil country tubular goods (OCTG) of C110 grade was thermally processed through quenching at 890 °C and tempering at 600 °C-720 °C for 30-90 min. The microstructures of all samples were characterized using field emission scanning electron microscopy (FESEM), electron backscattering diffraction (EBSD), transmission electron microscopy (TEM) and x-ray diffractometry (XRD). Also, the tensile properties were measured. The results indicated that the yield strength (YS) decreased as both the tempering temperature and duration increased, due to the coarsening of martensitic packet/block/lath structures, the reduction of dislocation density, as well as the increase of both the volume fraction and average diameter of the precipitates. The martensitic lath width was the key microstructural parameter controlling the YS of this heavily-tempered martensitic steel, whereas the corresponding relationship was in accordance with the Langford-Cohen model. Furthermore, the martensitic structure boundary and the solid solution strengthening were the two most significant factors dominating the YS, in comparison with the dislocation and precipitation strengthening.

Twinning in magnesium under dynamic loading

NASA Astrophysics Data System (ADS)

Dixit, Neha; Hazeli, Kavan; Ramesh, Kaliat T.

2015-09-01

Twinning is an important mode of deformation in magnesium (Mg) and its alloys at high strain rates. Twinning in this material leads to important effects such as mechanical anisotropy, texture evolution, tension-compression asymmetry, and sometimes non-Schmid effects. Extension twins in Mg can accommodate significant plastic deformation as they grow, and thus twinning affects the overall rate of plastic deformation. We use an experimental approach to study the deformation twinning mechanism under dynamic loading. We perform normal plate impact recovery experiments (with microsecond pulse durations) on pure polycrystalline Mg specimens. Estimates of average TB velocity under the known impact stress are obtained by characterization of twin sizes and aspect ratios developed within the target during the loading pulse. The measured average TB velocities in our experiments are of the order of several m s-1. These velocities are several orders of magnitude higher than those so far measured in Mg under quasi-static loading conditions. Electron back-scattered diffraction (EBSD) is then used to characterize the nature of the twins and the microstructural evolution. Detailed crystallographic analysis of the twins enables us to understand twin nucleation and growth of twin variants under dynamic loading.

Investigation of Abnormal Grain Growth in a Friction Stir Welded and Spin-Formed Al-Li Alloy 2195 Crew Module

NASA Technical Reports Server (NTRS)

Tayon, Wesley A.; Domack, Marcia S.; Hoffman, Eric K.; Hales, Stephen J.

2013-01-01

In order to improve manufacturing efficiency and reduce structural mass and costs in the production of launch vehicle structures, NASA is pursuing a wide-range of innovative, near-net shape manufacturing technologies. A technology that combines friction stir welding (FSW) and spin-forming has been applied to manufacture a single-piece crew module using Aluminum-Lithium (AL-Li) Alloy 2195. Plate size limitations for Al-Li alloy 2195 require that two plates be FSW together to produce a spin-forming blank of sufficient size to form the crew module. Subsequent forming of the FSW results in abnormal grain growth (AGG) within the weld region upon solution heat treatment (SHT), which detrimentally impacts strength, ductility, and fracture toughness. The current study seeks to identify microstructural factors that contribute to the development of AGG. Electron backscatter diffraction (EBSD) was used to correlate driving forces for AGG, such as stored energy, texture, and grain size distributions, with the propensity for AGG. Additionally, developmental annealing treatments prior to SHT are examined to reduce or eliminate the occurrence of AGG by promoting continuous, or uniform, grain growth

Constitutive Equation and Hot Compression Deformation Behavior of Homogenized Al–7.5Zn–1.5Mg–0.2Cu–0.2Zr Alloy

PubMed Central

He, Jianliang; Zhang, Datong; Zhang, Weiweng; Qiu, Cheng; Zhang, Wen

2017-01-01

The deformation behavior of homogenized Al–7.5Zn–1.5Mg–0.2Cu–0.2Zr alloy has been studied by a set of isothermal hot compression tests, which were carried out over the temperature ranging from 350 °C to 450 °C and the strain rate ranging from 0.001 s−1 to 10 s−1 on Gleeble-3500 thermal simulation machine. The associated microstructure was studied using electron back scattered diffraction (EBSD) and transmission electron microscopy (TEM). The results showed that the flow stress is sensitive to strain rate and deformation temperature. The shape of true stress-strain curves obtained at a low strain rate (≤0.1 s−1) conditions shows the characteristic of dynamic recrystallization (DRX). Two Arrhenius-typed constitutive equation without and with strain compensation were established based on the true stress-strain curves. Constitutive equation with strain compensation has more precise predictability. The main softening mechanism of the studied alloy is dynamic recovery (DRV) accompanied with DRX, particularly at deformation conditions, with low Zener-Holloman parameters. PMID:29057825

A novel ultrafine-grained Fe−22Mn−0.6C TWIP steel with superior strength and ductility

DOE Office of Scientific and Technical Information (OSTI.GOV)

Tian, Y.Z., E-mail: yztian@imr.ac.cn

A fully recrystallized ultrafine-grained (UFG) Fe−22wt.%Mn−0.6wt.%C twinning-induced plasticity (TWIP) steel with mean grain size of 576 nm was fabricated by cold rolling and annealing process. Tensile test showed that this UFG steel possessed high yield strength of 785 MPa, and unprecedented uniform elongation of 48%. The Hall-Petch relationship was verified from the coarse-grained (CG) regime to the ultrafine-grained (UFG) regime. The microstructures at specified tensile strains were characterized by electron backscattered diffraction (EBSD) and transmission electron microscopy (TEM). The microstructures and strain hardening behavior of the UFG TWIP steel were compared with the CG counterpart. The strong strain hardening capabilitymore » of the UFG steel is supposed to be responsible for the high strength and good ductility. - Highlights: • A fully recrystallized Fe−22Mn−0.6C TWIP steel with mean grain size of 576 nm was fabricated. • The ultrafine-grained (UFG) steel exhibits strong strain-hardening capability, excellent strength and ductility. • The Hall-Petch relationship is fitted well from the CG regime to the UFG regime.« less

Welding Behavior of Free Machining Stainless Steel

DOE Office of Scientific and Technical Information (OSTI.GOV)

BROOKS,JOHN A.; ROBINO,CHARLES V.; HEADLEY,THOMAS J.

2000-07-24

The weld solidification and cracking behavior of sulfur bearing free machining austenitic stainless steel was investigated for both gas-tungsten arc (GTA) and pulsed laser beam weld processes. The GTA weld solidification was consistent with those predicted with existing solidification diagrams and the cracking response was controlled primarily by solidification mode. The solidification behavior of the pulsed laser welds was complex, and often contained regions of primary ferrite and primary austenite solidification, although in all cases the welds were found to be completely austenite at room temperature. Electron backscattered diffraction (EBSD) pattern analysis indicated that the nature of the base metalmore » at the time of solidification plays a primary role in initial solidification. The solid state transformation of austenite to ferrite at the fusion zone boundary, and ferrite to austenite on cooling may both be massive in nature. A range of alloy compositions that exhibited good resistance to solidification cracking and was compatible with both welding processes was identified. The compositional range is bounded by laser weldability at lower Cr{sub eq}/Ni{sub eq} ratios and by the GTA weldability at higher ratios. It was found with both processes that the limiting ratios were somewhat dependent upon sulfur content.« less

Influence of friction stir processing on the room temperature fatigue cracking mechanisms of A356 aluminum alloy

DOE Office of Scientific and Technical Information (OSTI.GOV)

Nelaturu, Phalgun; Jana, Saumyadeep; Mishra, Rajiv S.

Here, failure by fatigue is a common problem associated with cast aluminum alloys due to defects like shrinkage porosities, non-metallic inclusions, etc. Friction stir processing (FSP) has recently emerged as an effective technique for local modification of microstructure. This study investigates the fatigue crack initiation and growth mechanisms in cast and FSPed A356 aluminum alloy. Two sets of parameters were used to friction stir the cast alloy resulting in the complete modification the cast microstructure to a wrought microstructure. Both the FSPed microstructures exhibited severe abnormal grain growth (AGG) after heat treatment leading to a multimodal grain size distribution –more » the grain sizes ranging from a few microns to a few millimeters. One of the FSP conditions displayed an excellent improvement in fatigue life by an order of magnitude, while the other condition displayed an unexpectedly large scatter in fatigue lives. Detailed study of the fractured fatigue specimens by electron back scattered diffraction (EBSD) revealed that both, fatigue crack initiation and propagation, were intimately tied to the grain size as well as the grain misorientations in the microstructure.« less

Formation of the ZnFe2O4 phase in an electric arc furnace off-gas treatment system.

PubMed

Suetens, T; Guo, M; Van Acker, K; Blanpain, B

2015-04-28

To better understand the phenomena of ZnFe2O4 spinel formation in electric arc furnace dust, the dust was characterized with particle size analysis, X-ray fluorescence (XRF), electron backscatter diffraction (EBSD), and electron probe micro-analysis (EPMA). Different ZnFe2O4 formation reaction extents were observed for iron oxide particles with different particle sizes. ZnO particles were present as both individual particles and aggregated on the surface of larger particles. Also, the slag particles found in the off-gas were shown not to react with the zinc vapor. After confirming the presence of a ZnFe2O4 formation reaction, the thermodynamic feasibility of in-process separation - a new electric arc furnace dust treatment technology - was reevaluated. The large air intake and the presence of iron oxide particles in the off-gas were included into the thermodynamic calculations. The formation of the stable ZnFe2O4 spinel phase was shown to be thermodynamically favorable in current electric arc furnace off-gas ducts conditions even before reaching the post combustion chamber. Copyright © 2015 Elsevier B.V. All rights reserved.

Influence of friction stir processing on the room temperature fatigue cracking mechanisms of A356 aluminum alloy

DOE PAGES

Nelaturu, Phalgun; Jana, Saumyadeep; Mishra, Rajiv S.; ...

2018-01-11

Here, failure by fatigue is a common problem associated with cast aluminum alloys due to defects like shrinkage porosities, non-metallic inclusions, etc. Friction stir processing (FSP) has recently emerged as an effective technique for local modification of microstructure. This study investigates the fatigue crack initiation and growth mechanisms in cast and FSPed A356 aluminum alloy. Two sets of parameters were used to friction stir the cast alloy resulting in the complete modification the cast microstructure to a wrought microstructure. Both the FSPed microstructures exhibited severe abnormal grain growth (AGG) after heat treatment leading to a multimodal grain size distribution –more » the grain sizes ranging from a few microns to a few millimeters. One of the FSP conditions displayed an excellent improvement in fatigue life by an order of magnitude, while the other condition displayed an unexpectedly large scatter in fatigue lives. Detailed study of the fractured fatigue specimens by electron back scattered diffraction (EBSD) revealed that both, fatigue crack initiation and propagation, were intimately tied to the grain size as well as the grain misorientations in the microstructure.« less

Damage morphology study of high cycle fatigued as-cast Mg–3.0Nd–0.2Zn–Zr (wt.%) alloy

DOE Office of Scientific and Technical Information (OSTI.GOV)

Yue, Haiyan; Fu, Penghuai, E-mail: fph112sjtu@sjtu.edu.cn; Peng, Liming

Laser scanning confocal microscopy (LSCM) and Electron back-scattered diffraction (EBSD) were applied to the study of surface morphology variation of as-cast Mg–3.0Nd–0.2Zn–Zr (NZ30K) (wt.%) alloy under tension-compression fatigue test at room temperature. Two kinds of typical damage morphologies were observed in fatigued NZ30K alloy: One was parallel lines on basal planes led by the cumulation of basal slips, called persistent slip markings (PSMs), and the other was lens shaped, thicker and in less density, led by the formation of twinning. The surface fatigue damage morphology evolution was analyzed in a statistical way. The influences of stress amplitude and grain orientationmore » on fatigue deformation mechanisms were discussed and the non-uniform deformation among grains and the PSMs, within twinning were described quantitatively. - Highlights: • Fatigue morphology evolution was studied by Laser Scanning Confocal Microscopy. • 3D morphology of persistent slip markings and twins was characterized. • Non-uniform deformation among grains, the PSMs and twins were quantified. • Initiations of fatigue crack were clearly investigated.« less

Laboratory multiple-crystal X-ray topography and reciprocal-space mapping of protein crystals: influence of impurities on crystal perfection

NASA Technical Reports Server (NTRS)

Hu, Z. W.; Thomas, B. R.; Chernov, A. A.

2001-01-01

Double-axis multiple-crystal X-ray topography, rocking-curve measurements and triple-axis reciprocal-space mapping have been combined to characterize protein crystals using a laboratory source. Crystals of lysozyme and lysozyme crystals doped with acetylated lysozyme impurities were examined. It was shown that the incorporation of acetylated lysozyme into crystals of lysozyme induces mosaic domains that are responsible for the broadening and/or splitting of rocking curves and diffraction-space maps along the direction normal to the reciprocal-lattice vector, while the overall elastic lattice strain of the impurity-doped crystals does not appear to be appreciable in high angular resolution reciprocal-space maps. Multiple-crystal monochromatic X-ray topography, which is highly sensitive to lattice distortions, was used to reveal the spatial distribution of mosaic domains in crystals which correlates with the diffraction features in reciprocal space. Discussions of the influence of acetylated lysozyme on crystal perfection are given in terms of our observations.

Laboratory multiple-crystal X-ray topography and reciprocal-space mapping of protein crystals: influence of impurities on crystal perfection.

PubMed

Hu, Z W; Thomas, B R; Chernov, A A

2001-06-01

Double-axis multiple-crystal X-ray topography, rocking-curve measurements and triple-axis reciprocal-space mapping have been combined to characterize protein crystals using a laboratory source. Crystals of lysozyme and lysozyme crystals doped with acetylated lysozyme impurities were examined. It was shown that the incorporation of acetylated lysozyme into crystals of lysozyme induces mosaic domains that are responsible for the broadening and/or splitting of rocking curves and diffraction-space maps along the direction normal to the reciprocal-lattice vector, while the overall elastic lattice strain of the impurity-doped crystals does not appear to be appreciable in high angular resolution reciprocal-space maps. Multiple-crystal monochromatic X-ray topography, which is highly sensitive to lattice distortions, was used to reveal the spatial distribution of mosaic domains in crystals which correlates with the diffraction features in reciprocal space. Discussions of the influence of acetylated lysozyme on crystal perfection are given in terms of our observations.

DOE Office of Scientific and Technical Information (OSTI.GOV)

Frølich, S.; Leemreize, H.; Jakus, A.

A model sample consisting of two different hydroxyapatite (hAp) powders was used as a bone phantom to investigate the extent to which X-ray diffraction tomography could map differences in hAp lattice constants and crystallite size. The diffraction data were collected at beamline 1-ID, the Advanced Photon Source, using monochromatic 65 keV X-radiation, a 25 × 25 µm pinhole beam and translation/rotation data collection. The diffraction pattern was reconstructed for each volume element (voxel) in the sample, and Rietveld refinement was used to determine the hAp lattice constants. The crystallite size for each voxel was also determined from the 00.2 hApmore » diffraction peak width. The results clearly show that differences between hAp powders could be measured with diffraction tomography.« less

Three-dimensional distribution of polymorphs and magnesium in a calcified underwater attachment system by diffraction tomography

PubMed Central

Leemreize, Hanna; Almer, Jonathan D.; Stock, Stuart R.; Birkedal, Henrik

2013-01-01

Biological materials display complicated three-dimensional hierarchical structures. Determining these structures is essential in understanding the link between material design and properties. Herein, we show how diffraction tomography can be used to determine the relative placement of the calcium carbonate polymorphs calcite and aragonite in the highly mineralized holdfast system of the bivalve Anomia simplex. In addition to high fidelity and non-destructive mapping of polymorphs, we use detailed analysis of X-ray diffraction peak positions in reconstructed powder diffraction data to determine the local degree of Mg substitution in the calcite phase. These data show how diffraction tomography can provide detailed multi-length scale information on complex materials in general and of biomineralized tissues in particular. PMID:23804437

An Excel Spreadsheet for a One-Dimensional Fourier Map in X-ray Crystallography

ERIC Educational Resources Information Center

Clegg, William

2004-01-01

The teaching of crystal structure determination with single-crystal X-ray diffraction at undergraduate level faces numerous challenges. Single-crystal X-ray diffraction is used in a vast range of chemical research projects and forms the basis for a high proportion of structural results that are presented to high-school, undergraduate, and graduate…

Impact-Induced Chondrule Deformation and Aqueous Alteration of CM2 Murchison

NASA Technical Reports Server (NTRS)

Hanna, R. D.; Zolensky, M.; Ketcham, R. A.; Behr, W. M.; Martinez, J. E.

2014-01-01

Deformed chondrules in CM2 Murchison have been found to define a prominent foliation [1,2] and lineation [3] in 3D using X-ray computed tomography (XCT). It has been hypothesized that chondrules in foliated chondrites deform by "squeezing" into surrounding pore space [4,5], a process that also likely removes primary porosity [6]. However, shock stage classification based on olivine extinction in Murchison is consistently low (S1-S2) [4-5,7] implying that significant intracrystalline plastic deformation of olivine has not occurred. One objective of our study is therefore to determine the microstructural mechanisms and phases that are accommodating the impact stress and resulting in relative displacements within the chondrules. Another question regarding impact deformation in Murchison is whether it facilitated aqueous alteration as has been proposed for the CMs which generally show a positive correlation between degree of alteration and petrofabric strength [7,2]. As pointed out by [2], CM Murchison represents a unique counterpoint to this correlation: it has a strong petrofabric but a relatively low degree of aqueous alteration. However, Murchison may not represent an inconsistency to the proposed causal relationship between impact and alteration, if it can be established that the incipient aqueous alteration post-dated chondrule deformation. Methods: Two thin sections from Murchison sample USNM 5487 were cut approximately perpendicular to the foliation and parallel to lineation determined by XCT [1,3] and one section was additionally polished for EBSD. Using a combination of optical petrography, SEM, EDS, and EBSD several chondrules were characterized in detail to: determine phases, find microstructures indicative of strain, document the geometric relationships between grain-scale microstructures and the foliation and lineation direction, and look for textural relationships of alteration minerals (tochilinite and Mg-Fe serpentine) that indicate timing of their formation relative to deformation event(s). Preliminary Results: Deformed chondrules are dominated by forsterite and clinoenstatite with lesser amounts of Fe-Mg serpentine, sulfides, and low calcium pyroxene. Olivine grains are commonly fractured but generally show sharp optical extinction. The pyroxene, in contrast, is not only fractured but also often displays undulose extinction. In addition, the clinoenstatite is frequently twinned but it is unclear whether the twins are the result of mechanical deformation or inversion from protoenstatite [8]. EBSD work is currently ongoing to determine if areas of higher crystallographic strain can be imaged and mapped, and to determine the pyroxene twin orientations. In regards to alteration, we have found evidence for post-deformation formation of tochilinite and Mg-Fe serpentine indicating that aqueous alteration has indeed post-dated the deformation of the chondrules.

Residual Stress Induced Mechanical Property Enhancement in Steel Encapsulated Light Metal Matrix Composites

NASA Astrophysics Data System (ADS)

Fudger, Sean James

Macro hybridized systems consisting of steel encapsulated light metal matrix composites (MMCs) were produced with the goal of creating a low cost/light weight composite system with enhanced mechanical properties. MMCs are frequently incorporated into advanced material systems due to their tailorable material properties. However, they often have insufficient ductility for many structural applications. The macro hybridized systems take advantage of the high strength, modulus, and damage tolerance of steels and high specific stiffness and low density of MMCs while mitigating the high density of steels and the poor ductility of MMCs. Furthermore, a coefficient of thermal expansion (CTE) mismatch induced residual compressive stress method is utilized as a means of improving the ductility of the MMCs and overall efficiency of the macro hybridized systems. Systems consisting of an A36, 304 stainless steel, or NitronicRTM 50 stainless steel shell filled with an Al-SiC, Al-Al2O3, or Mg-B4C MMC are evaluated in this work. Upon cooling from processing temperatures, residual strains are generated due to a CTE mismatch between each of the phases. The resulting systems offer higher specific properties and a more structurally efficient system can be attained. Mechanical testing was performed and improvements in yield stress, ultimate tensile stress, and ductility were observed. However, the combination of these dissimilar materials often results in the formation of intermetallic compounds. In certain loading situations, these typically brittle intermetallic layers can result in degraded performance. X-ray Diffraction (XRD), X-ray Energy Dispersive Spectroscopy (EDS), and Electron Backscatter Diffraction (EBSD) are utilized to characterize the intermetallic layer formation at the interface between the steel and MMC. As the residual stress condition in each phase has a large impact on the mechanical property improvement, accurate quantification of these strains/stresses is paramount. X-ray Diffraction Residual Stress Analysis (XRD-RSA) or Neutron diffraction was performed on numerous systems in multiple steel shell thickness variations. The analysis shows variation in the measured strain and stress results due to outer steel thickness, difference in CTE between materials, and relative position within the composite. Improvements in mechanical properties, namely ductility and yield stress, are a direct result of these measured strains.

Effect of autoclave induced low-temperature degradation on the adhesion energy between yttria-stabilized zirconia veneered with porcelain.

PubMed

Li, Kai Chun; Waddell, J Neil; Prior, David J; Ting, Stephanie; Girvan, Liz; van Vuuren, Ludwig Jansen; Swain, Michael V

2013-11-01

To investigate the effect of autoclave induced low-temperature degradation on the adhesion energy between yttria-stabilized zirconia veneered with porcelain. The strain energy release rate using a four-point bending stable fracture test was evaluated for two different porcelains [leucite containing (VM9) and glass (Zirox) porcelain] veneered to zirconia. Prior to veneering the zirconia had been subjected to 0 (control), 1, 5, 10 and 20 autoclave cycles. The specimens were manufactured to a total bi-layer dimension of 30 mm × 8 mm × 3 mm. Subsequent scanning electron microscopy/energy dispersive spectrometry, electron backscatter diffraction and X-ray diffraction analysis were performed to identify the phase transformation and fracture behavior. The strain energy release rate for debonding of the VM9 specimens were significantly higher (p<0.05) compared to the Zirox specimens across all test groups. Increasing autoclave cycles lowered the strain energy release rate significantly (p<0.05) from 18.67 J/m(2) (control) to the lowest of 12.79 J/m(2) (cycle 10) for only the VM9 specimens. SEM analyses showed predominant cohesive fracture within the porcelain for all cycle groups. XRD analysis of the substrate prior to veneering confirmed a tetragonal to monoclinic phase transformation with increasing the number of autoclave cycles between 5 and 20. The monoclinic phase reverted back to tetragonal phase after undergoing conventional porcelain firing cycles. EBSD data showed significant changes of the grain size distribution between the control and autoclaved specimen (cycle 20). Increasing autoclave cycles only significantly decreased the adhesion of the VM9 layered specimens. In addition, a conventional porcelain firing schedule completely reverted the monoclinic phase back to tetragonal. Copyright © 2013 Academy of Dental Materials. Published by Elsevier Ltd. All rights reserved.

Microstructure and partitioning behavior characteristics in low carbon steels treated by hot-rolling direct quenching and dynamical partitioning processes

DOE Office of Scientific and Technical Information (OSTI.GOV)

Li, Yun-jie; Li, Xiao-lei; Yuan, Guo, E-mail: yuan

2016-11-15

In this work, a new process and composition design are proposed for “quenching and partitioning” or Q&P treatment. Three low carbon steels were treated by hot-rolling direct quenching and dynamical partitioning processes (DQ&P). The effects of proeutectoid ferrite and carbon concentration on microstructure evolution and mechanical properties were investigated. The present work obtained DQ&P prototype steels with good mechanical properties and established a new notion on compositions for Q&P processing. Microstructures were characterized by means of electro probe microanalyzer (EPMA), scanning electron microscopy (SEM), electron backscatter diffraction (EBSD), transmission electron microscopy (TEM) and X-ray diffraction (XRD), especially the morphology andmore » size of retained austenite. Mechanical properties were measured by uniaxial tensile tests. The results indicated that introducing proeutectoid ferrite can increase the volume fraction of retained austenite and thus improve mechanical properties. TEM observation showed that retained austenite included the film-like inter-lath austenite and blocky austenite located in martensite/ferrite interfaces or surrounded by ferrites. It was interesting that when the carbon concentration is as low as ~ 0.078%, the film-like inter-lath untransformed austenite cannot be stabilized to room temperature and almost all of them transformed into twin martensite. The blocky retained austenite strengthened the interfaces and transformed into twin martensite during the tensile deformation process. The PSEs of specimens all exceeded 20 GPa.%. - Highlights: •This study focused on a new process: Q&P process applying dynamical partitioning. •Ferrite can increase the volume fraction of retained austenite. •The film-like austenite and the blocky austenite were observed. •The low carbon steels treated by new process reached PSEs higher than 20 GPa.%.« less

Analysis of WC/Ni-Based Coatings Deposited by Controlled Short-Circuit MIG Welding

NASA Astrophysics Data System (ADS)

Vespa, P.; Pinard, P. T.; Gauvin, R.; Brochu, M.

2012-06-01

This study investigates the recently developed controlled short-circuit metal inert gas (CSC-MIG) welding system for depositing WC/Ni-based claddings on carbon steel substrates. WC/Ni-based coatings deposited by CSC-MIG were analyzed by optical light microscopy and scanning electron microscopy (SEM) equipped with energy dispersive spectroscopy (EDS) and electron backscatter diffraction (EBSD) capabilities. X-ray diffraction (XRD) and hardness measurements of depositions are also reported. The CSC-MIG welding system provides a significant amount of user control over the current waveform during welding and has lower heat input when compared with traditional MIG welding. Heat input for the analyzed coatings ranged from 10.1 to 108.7 J/mm. Metallurgically bonded coatings free from spatter and with 0.75% average porosity were produced. It was found that the detrimental decarburization of the WC particles seen in thermal spray systems does not occur when welding with the CSC-MIG. Precipitation of a reaction layer around the reinforcing phase was identified as WC; the average thickness of which increases from 3.8 to 7.2 μm for the low and high heat input condition, respectively. Precipitation of newly formed WC particles was observed; their size distribution increased from D 50 of 2.4 μm in the low heat input weldment to 6.75 μm in the high heat input weldment. The level of dilution of the reinforcing phase increases significantly with heat input. The hardness of the deposited coatings decreases from 587 HV10 to 410 HV10 when the energy input was increased from 10.1 to 108.7 J/mm.

The Effect of Milling Time on the Microstructural Characteristics and Strengthening Mechanisms of NiMo-SiC Alloys Prepared via Powder Metallurgy.

PubMed

Yang, Chao; Muránsky, Ondrej; Zhu, Hanliang; Thorogood, Gordon J; Avdeev, Maxim; Huang, Hefei; Zhou, Xingtai

2017-04-06

A new generation of alloys, which rely on a combination of various strengthening mechanisms, has been developed for application in molten salt nuclear reactors. In the current study, a battery of dispersion and precipitation-strengthened (DPS) NiMo-based alloys containing varying amounts of SiC (0.5-2.5 wt %) were prepared from Ni-Mo-SiC powder mixture via a mechanical alloying (MA) route followed by spark plasma sintering (SPS) and rapid cooling. Neutron Powder Diffraction (NPD), Electron Back Scattering Diffraction (EBSD), and Transmission Electron Microscopy (TEM) were employed in the characterization of the microstructural properties of these in-house prepared NiMo-SiC DPS alloys. The study showed that uniformly-dispersed SiC particles provide dispersion strengthening, the precipitation of nano-scale Ni₃Si particles provides precipitation strengthening, and the solid-solution of Mo in the Ni matrix provides solid-solution strengthening. It was further shown that the milling time has significant effects on the microstructural characteristics of these alloys. Increased milling time seems to limit the grain growth of the NiMo matrix by producing well-dispersed Mo₂C particles during sintering. The amount of grain boundaries greatly increases the Hall-Petch strengthening, resulting in significantly higher strength in the case of 48-h-milled NiMo-SiC DPS alloys compared with the 8-h-milled alloys. However, it was also shown that the total elongation is considerably reduced in the 48-h-milled NiMo-SiC DPS alloy due to high porosity. The porosity is a result of cold welding of the powder mixture during the extended milling process.

Microstructure characterization of LAE442 magnesium alloy processed by extrusion and ECAP

DOE Office of Scientific and Technical Information (OSTI.GOV)

Minárik, Peter; Král, Robert; Pešička, Josef

2016-02-15

The magnesium alloy LAE442 was processed by extrusion and equal channel angular pressing (ECAP) to achieve ultrafine grained microstructure. Detailed characterization of the microstructure was performed by scanning electron microscope, electron back scattered diffraction (EBSD) and transmission electron microscope. The initial, as-cast, microstructure consisted of large grains of ~ 1 mm. The grain refinement due to the processing by severe plastic deformation led to a decrease of the average grain size to ~ 1.7 μm after the final step of ECAP. A detailed characterization of secondary phases showed the precipitation of Al{sub 11}RE{sub 3}, Al{sub 2}Ca and Al{sub 10}RE{sub 2}Mn{submore » 7} intermetallic phases. X-ray diffraction measurements proved that Li is dissolved within the magnesium matrix in the as-cast condition. Newly formed Al{sub 3}Li phase was observed after ECAP. The texture formation due to the extrusion and ECAP was different from that in the other magnesium alloys due to the activation of non-basal slip systems as a result of the decrease of the c/a ratio. - Highlights: • Combined extrusion and equal channel angular pressing results in significant grain refinement by factor 1000 approximately. • Al{sub 11}RE{sub 3}, Al{sub 2}Ca and Al{sub 10}RE{sub 2}Mn{sub 7} secondary phases are present in the as-cast material while Li was dissolved in the Mg matrix. • Extrusion and ECAP have no effect on the composition of the secondary phases but they influence strongly their distribution. • Texture evolution is affected by decrease of c/a ratio due to the presence of Li and resulting activation of non-basal slip.« less

Electron Beam Welding of IN792 DS: Effects of Pass Speed and PWHT on Microstructure and Hardness.

PubMed

Angella, Giuliano; Barbieri, Giuseppe; Donnini, Riccardo; Montanari, Roberto; Richetta, Maria; Varone, Alessandra

2017-09-05

Electron Beam (EB) welding has been used to realize seams on 2 mm-thick plates of directionally solidified (DS) IN792 superalloy. The first part of this work evidenced the importance of pre-heating the workpiece to avoid the formation of long cracks in the seam. The comparison of different pre-heating temperatures (PHT) and pass speeds ( v ) allowed the identification of optimal process parameters, namely PHT = 300 °C and v = 2.5 m/min. The microstructural features of the melted zone (MZ); the heat affected zone (HAZ), and base material (BM) were investigated by optical microscopy (OM), scanning electron microscopy (SEM), energy dispersion spectroscopy (EDS), electron back-scattered diffraction (EBSD), X-ray diffraction (XRD), and micro-hardness tests. In the as-welded condition; the structure of directionally oriented grains was completely lost in MZ. The γ' phase in MZ consisted of small (20-40 nm) round shaped particles and its total amount depended on both PHT and welding pass speed, whereas in HAZ, it was the same BM. Even if the amount of γ' phase in MZ was lower than that of the as-received material, the nanometric size of the particles induced an increase in hardness. EDS examinations did not show relevant composition changes in the γ' and γ phases. Post-welding heat treatments (PWHT) at 700 and 750 °C for two hours were performed on the best samples. After PWHTs, the amount of the ordered phase increased, and the effect was more pronounced at 750 °C, while the size of γ' particles in MZ remained almost the same. The hardness profiles measured across the joints showed an upward shift, but peak-valley height was a little lower, indicating more homogeneous features in the different zones.

The Effect of Milling Time on the Microstructural Characteristics and Strengthening Mechanisms of NiMo-SiC Alloys Prepared via Powder Metallurgy

PubMed Central

Yang, Chao; Muránsky, Ondrej; Zhu, Hanliang; Thorogood, Gordon J.; Avdeev, Maxim; Huang, Hefei; Zhou, Xingtai

2017-01-01

A new generation of alloys, which rely on a combination of various strengthening mechanisms, has been developed for application in molten salt nuclear reactors. In the current study, a battery of dispersion and precipitation-strengthened (DPS) NiMo-based alloys containing varying amounts of SiC (0.5–2.5 wt %) were prepared from Ni-Mo-SiC powder mixture via a mechanical alloying (MA) route followed by spark plasma sintering (SPS) and rapid cooling. Neutron Powder Diffraction (NPD), Electron Back Scattering Diffraction (EBSD), and Transmission Electron Microscopy (TEM) were employed in the characterization of the microstructural properties of these in-house prepared NiMo-SiC DPS alloys. The study showed that uniformly-dispersed SiC particles provide dispersion strengthening, the precipitation of nano-scale Ni3Si particles provides precipitation strengthening, and the solid-solution of Mo in the Ni matrix provides solid-solution strengthening. It was further shown that the milling time has significant effects on the microstructural characteristics of these alloys. Increased milling time seems to limit the grain growth of the NiMo matrix by producing well-dispersed Mo2C particles during sintering. The amount of grain boundaries greatly increases the Hall–Petch strengthening, resulting in significantly higher strength in the case of 48-h-milled NiMo-SiC DPS alloys compared with the 8-h-milled alloys. However, it was also shown that the total elongation is considerably reduced in the 48-h-milled NiMo-SiC DPS alloy due to high porosity. The porosity is a result of cold welding of the powder mixture during the extended milling process. PMID:28772747

Multiscale phase mapping of LiFePO4-based electrodes by transmission electron microscopy and electron forward scattering diffraction.

PubMed

Robert, Donatien; Douillard, Thierry; Boulineau, Adrien; Brunetti, Guillaume; Nowakowski, Pawel; Venet, Denis; Bayle-Guillemaud, Pascale; Cayron, Cyril

2013-12-23

LiFePO4 and FePO4 phase distributions of entire cross-sectioned electrodes with various Li content are investigated from nanoscale to mesoscale, by transmission electron microscopy and by the new electron forward scattering diffraction technique. The distributions of the fully delithiated (FePO4) or lithiated particles (LiFePO4) are mapped on large fields of view (>100 × 100 μm(2)). Heterogeneities in thin and thick electrodes are highlighted at different scales. At the nanoscale, the statistical analysis of 64 000 particles unambiguously shows that the small particles delithiate first. At the mesoscale, the phase maps reveal a core-shell mechanism at the scale of the agglomerates with a preferential pathway along the electrode porosities. At larger scale, lithiation occurs in thick electrodes "stratum by stratum" from the surface in contact with electrolyte toward the current collector.

Diffraction gratings used as identifying markers

DOEpatents

Deason, Vance A.; Ward, Michael B.

1991-01-01

A finely detailed defraction grating is applied to an object as an identifier or tag which is unambiguous, difficult to duplicate, or remove and transfer to another item, and can be read and compared with prior readings with relative ease. The exact pattern of the defraction grating is mapped by diffraction moire techniques and recorded for comparison with future readings of the same grating.

Transmission Kikuchi diffraction and transmission electron forescatter imaging of electropolished and FIB manufactured TEM specimens

DOE Office of Scientific and Technical Information (OSTI.GOV)

Zieliński, W., E-mail: wiziel@inmat.pw.edu.pl; Płociński, T.; Kurzydłowski, K.J.

2015-06-15

We present a study of the efficiency of the utility of scanning electron microscope (SEM)-based transmission methods for characterizing grain structure in thinned bulk metals. Foils of type 316 stainless steel were prepared by two methods commonly used for transmission electron microscopy — double-jet electropolishing and focused ion beam milling. A customized holder allowed positioning of the foils in a configuration appropriate for both transmission electron forward scatter diffraction, and for transmission imaging by the use of a forescatter detector with two diodes. We found that both crystallographic orientation maps and dark-field transmitted images could be obtained for specimens preparedmore » by either method. However, for both methods, preparation-induced artifacts may affect the quality or accuracy of transmission SEM data, especially those acquired by the use of transmission Kikuchi diffraction. Generally, the quality of orientation data was better for specimens prepared by electropolishing, due to the absence of ion-induced damage. - Highlights: • The transmission imaging and diffraction techniques are emerging in scanning electron microscopy (SEM) as promising new field of materials characterization. • The manuscript titled: “Transmission Kikuchi Diffraction and Transmission Electron Forescatter Imaging of Electropolished and FIB Manufactured TEM Specimens” documents how different specimen thinning procedures can effect efficiency of transmission Kikuchi diffraction and transmission electron forescatter imaging. • The abilities to make precision crystallographic orientation maps and dark-field images in transmission was studied on electropolished versus focus ion beam manufactured TEM specimens. • Depending on the need, electropolished and focused ion beam technique may produce suitable specimens for transmission imaging and diffraction in SEM.« less

Electron transfer in a virtual quantum state of LiBH4 induced by strong optical fields and mapped by femtosecond x-ray diffraction.

PubMed

Stingl, J; Zamponi, F; Freyer, B; Woerner, M; Elsaesser, T; Borgschulte, A

2012-10-05

Transient polarizations connected with a spatial redistribution of electronic charge in a mixed quantum state are induced by optical fields of high amplitude. We determine for the first time the related transient electron density maps, applying femtosecond x-ray powder diffraction as a structure probe. The prototype ionic material LiBH4 driven nonresonantly by an intense sub-40 fs optical pulse displays a large-amplitude fully reversible electron transfer from the BH4(-) anion to the Li+ cation during excitation. Our results establish this mechanism as the source of the strong optical polarization which agrees quantitatively with theoretical estimates.

Synchrotron X-ray studies of the keel of the short-spined sea urchin Lytechinus variegatus: absorption microtomography (microCT) and small beam diffraction mapping.

PubMed

Stock, S R; Barss, J; Dahl, T; Veis, A; Almer, J D; Carlo, F

2003-05-01

In sea urchin teeth, the keel plays an important structural role, and this paper reports results of microstructural characterization of the keel of Lytechinus variegatus using two noninvasive synchrotron x-ray techniques: x-ray absorption microtomography (microCT) and x-ray diffraction mapping. MicroCT with 14 keV x-rays mapped the spatial distribution of mineral at the 1.3 microm level in a millimeter-sized fragment of a mature portion of the keel. Two rows of low absorption channels (i.e., primary channels) slightly less than 10 microm in diameter were found running linearly from the flange to the base of the keel and parallel to its sides. The primary channels paralleled the oral edge of the keel, and the microCT slices revealed a planar secondary channel leading from each primary channel to the side of the keel. The primary and secondary channels were more or less coplanar and may correspond to the soft tissue between plates of the carinar process. Transmission x-ray diffraction with 80.8 keV x-rays and a 0.1 mm beam mapped the distribution of calcite crystal orientations and the composition Ca(1-x)Mg(x)CO(3) of the calcite. Unlike the variable Mg concentration and highly curved prisms found in the keel of Paracentrotus lividus, a constant Mg content (x = 0.13) and relatively little prism curvature was found in the keel of Lytechinus variegatus.

Grazing-incidence X-ray diffraction from a crystal with subsurface defects

DOE Office of Scientific and Technical Information (OSTI.GOV)

Gaevskii, A. Yu., E-mail: transilv@mail.ru; Golentus, I. E.

2015-03-15

The diffraction of X rays incident on a crystal surface under grazing angles under conditions of total external reflection has been investigated. An approach is proposed in which exact solutions to the dynamic problem of grazing-incidence diffraction in an ideal crystal are used as initial functions to calculate the diffuse component of diffraction in a crystal with defects. The diffuse component of diffraction is calculated for a crystal with surface defects of a dilatation-center type. Exact formulas of the continuum theory which take into account the mirror-image forces are used for defect-induced atomic displacements. Scattering intensity maps near Bragg peaksmore » are constructed for different scan modes, and the conditions for detecting primarily the diffuse component are determined. The results of dynamic calculations of grazing-incidence diffraction in defect-containing crystals are compared with calculations in the kinematic approximation.« less

Strain Distribution in a Partially Molten Crust: Insights from the AMS Study of Carlos Chagas Anatexite, ARAÇUAI Belt (se Brazil)

NASA Astrophysics Data System (ADS)

Cavalcante, G.; Silva, M.; Vauchez, A. R.

2012-12-01

Anatectic domains, characterized by abundant migmatites, represent portions of the middle crust that have been partially molten. The Carlos Chagas anatexite is a unit that includes diatexites, metaxites and anatetic, peraluminous granites. It is localized in eastern domain of the Araçuaí Belt, which was formed during the amalgamation of West Gondwana by the collision of the Sao Francisco and Congo cratons. This orogenic segment underwent a synkinematic high temperature (>750oC)-low pressure (~ 6MPa) metamorphism that causes widespread partial melting of the middle crust. The Carlos Chagas unit is composed by quartz, feldspar, garnet, biotite, sillimanite, ilmenite, rutile and cordierite. U-Pb data indicates that its crystallization occurred c. a. 574 ~ 3 Ma. The main feature of this migmatite is the presence of a pervasive magmatic foliation, which is marked by the preferential alignment of biotite, alkali feldspars and plagioclase. At the grain scale, quartz displays evidence of interstitial crystallization and few solid-state deformation fabrics are observed. We used anisotropy of magnetic susceptibility (AMS) as a tool for recovering mineral fabric and thus the flow field of the Carlos Chagas anatexite. Magnetic properties of 153 samples were measured. They yield dominantly low values of the bulk magnetic susceptibility (km <360 x 10-6 SI), low anisotropy degrees (1.03 - 1.19), and the mean shape parameter ranges from - 0.3 to 0.8, with oblate ellipsoids (T > 0) being dominantly more frequent than prolates ones. These magnetics characteristics are consistent with biotite being the dominant carrier of the AMS. Magnetic foliations and lineations suggest two main structural patterns. The northern portion of the studied area shows shallowly plunging lineations (02° - 20°) to SE (140°-120°) or NW (340°-300°), while the foliation strikes NW-SE with shallow dips (03°-10°). Local subvertical foliation dips (70°) are due to NE-SW trending transcurrent shear zones. The southern region shows complex magnetic fabric patterns. Magnetic lineation plunges range from 05° to 58°, in varied directions, while the foliation strikes from NW-SE to NE-SW with low to high dips, lacking a statistical preferred orientation. Using electron backscatter diffraction (EBSD) analysis we investigated the correlation of the biotite crystallographic fabrics with the AMS fabric and structural field measurements of the Carlos Chagas anatexite. EBSD data for biotite document a correspondence between the <001> direction of biotite and k3 (as well as macroscopic foliation). In hot orogens such as the orogenic sector studied here, strain localization is not efficient and rocks are deformed homogeneously. Field data, AMS and EBSD studies suggest that, in the anatectic unit as well as in the adjacent units of the Araçuaí belt, the Africa-South America convergence resulted in the development of a complex, 3D strain field in huge volumes of magmatic and anatetic rocks, which hinder a simpler, high-temperature plastic flow regime.

Scanning force microscope for in situ nanofocused X-ray diffraction studies

PubMed Central

Ren, Zhe; Mastropietro, Francesca; Davydok, Anton; Langlais, Simon; Richard, Marie-Ingrid; Furter, Jean-Jacques; Thomas, Olivier; Dupraz, Maxime; Verdier, Marc; Beutier, Guillaume; Boesecke, Peter; Cornelius, Thomas W.

2014-01-01

A compact scanning force microscope has been developed for in situ combination with nanofocused X-ray diffraction techniques at third-generation synchrotron beamlines. Its capabilities are demonstrated on Au nano-islands grown on a sapphire substrate. The new in situ device allows for in situ imaging the sample topography and the crystallinity by recording simultaneously an atomic force microscope (AFM) image and a scanning X-ray diffraction map of the same area. Moreover, a selected Au island can be mechanically deformed using the AFM tip while monitoring the deformation of the atomic lattice by nanofocused X-ray diffraction. This in situ approach gives access to the mechanical behavior of nanomaterials. PMID:25178002

Insights into photosystem II from isomorphous difference Fourier maps of femtosecond X-ray diffraction data and quantum mechanics/molecular mechanics structural models

DOE PAGES

Wang, Jimin; Askerka, Mikhail; Brudvig, Gary W.; ...

2017-01-12

Understanding structure–function relations in photosystem II (PSII) is important for the development of biomimetic photocatalytic systems. X-ray crystallography, computational modeling, and spectroscopy have played central roles in elucidating the structure and function of PSII. Recent breakthroughs in femtosecond X-ray crystallography offer the possibility of collecting diffraction data from the X-ray free electron laser (XFEL) before radiation damage of the sample, thereby overcoming the main challenge of conventional X-ray diffraction methods. However, the interpretation of XFEL data from PSII intermediates is challenging because of the issues regarding data-processing, uncertainty on the precise positions of light oxygen atoms next to heavy metalmore » centers, and different kinetics of the S-state transition in microcrystals compared to solution. Lastly, we summarize recent advances and outstanding challenges in PSII structure–function determination with emphasis on the implementation of quantum mechanics/molecular mechanics techniques combined with isomorphous difference Fourier maps, direct methods, and high-resolution spectroscopy.« less

Insights into Photosystem II from Isomorphous Difference Fourier Maps of Femtosecond X-ray Diffraction Data and Quantum Mechanics/Molecular Mechanics Structural Models.

PubMed

Wang, Jimin; Askerka, Mikhail; Brudvig, Gary W; Batista, Victor S

2017-02-10

Understanding structure-function relations in photosystem II (PSII) is important for the development of biomimetic photocatalytic systems. X-ray crystallography, computational modeling, and spectroscopy have played central roles in elucidating the structure and function of PSII. Recent breakthroughs in femtosecond X-ray crystallography offer the possibility of collecting diffraction data from the X-ray free electron laser (XFEL) before radiation damage of the sample, thereby overcoming the main challenge of conventional X-ray diffraction methods. However, the interpretation of XFEL data from PSII intermediates is challenging because of the issues regarding data-processing, uncertainty on the precise positions of light oxygen atoms next to heavy metal centers, and different kinetics of the S-state transition in microcrystals compared to solution. Here, we summarize recent advances and outstanding challenges in PSII structure-function determination with emphasis on the implementation of quantum mechanics/molecular mechanics techniques combined with isomorphous difference Fourier maps, direct methods, and high-resolution spectroscopy.

Insights into photosystem II from isomorphous difference Fourier maps of femtosecond X-ray diffraction data and quantum mechanics/molecular mechanics structural models

DOE Office of Scientific and Technical Information (OSTI.GOV)

Wang, Jimin; Askerka, Mikhail; Brudvig, Gary W.

Understanding structure–function relations in photosystem II (PSII) is important for the development of biomimetic photocatalytic systems. X-ray crystallography, computational modeling, and spectroscopy have played central roles in elucidating the structure and function of PSII. Recent breakthroughs in femtosecond X-ray crystallography offer the possibility of collecting diffraction data from the X-ray free electron laser (XFEL) before radiation damage of the sample, thereby overcoming the main challenge of conventional X-ray diffraction methods. However, the interpretation of XFEL data from PSII intermediates is challenging because of the issues regarding data-processing, uncertainty on the precise positions of light oxygen atoms next to heavy metalmore » centers, and different kinetics of the S-state transition in microcrystals compared to solution. Lastly, we summarize recent advances and outstanding challenges in PSII structure–function determination with emphasis on the implementation of quantum mechanics/molecular mechanics techniques combined with isomorphous difference Fourier maps, direct methods, and high-resolution spectroscopy.« less

Late Cretaceous extensional denudation along a marble detachment fault zone in the Kırşehir massif near Kaman, central Turkey

NASA Astrophysics Data System (ADS)

Lefebvre, Côme; Barnhoorn, Auke; van Hinsbergen, Douwe J. J.; Kaymakci, Nuretdin; Vissers, Reinoud L. M.

2011-08-01

In the Central Anatolian Crystalline Complex (CACC), 100 km scale metamorphic domains were exhumed in a context of north-south plate convergence during late Cretaceous to Cenozoic times. The timing, kinematics and mechanisms of exhumation have been the focus of previous studies in the southern Niğde Massif. In this study, we investigate the unexplored northern area regarding the tectonic features preserved on the edges of the Kırşehir Massif, based on detailed field-mapping in the Kaman area where high-grade metasediments, non-metamorphic ophiolites and monzonitic plutons are locally exposed together. Close to the contact with the ophiolites, west-dipping foliated marble-rich rocks display mylonites and discrete protomylonites with normal shear senses indicating a general top-to-the W-NW direction. Both of these structures have been brittlely overprinted into cataclastic corridors parallel to the main foliation. The mylonite series and superimposed brittle structures together define the Kaman fault zone. The study of the evolution of calcite deformation fabrics along an EW section supported by Electron Back Scattered Diffraction measurements (EBSD) on representative fabrics indicates that the Kaman fault zone represents an extensional detachment. In Ömerhacılı, in the vicinity of the Baranadağ quartz-monzonite, the metamorphic sequence shows static annealing of the calcite mylonitic fabrics. This evidence suggests that intrusion took place at shallow depth (˜10 km) into an already exhuming metamorphic sequence. As a consequence for the Kaman area, buried metasediments have been rapidly exhumed between 84 and 74 Ma (˜1 km/Ma) where exhumation along a detachment zone, displaying a top-to-the W-NW shear motion, took place in the mid to upper crust prior to magmatic intrusion in the late Campanian. As the intrusion cut through the detachment fault, the main shearing deformation ceased. Brittle tectonics coupled with erosion likely took over during the final unroofing stages at a slower rate (<0.2 km/Ma), until the pertinent rocks reached the Earth's surface in the late Paleocene.

Variation in the Helical Structure of Native Collagen

DTIC Science & Technology

2014-02-24

unsampled molecular transform of the sample (non-crystalline diffraction arising from the helical symmetry), these patterns also contain Bragg peaks...tissues may be treated as analogous to that from a single macromolecular crystal. Except that it arises from many fibrils within the sample , giving rise...density maps, constructed from experimentally determined phases and observed amplitudes, showed good agreement. The observed diffraction and the simulated

Symposium LL: Nanowires--Synthesis Properties Assembly and Application

DTIC Science & Technology

2010-09-10

dedicated hard x - ray microscopy beamline is operated in partnership with the Advanced Photon Source to provide fluorescence, diffraction, and...characterized by scanning electron microscopy (SEM), transmission electron microscopy (TEM) and X - ray diffraction (XRD) measurements, proving it to be...Investigation of Preferred Growth Direction of GaN Nanorods by Synchrotron X - ray Reciprocal Space Mapping. Yuri Sohn1, Sanghwa Lee1, Chinkyo Kim1 and Dong

Effects of Changing Hot Rolling Direction on Microstructure, Texture and Mechanical Properties of Cu-2.7Be Sheets

NASA Astrophysics Data System (ADS)

Zhu, Daibo; Liu, Chuming; Yu, Haijun; Han, Tan

2018-03-01

A hot rolling scheme (cross-rolling and unidirectional rolling) was adopted to process Cu-2.7Be sheets used as multiplier dynodes in photomultiplier. The effects of changing rolling direction on microstructure, texture and mechanical properties were studied by a combination of XRD, EBSD and TEM. It was found that higher copper-type texture and lower brass texture intensity were obtained in the ultimately cross-rolling (CR) sheet compared with the unidirectional rolling (UR) sheet.The EBSD results indicated that the grain orientation from mainly < {101} > for UR sample turns to random for CR sample. Great enhancements in YS and UTS after unidirectional rolling were attributed to the massive and polygonal γ precipitates. The CR sample exhibited lower anisotropy, because of the increase of S and γ precipitates with spherical and tiny shape.

Surface polishing of niobium for superconducting radio frequency (SRF) cavity applications

DOE Office of Scientific and Technical Information (OSTI.GOV)

Zhao, Liang

2014-08-01

Niobium cavities are important components in modern particle accelerators based on superconducting radio frequency (SRF) technology. The interior of SRF cavities are cleaned and polished in order to produce high accelerating field and low power dissipation on the cavity wall. Current polishing methods, buffered chemical polishing (BCP) and electro-polishing (EP), have their advantages and limitations. We seek to improve current methods and explore laser polishing (LP) as a greener alternative of chemical methods. The topography and removal rate of BCP at different conditions (duration, temperature, sample orientation, flow rate) was studied with optical microscopy, scanning electron microscopy (SEM), and electronmore » backscatter diffraction (EBSD). Differential etching on different crystal orientations is the main contributor to fine grain niobium BCP topography, with gas evolution playing a secondary role. The surface of single crystal and bi-crystal niobium is smooth even after heavy BCP. The topography of fine grain niobium depends on total removal. The removal rate increases with temperature and surface acid flow rate within the rage of 0~20 °C, with chemical reaction being the possible dominate rate control mechanism. Surface flow helps to regulate temperature and avoid gas accumulation on the surface. The effect of surface flow rate on niobium EP was studied with optical microscopy, atomic force microscopy (AFM), and power spectral density (PSD) analysis. Within the range of 0~3.7 cm/s, no significant difference was found on the removal rate and the macro roughness. Possible improvement on the micro roughness with increased surface flow rate was observed. The effect of fluence and pulse accumulation on niobium topography during LP was studied with optical microscopy, SEM, AFM, and PSD analysis. Polishing on micro scale was achieved within fluence range of 0.57~0.90 J/cm2, with pulse accumulation adjusted accordingly. Larger area treatment was proved possible by overlapping laser tracks at proper ratio. Comparison of topography and PSD indicates that LP smooths the surface in a way similar to EP. The optimized LP parameters were applied to different types of niobium surfaces representing different stages in cavity fabrication. LP reduces the sharpness on rough surfaces effectively, while doing no harm to smooth surfaces. Secondary ion mass spectrometer (SIMS) analysis showed that LP reduces the oxide layer slightly and no contamination occurred from LP. EBSD showed no significant change on crystal structure after LP.« less

The habit of crystals in aggregates: five parameter grain boundary characterization of olivine

NASA Astrophysics Data System (ADS)

Marquardt, K.; Rohrer, G. S.; Morales, L. F. G.; De Graef, M.; Farla, R. J.

2016-12-01

There is growing evidence that the presence of interfaces in rocks, including phase and grain boundaries influence macroscopic properties. To model resulting bulk rock properties and ultimately interpret geophysical signals, such as electrical conductivity, knowledge about the relative abundance of specific grain boundaries is needed. To date, neither the anisotropic frequency of appearance of specific grain boundaries nor its dependence on chemical composition is known for rock forming minerals. Here, we report detailed interface characterizations in olivine, the most abundant phase in the upper mantle. To obtain the area distribution of the geometrically varying interfaces, which is among the most fundamental information, we used electron backscatter diffraction (EBSD) to detect the orientations of over 3x104grains corresponding to more than 6000 mm length of grain boundary separating them. Subsequently we used a stereological approach to determine the grain boundary character distribution (GBCD), defined as the relative areas of grain boundaries of different types, distinguished by their five degrees of freedom (Rohrer et al. 2004). We discuss data collected from different olivine aggregates with chemical compositions ranging from Mg2SiO4 forsterite to Mg1.8Fe0.2SiO4 derived from different synthesis methods. We show that standard EBSD indexing as commonly used is sufficient for many applications, but when characterizing grain boundaries higher accuracy and precision is fundamental and provided by the new dictionary indexing approach, where clean up procedures, that can cause artifacts, are superfluous. The grain boundary planes show a preference for low index planes, which is in agreement with observations on other materials (e.g. MgO, TiO2, SrTiO3, MgAl2O4). We find that the principal crystallographic planes have the lowest energies resulting in crystal habits dominated by (001) planes, followed by (010) and (001) planes and that 90°/[001] (100)(010) are the most frequent grain boundaries, for pure forsterite aggregates. However in the absence of any impurities such as Al or Ca on the grain boundaries the (001) planes dominate the crystal habits. Rohrer G. S. et al. (2004) The distribution of internal interfaces in polycrystals. Zeitschrift für Met. 95, 197-214.

Characterization of a bent Laue double-crystal beam-expanding monochromator

DOE PAGES

Martinson, Mercedes; Samadi, Nazanin; Shi, Xianbo; ...

2017-10-19

A bent Laue double-crystal monochromator system has been designed for vertically expanding the X-ray beam at the Canadian Light Source's BioMedical Imaging and Therapy beamlines. Expansion by a factor of 12 has been achieved without deteriorating the transverse coherence of the beam, allowing phase-based imaging techniques to be performed with high flux and a large field of view. However, preliminary studies revealed a lack of uniformity in the beam, presumed to be caused by imperfect bending of the silicon crystal wafers used in the system. Results from finite-element analysis of the system predicted that the second crystal would be mostmore » severely affected and has been shown experimentally. It has been determined that the majority of the distortion occurs in the second crystal and is likely caused by an imperfection in the surface of the bending frame. Here, measurements were then taken to characterize the bending of the crystal using both mechanical and diffraction techniques. In particular, two techniques commonly used to map dislocations in crystal structures have been adapted to map local curvature of the bent crystals. One of these, a variation of Berg–Berrett topography, has been used to quantify the diffraction effects caused by the distortion of the crystal wafer. This technique produces a global mapping of the deviation of the diffraction angle relative to a perfect cylinder. Finally, this information is critical for improving bending and measuring tolerances of imperfections by correlating this mapping to areas of missing intensity in the beam.« less

Characterization of a bent Laue double-crystal beam-expanding monochromator

DOE Office of Scientific and Technical Information (OSTI.GOV)

Martinson, Mercedes; Samadi, Nazanin; Shi, Xianbo

A bent Laue double-crystal monochromator system has been designed for vertically expanding the X-ray beam at the Canadian Light Source's BioMedical Imaging and Therapy beamlines. Expansion by a factor of 12 has been achieved without deteriorating the transverse coherence of the beam, allowing phase-based imaging techniques to be performed with high flux and a large field of view. However, preliminary studies revealed a lack of uniformity in the beam, presumed to be caused by imperfect bending of the silicon crystal wafers used in the system. Results from finite-element analysis of the system predicted that the second crystal would be mostmore » severely affected and has been shown experimentally. It has been determined that the majority of the distortion occurs in the second crystal and is likely caused by an imperfection in the surface of the bending frame. Here, measurements were then taken to characterize the bending of the crystal using both mechanical and diffraction techniques. In particular, two techniques commonly used to map dislocations in crystal structures have been adapted to map local curvature of the bent crystals. One of these, a variation of Berg–Berrett topography, has been used to quantify the diffraction effects caused by the distortion of the crystal wafer. This technique produces a global mapping of the deviation of the diffraction angle relative to a perfect cylinder. Finally, this information is critical for improving bending and measuring tolerances of imperfections by correlating this mapping to areas of missing intensity in the beam.« less

Net shape processing of alnico magnets by additive manufacturing

DOE PAGES

White, Emma Marie Hamilton; Kassen, Aaron Gregory; Simsek, Emrah; ...

2017-06-07

Alternatives to rare earth permanent magnets, such as alnico, will reduce supply instability, increase sustainability, and could decrease the cost of permanent magnets, especially for high temperature applications, such as traction drive motors. Alnico magnets with moderate coercivity, high remanence, and relatively high energy product are conventionally processed by directional solidification and (significant) final machining, contributing to increased costs and additional material waste. Additive manufacturing (AM) is developing as a cost effective method to build net-shape three-dimensional parts with minimal final machining and properties comparable to wrought parts. This work describes initial studies of net-shape fabrication of alnico magnets bymore » AM using a laser engineered net shaping (LENS) system. High pressure gas atomized (HPGA) pre-alloyed powders of two different modified alnico “8” compositions, with high purity and sphericity, were built into cylinders using the LENS process, followed by heat treatment. The magnetic properties showed improvement over their cast and sintered counterparts. The resulting alnico permanent magnets were characterized using scanning electron microscopy (SEM), energy dispersive spectroscopy (EDS), electron backscatter diffraction (EBSD), and hysteresisgraph measurements. Furthermore, these results display the potential for net-shape processing of alnico permanent magnets for use in next generation traction drive motors and other applications requiring high temperatures and/or complex engineered part geometries.« less

Effect of Intercritical Annealing on Microstructural Evolution and Properties of Quenched & Partitioned (Q&P) Steels

NASA Astrophysics Data System (ADS)

Wu, Riming; Jin, Xuejun; Wang, Chenglin; Wang, Li

2016-04-01

Transformation of metastable austenite into martensite in novel quenched & partitioned (Q&P) steels improves sheet formability, allowing this class of high-strength steels to be used for automotive structural components. The current work studies the microstructural evolution by varying intercritical annealing time ( t a), as well as its influence on the martensite-austenite constituent and mechanical properties of Q&P steels. As the t a was prolonged, the morphology of retained austenite progressively transformed from block to a mixture of block and film, and finally changed to totally film. Based on electron back-scatter diffraction (EBSD) measurements and uniaxial tensile response, the holding time of 600 s at 760 °C was determined to produce the best results in terms of highest volume fraction of retained austenite ( f γ = 15.8%) and largest strain (26.8%) at the ultimate tensile strength (892 MPa). This difference in work-hardening behavior corresponds directly to the transformation rate of retained austenite with different morphology. The slower rate of transformation of filmy austenite allowed for work hardening to persist at high strains where the transformation effect had already been exhausted in the blocky one. There is great potential for properties improvement through adjustment of metastability of retained austenite.

Exploring the relative contribution of mineralogy and CPO to the seismic velocity anisotropy of evaporites

NASA Astrophysics Data System (ADS)

Vargas-Meleza, Liliana; Healy, David; Alsop, G. Ian; Timms, Nicholas E.

2015-01-01

We present the influence of mineralogy and microstructure on the seismic velocity anisotropy of evaporites. Bulk elastic properties and seismic velocities are calculated for a suite of 20 natural evaporite samples, which consist mainly of halite, anhydrite, and gypsum. They exhibit strong fabrics as a result of tectonic and diagenetic processes. Sample mineralogy and crystallographic preferred orientation (CPO) were obtained with the electron backscatter diffraction (EBSD) technique and the data used for seismic velocity calculations. Bulk seismic properties for polymineralic evaporites were evaluated with a rock recipe approach. Ultrasonic velocity measurements were also taken on cube shaped samples to assess the contribution of grain-scale shape preferred orientation (SPO) to the total seismic anisotropy. The sample results suggest that CPO is responsible for a significant fraction of the bulk seismic properties, in agreement with observations from previous studies. Results from the rock recipe indicate that increasing modal proportion of anhydrite grains can lead to a greater seismic anisotropy of a halite-dominated rock. Conversely, it can lead to a smaller seismic anisotropy degree of a gypsum-dominated rock until an estimated threshold proportion after which anisotropy increases again. The difference between the predicted anisotropy due to CPO and the anisotropy measured with ultrasonic velocities is attributed to the SPO and grain boundary effects in these evaporites.

Magnetostrictive performance of additively manufactured CoFe rods using the LENS (TM) system

DOE Office of Scientific and Technical Information (OSTI.GOV)

Jones, Nicholas J.; Yoo, Jin-Hyeong; Ott, Ryan T.

Magnetostrictive materials exhibit a strain in the presence of a variable magnetic field. While they normally require large, highly oriented crystallographic grains for high strain values, metal additive manufacturing (3D printing) may be able to produce highly textured polycrystalline rods, with properties comparable to those manufactured using the more demanding free standing zone melting (FSZM) technique. Rods of Co 75.8Fe 24.2 and Co 63.7Fe 36.3 have been fabricated using the Laser engineered net shaping (LENS TM) system to evaluate the performance of additively manufactured magnetic and magnetostrictive materials. The 76% Co sample showed an average magnetostriction (λ) of 86 ppmmore » at a stress of 124 MPa; in contrast, the 64% Co sample showed only 27 ppm at the same stress. For direct comparison, a Co 67Fe 33 single crystal disk, also measured as part of this study, exhibited a magnetostriction value of 131 and 91 microstrain in the [100] and [111] directions, respectively, with a calculated polycrystalline value (λ s) of 107 microstrain. Electron back scattered diffraction (EBSD) has been used to qualitatively link the performance with crystallographic orientation and phase information, showing only the BCC phase in the 76% Co sample, but three different phases (BCC, FCC, and HCP) in the 64% Co sample.« less

EBSDinterp 1.0: A MATLAB® Program to Perform Microstructurally Constrained Interpolation of EBSD Data.

PubMed

Pearce, Mark A

2015-08-01

EBSDinterp is a graphic user interface (GUI)-based MATLAB® program to perform microstructurally constrained interpolation of nonindexed electron backscatter diffraction data points. The area available for interpolation is restricted using variations in pattern quality or band contrast (BC). Areas of low BC are not available for interpolation, and therefore cannot be erroneously filled by adjacent grains "growing" into them. Points with the most indexed neighbors are interpolated first and the required number of neighbors is reduced with each successive round until a minimum number of neighbors is reached. Further iterations allow more data points to be filled by reducing the BC threshold. This method ensures that the best quality points (those with high BC and most neighbors) are interpolated first, and that the interpolation is restricted to grain interiors before adjacent grains are grown together to produce a complete microstructure. The algorithm is implemented through a GUI, taking advantage of MATLAB®'s parallel processing toolbox to perform the interpolations rapidly so that a variety of parameters can be tested to ensure that the final microstructures are robust and artifact-free. The software is freely available through the CSIRO Data Access Portal (doi:10.4225/08/5510090C6E620) as both a compiled Windows executable and as source code.

Magnetostrictive performance of additively manufactured CoFe rods using the LENSTM system

NASA Astrophysics Data System (ADS)

Jones, Nicholas J.; Yoo, Jin-Hyeong; Ott, Ryan T.; Lambert, Paul K.; Petculescu, Gabriela; Simsek, Emrah; Schlagel, Deborah; Lograsso, Thomas A.

2018-05-01

Magnetostrictive materials exhibit a strain in the presence of a variable magnetic field. While they normally require large, highly oriented crystallographic grains for high strain values, metal additive manufacturing (3D printing) may be able to produce highly textured polycrystalline rods, with properties comparable to those manufactured using the more demanding free standing zone melting (FSZM) technique. Rods of Co75.8Fe24.2 and Co63.7Fe36.3 have been fabricated using the Laser engineered net shaping (LENSTM) system to evaluate the performance of additively manufactured magnetic and magnetostrictive materials. The 76% Co sample showed an average magnetostriction (λ) of 86 ppm at a stress of 124 MPa; in contrast, the 64% Co sample showed only 27 ppm at the same stress. For direct comparison, a Co67Fe33 single crystal disk, also measured as part of this study, exhibited a magnetostriction value of 131 and 91 microstrain in the [100] and [111] directions, respectively, with a calculated polycrystalline value (λs) of 107 microstrain. Electron back scattered diffraction (EBSD) has been used to qualitatively link the performance with crystallographic orientation and phase information, showing only the BCC phase in the 76% Co sample, but three different phases (BCC, FCC, and HCP) in the 64% Co sample.

High Pressure Pneumatic Forming of Ti-3Al-2.5V Titanium Tubes in a Square Cross-Sectional Die

PubMed Central

Liu, Gang; Wang, Jianlong; Dang, Kexin; Tang, Zejun

2014-01-01

A new high strain rate forming process for titanium alloys is presented and named High Pressure Pneumatic Forming (HPPF), which might be applicable to form certain tubular components with irregular cross sections with high efficiency, both with respect to energy cost and time consumption. HPPF experiments were performed on Ti-3Al-2.5V titanium alloy tubes using a square cross-sectional die with a small corner radius. The effects of forming of pressure and temperature on the corner filling were investigated and the thickness distributions after the HPPF processes at various pressure levels are discussed. At the same time, the stress state, strain and strain rate distribution during the HPPF process were numerically analyzed by the finite element method. Microstructure evolution of the formed tubes was also analyzed by using electron back scattering diffraction (EBSD). Because of different stress states, the strain and strain rate are very different at different areas of the tube during the corner filling process, and consequently the microstructure of the formed component is affected to some degree. The results verified that HPPF is a potential technology to form titanium tubular components with complicated geometrical features with high efficiency. PMID:28788173

High- and Low-Temperature Deformation Behavior of Different Orientation Hot-Rolled Annealed Zircaloy-4

NASA Astrophysics Data System (ADS)

Zong, Yingying; Gen, Qingfeng; Jiang, Hongwei; Shan, Debin; Guo, Bin

2018-03-01

In this paper, the hot-rolled annealed Zircaloy-4 samples with different orientation were subjected to uniaxial compression with a strain rate of 0.001 s-1 to obtain the stress-strain curves of different initial orientation samples at different temperatures. Electron backscatter diffraction (EBSD) technique and transmission electron microscope (TEM) technique were used to analyze the microstructures and textures of compressed samples. The mechanical properties and microstructural evolution of rolling directions (RD), transverse directions (TD) and normal directions (ND) were investigated under the conditions of - 150 °C low temperature, room temperature and 200 °C high temperature (simulated lunar temperature environment). The results show that the strength of Zircaloy-4 decreases with the increase in deformation temperature, and the strength in three orientations is ND > TD > RD. The deformation mechanism of hot-rolled annealed Zircaloy-4 with different orientation is different. In RD, { 10\\bar{1}0} < {a} > prismatic slip has the highest Schmid factor (SF), so it is most easy to activate the slip, followed by TD orientation, and ND orientation is the most difficult to activate. The deformed grains abide slip→twinning→slip rule, and the different orientation Zircaloy-4 deformation mechanisms mainly are the twinning coordinated with the slip.

Microstructure evolution of a ZrC coating layer in TRISO particles during high-temperature annealing

NASA Astrophysics Data System (ADS)

Kim, Daejong; Chun, Young Bum; Ko, Myeong Jin; Lee, Hyeon-Geun; Cho, Moon-Sung; Park, Ji Yeon; Kim, Weon-Ju

2016-10-01

The influence of high-temperature annealing on the microstructure of zirconium carbide (ZrC) was investigated in relation to its application as a coating layer of a nuclear fuel in a very high temperature gas cooled reactor. ZrC was deposited as a constituent coating layer of TRISO coated particles by a fluidized bed chemical vapor deposition method using a ZrCl4-CH4-Ar-H2 system. The grain growth of ZrC during high-temperature annealing was strongly influenced by the co-deposition of free carbon. Sub-stoichiometric ZrC coatings have experienced a significant grain growth during high-temperature annealing at 1800 °C and 1900 °C for 1 h. On the other hand, a dual phase of stoichiometric ZrC and free carbon experienced little grain growth. It was revealed that the free carbon of the as-deposited ZrC was primarily distributed within the ZrC grains but was redistributed to the grain boundaries after annealing. Consequently, carbon at the grain boundary retarded the grain growth of ZrC. Electron backscatter diffraction (EBSD) results showed that as-deposited ZrC had (001) a preferred orientation that kept its favored direction after significant grain growth during annealing. The hardness slightly decreased as the grain growth progressed.

Comparative study on twinning characteristics during two post-weld compression paths and their effects on joint enhancement.

PubMed

Liu, Zhe; Xin, Renlong; Li, Dongrong; Sun, Liyun; Liu, Qing

2016-12-23

Friction stir welding (FSW) has promising application potential in Mg alloys. However, the texture distribution in stir zone (SZ) is usually complicated for Mg alloys, which deterioriates the joint performance. In this study, the texture distribution in SZ was tailored by applying two kinds of post-weld compression deformation along normal direction (ND) or welding direction (WD) of the FSWed AZ31 Mg alloy plates. The twinning behavior and texture change in the various regions of SZ were then evaluated by electron back scatter diffraction (EBSD) characterization. The effect of texture change on the joint performance was discussed in terms of Schmid factors (SFs) for basal slip and extension twinning. The results showed that profuse extension twins were formed through the whole SZ for the sample subjected to compression along ND, whereas they were observed mainly in SZ-side for the sample compressed along WD. Most of the twins were present in the forms of twin bands or chains. The directions of the twin bands or chains were related to the habit plane traces of selected twin variants. The ND post-weld compression had better strengthening effects on the joints compared to the WD compression, and the underline mechanism was discussed.

Comparative study on twinning characteristics during two post-weld compression paths and their effects on joint enhancement

PubMed Central

Liu, Zhe; Xin, Renlong; Li, Dongrong; Sun, Liyun; Liu, Qing

2016-01-01

Friction stir welding (FSW) has promising application potential in Mg alloys. However, the texture distribution in stir zone (SZ) is usually complicated for Mg alloys, which deterioriates the joint performance. In this study, the texture distribution in SZ was tailored by applying two kinds of post-weld compression deformation along normal direction (ND) or welding direction (WD) of the FSWed AZ31 Mg alloy plates. The twinning behavior and texture change in the various regions of SZ were then evaluated by electron back scatter diffraction (EBSD) characterization. The effect of texture change on the joint performance was discussed in terms of Schmid factors (SFs) for basal slip and extension twinning. The results showed that profuse extension twins were formed through the whole SZ for the sample subjected to compression along ND, whereas they were observed mainly in SZ-side for the sample compressed along WD. Most of the twins were present in the forms of twin bands or chains. The directions of the twin bands or chains were related to the habit plane traces of selected twin variants. The ND post-weld compression had better strengthening effects on the joints compared to the WD compression, and the underline mechanism was discussed. PMID:28008982

Messengers from the deep: Fossil wadsleyite-chromite microstructures from the Mantle Transition Zone.

PubMed

Satsukawa, Takako; Griffin, William L; Piazolo, Sandra; O'Reilly, Suzanne Y

2015-11-13

Investigations of the Mantle Transition Zone (MTZ; 410-660 km deep) by deformation experiments and geophysical methods suggest that the MTZ has distinct rheological properties, but their exact cause is still unclear due to the lack of natural samples. Here we present the first direct evidence for crystal-plastic deformation by dislocation creep in the MTZ using a chromitite from the Luobusa peridotite (E. Tibet). Chromite grains show exsolution of diopside and SiO2, suggesting previous equilibration in the MTZ. Electron backscattered diffraction (EBSD) analysis reveals that olivine grains co-existing with exsolved phases inside chromite grains and occurring on chromite grain boundaries have a single pronounced crystallographic preferred orientation (CPO). This suggests that olivine preserves the CPO of a high-pressure polymorph (wadsleyite) before the high-pressure polymorph of chromite began to invert and exsolve. Chromite also shows a significant CPO. Thus, the fine-grained high-pressure phases were deformed by dislocation creep in the MTZ. Grain growth in inverted chromite produced an equilibrated microstructure during exhumation to the surface, masking at first sight its MTZ deformation history. These unique observations provide a window into the deep Earth, and constraints for interpreting geophysical signals and their geodynamic implications in a geologically robust context.

Characteristics of biogenic calcite in the prismatic layer of a pearl oyster, Pinctada fucata.

PubMed

Okumura, Taiga; Suzuki, Michio; Nagasawa, Hiromichi; Kogure, Toshihiro

2010-10-01

The fine structure of the calcite prism in the outer layer of a pearl oyster, Pinctada fucata, has been investigated using various electron beam techniques, in order to understand its characteristics and growth mechanism including the role of intracrystalline organic substances. As the calcite prismatic layer grows thicker, sinuous boundaries develop to divide the prism into a number of domains. The crystal misorientation between the adjacent domains is several to more than ten degrees. The component of the misorientation is mainly the rotation about the c-axis. There is no continuous organic membrane at the boundaries. Furthermore, the crystal orientation inside the domains changes gradually, as indicated by the electron back-scattered diffraction (EBSD) in a scanning electron microscope (SEM). Transmission electron microscopy (TEM) examination revealed that the domain consists of sub-grains of a few hundred nanometers divided by small-angle grain boundaries, which are probably the origin of the gradual change of the crystal orientation inside the domains. Spherular Fresnel contrasts were often observed at the small-angle grain boundaries, in defocused TEM images. Electron energy-loss spectroscopy (EELS) indicated the spherules are organic macromolecules, suggesting that incorporation of organic macromolecules during the crystal growth forms the sub-grain structure of the calcite prism.

Effect of W and N on mechanical properties of reduced activation ferritic/martensitic EUROFER-based steel grades

NASA Astrophysics Data System (ADS)

Puype, A.; Malerba, L.; De Wispelaere, N.; Petrov, R.; Sietsma, J.

2018-04-01

The C, N, and W content in EUROFER97, a 9CrWVTa reduced-activation ferritic/martensitic (RAFM) steel, was varied to obtain an experimental assessment of the main effects of the compositional variation on the mechanical properties and microstructural characteristics of six different experimental grades. Light optical microscopy (LOM) and electron back-scattered diffraction (EBSD) revealed in almost all cases a fine tempered lath martensite structure. Analyses of transmission electron micrographs, together with inductively coupled plasma mass spectrometry (ICPMS) and energy-dispersive x-ray spectroscopy (EDS) data, shows the precipitation state and spatial distribution of MxCy (M = Cr, W and Fe) and MX (M = V and/or Ta, X = C or N) carbonitrides within the matrix. The mechanical characterization of the six different steel grades was carried out by means of A50 tensile testing and Charpy tests on standard specimens (55 × 10 × 10 mm3). Lowering the carbon content and keeping the nitrogen content higher than 0.02 wt%, leads to a reduction of the ductile-to-brittle-transition-temperature (DBTT) in comparison with EUROFER97-2. The addition of tungsten further reduces the DBTT to - 94 °C, while maintaining good tensile strength and elongation.

Thermomechanical processing of aluminum micro-alloyed with Sc, Zr, Ti, B, and C

NASA Astrophysics Data System (ADS)

McNamara, Cameron T.

Critical exploration of the minimalistic high strength low alloy aluminum (HSLA-Al) paradigm is necessary for the continued development of advanced aluminum alloys. In this study, scandium (Sc) and zirconium (Zr) are examined as the main precipitation strengthening additions, while magnesium (Mg) is added to probe the synergistic effects of solution and precipitation hardening, as well as the grain refinement during solidification afforded by a moderate growth restriction factor. Further, pathways of recrystallization are explored in several potential HSLA-Al syste =ms sans Sc. Aluminum-titanium-boron (Al-Ti-B) and aluminum-titanium-carbon (Al-Ti-C) grain refining master alloys are added to a series of Al-Zr alloys to examine both the reported Zr poisoning effect on grain size reduction and the impact on recrystallization resistance through the use of electron backscattered diffraction (EBSD) imaging. Results include an analysis of active strengthening mechanisms and advisement for both constitution and thermomechanical processing of HSLA-Al alloys for wrought or near-net shape cast components. The mechanisms of recrystallization are discussed for alloys which contain a bimodal distribution of particles, some of which act as nucleation sites for grain formation during annealing and others which restrict the growth of the newly formed grains.

Influence of Sc on microstructure and mechanical properties of Al-Si-Mg-Cu-Zr alloy

NASA Astrophysics Data System (ADS)

Li, Yukun; Du, Xiaodong; Zhang, Ya; Zhang, Zhen; Fu, Junwei; Zhou, Shi'ang; Wu, Yucheng

2018-02-01

In the present study, the effects of Mg, Cu, Sc and Zr combined additions on the microstructure and mechanical properties of hypoeutectic Al-Si cast alloy were systematically investigated. Characterization techniques such as optical microscopy (OM), scanning electron microscope (SEM), energy dispersive spectrometer (EDS), electron back-scatter diffraction (EBSD), atomic force microscopy (AFM), transmission electron microscope (TEM), Brinell hardness tester and universal testing machine were employed to analyze the microstructure and mechanical properties. The results showed that Sc served as modifier on the microstructure of Al-3Si-0.45Mg-0.45Cu-0.2Zr alloys, including modification of eutectic Si and grains. Extraordinarily, grain refinement was found to be related to the primary particles, which exhibited a close orientation to matrix. After T6 heat treatment, the grain structures were composed of nano-scaled secondary Al3(Sc, Zr) precipitates and spherical eutectic Si. Combined with T6 heat treatment, the highest hardness, yield strength, ultimate tensile strength and elongation were achieved in 0.56 wt.% Sc-modified alloy. Interestingly, the strength and ductility had a similar tendency. This paper demonstrated that combined additions of Mg, Cu, Sc and Zr could significantly improve the microstructure and performance of the hypoeutectic Al-Si cast alloy.

DOE Office of Scientific and Technical Information (OSTI.GOV)

White, Emma Marie Hamilton; Kassen, Aaron Gregory; Simsek, Emrah

Alternatives to rare earth permanent magnets, such as alnico, will reduce supply instability, increase sustainability, and could decrease the cost of permanent magnets, especially for high temperature applications, such as traction drive motors. Alnico magnets with moderate coercivity, high remanence, and relatively high energy product are conventionally processed by directional solidification and (significant) final machining, contributing to increased costs and additional material waste. Additive manufacturing (AM) is developing as a cost effective method to build net-shape three-dimensional parts with minimal final machining and properties comparable to wrought parts. This work describes initial studies of net-shape fabrication of alnico magnets bymore » AM using a laser engineered net shaping (LENS) system. High pressure gas atomized (HPGA) pre-alloyed powders of two different modified alnico “8” compositions, with high purity and sphericity, were built into cylinders using the LENS process, followed by heat treatment. The magnetic properties showed improvement over their cast and sintered counterparts. The resulting alnico permanent magnets were characterized using scanning electron microscopy (SEM), energy dispersive spectroscopy (EDS), electron backscatter diffraction (EBSD), and hysteresisgraph measurements. Furthermore, these results display the potential for net-shape processing of alnico permanent magnets for use in next generation traction drive motors and other applications requiring high temperatures and/or complex engineered part geometries.« less

Characterization of the effects of different tempers and aging temperatures on the precipitation behavior of Al-Mg (5.25at.%)-Mn alloys

DOE PAGES

Yi, Gaosong; Littrell, Kenneth C.; Poplawsky, Jonathan D.; ...

2017-01-11

We investigated the effects of different tempers (H131 and H116) and different aging temperatures (50 and 70 °C) on the precipitation behavior of Al-Mg (5.25 at.%)-Mn (Al 5083) alloys aged for a long time (41 and 30 months) using electron backscatter diffraction(EBSD), scanning transmission electron microscopy(STEM), energy-dispersive X-ray spectroscopy(EDS), atom probe tomography (APT), and small angle neutron scattering (SANS). Results for the GP zones and β'' phases were found in Al 5083 H116 aged at 50 °C for 24 months using APT. EDS and SANS revealed that a phase transformation process from GP zones to β'/β phases occurred for precipitatesmore » formed in both Al 5083 H131 and H116 aged at 70 °C. The effective diffusion coefficient of Mg in Al 5083 H131 is 1.8 times of that in Al 5083 H116 aged at 70 °C. The precipitation process in Al 5083 H116 aged at 50 °C is much slower than that in the sample aged at 70 °C. Finally, we identified the coarsening process in Al 5083 H131 and H116 aged at 70 °C for > 9 months.« less

Strain partitioning along the Mahanadi Shear Zone: Implications for paleo-tectonics of the Eastern Ghats Province, India

NASA Astrophysics Data System (ADS)

Bose, Subham; Gupta, Saibal

2018-05-01

During Indo-Antarctic collision at c. 1.0 Ga, Eastern Ghats Province (EGP) granulites amalgamated with the Archean Indian craton. The northern boundary of the EGP was subsequently reworked, undergoing dextral strike-slip shearing at 0.5 Ga. This study documents a phase of dextral shearing within the EGP along WNW-ESE trending shear planes in c. 0.5 Ga mylonites of the Mahanadi Shear Zone. Regional structural trends in the EGP show a swing from NE-SW to the south of the shear zone, to WNW-ESE to its north. The mylonitic shear zone foliation has a sub-horizontal lineation associated with a prominent dextral shear sense in near-horizontal sections. Electron Back Scatter Diffraction (EBSD) studies on quartz confirm that mylonitisation was associated with dextral strike-slip movement in the greenschist facies. North of the Mahanadi Shear Zone, strain was partitioned into narrow dextral strike-slip shear zones along which the older granulite fabrics were transposed parallel to later WNW-ESE trending shear planes at lower grades of metamorphism. This regional-scale shearing at ∼ 500 Ma possibly resulted in a significant dextral shift of the northern EGP with respect to the south. The shear zone was reactivated in the Permian time during deposition of Gondwana sediments in the Mahanadi basin.

Biomineral shell formation under ocean acidification: a shift from order to chaos.

PubMed

Fitzer, Susan C; Chung, Peter; Maccherozzi, Francesco; Dhesi, Sarnjeet S; Kamenos, Nicholas A; Phoenix, Vernon R; Cusack, Maggie

2016-02-15

Biomineral production in marine organisms employs transient phases of amorphous calcium carbonate (ACC) in the construction of crystalline shells. Increasing seawater pCO2 leads to ocean acidification (OA) with a reduction in oceanic carbonate concentration which could have a negative impact on shell formation and therefore survival. We demonstrate significant changes in the hydrated and dehydrated forms of ACC in the aragonite and calcite layers of Mytilus edulis shells cultured under acidification conditions (1000 μatm pCO2) compared to present day conditions (380 μatm pCO2). In OA conditions, Mytilus edulis has more ACC at crystalisation sites. Here, we use the high-spatial resolution of synchrotron X-ray Photo Emission Electron Microscopy (XPEEM) combined with X-ray Absorption Spectroscopy (XAS) to investigate the influence of OA on the ACC formation in the shells of adult Mytilus edulis. Electron Backscatter Diffraction (EBSD) confirms that OA reduces crystallographic control of shell formation. The results demonstrate that OA induces more ACC formation and less crystallographic control in mussels suggesting that ACC is used as a repair mechanism to combat shell damage under OA. However, the resultant reduced crystallographic control in mussels raises concerns for shell protective function under predation and changing environments.

Biomineral shell formation under ocean acidification: a shift from order to chaos

PubMed Central

Fitzer, Susan C.; Chung, Peter; Maccherozzi, Francesco; Dhesi, Sarnjeet S.; Kamenos, Nicholas A.; Phoenix, Vernon R.; Cusack, Maggie

2016-01-01

Biomineral production in marine organisms employs transient phases of amorphous calcium carbonate (ACC) in the construction of crystalline shells. Increasing seawater pCO2 leads to ocean acidification (OA) with a reduction in oceanic carbonate concentration which could have a negative impact on shell formation and therefore survival. We demonstrate significant changes in the hydrated and dehydrated forms of ACC in the aragonite and calcite layers of Mytilus edulis shells cultured under acidification conditions (1000 μatm pCO2) compared to present day conditions (380 μatm pCO2). In OA conditions, Mytilus edulis has more ACC at crystalisation sites. Here, we use the high-spatial resolution of synchrotron X-ray Photo Emission Electron Microscopy (XPEEM) combined with X-ray Absorption Spectroscopy (XAS) to investigate the influence of OA on the ACC formation in the shells of adult Mytilus edulis. Electron Backscatter Diffraction (EBSD) confirms that OA reduces crystallographic control of shell formation. The results demonstrate that OA induces more ACC formation and less crystallographic control in mussels suggesting that ACC is used as a repair mechanism to combat shell damage under OA. However, the resultant reduced crystallographic control in mussels raises concerns for shell protective function under predation and changing environments. PMID:26876022

Hot deformation behavior of microstructural constituents in a duplex stainless steel during high-temperature straining

NASA Astrophysics Data System (ADS)

Momeni, Amir; Kazemi, Shahab; Bahrani, Ali

2013-10-01

The hot deformation characteristics of 1.4462 duplex stainless steel (DSS) were analyzed by considering strain partitioning between austenite and ferrite constituents. The individual behavior of ferrite and austenite in microstructure was studied in an iso-stress condition. Hot compression tests were performed at temperatures of 800-1100°C and strain rates of 0.001-1 s-1. The flow stress was modeled by a hyperbolic sine constitutive equation, the corresponding constants and apparent activation energies were determined for the studied alloys. The constitutive equation and law of mixture were used to measure the contribution factor of each phase at any given strain. It is found that the contribution factor of ferrite exponentially declines as the Zener-Hollomon parameter ( Z) increases. On the contrary, the austenite contribution polynomially increases with the increase of Z. At low Z values below 2.6.×1015 (ln Z=35.5), a negative contribution factor is determined for austenite that is attributed to dynamic recrystallization. At high Z values, the contribution factor of austenite is about two orders of magnitude greater than that of ferrite, and therefore, austenite can accommodate more strain. Microstructural characterization via electron back-scattered diffraction (EBSD) confirms the mechanical results and shows that austenite recrystallization is possible only at high temperature and low strain rate.

Gradient Nanostructured Tantalum by Thermal-Mechanical Ultrasonic Impact Energy.

PubMed

Chae, Jong-Min; Lee, Keun-Oh; Amanov, Auezhan

2018-03-20

Microstructural evolution and wear performance of Tantalum (Ta) treated by ultrasonic nanocrystalline surface modification (UNSM) at 25 and 1000 °C were reported. The UNSM treatment modified a surface along with subsurface layer with a thickness in the range of 20 to 150 µm, which depends on the UNSM treatment temperature, via the surface severe plastic deformation (S²PD) method. The cross-sectional microstructure of the specimens was observed by electron backscattered diffraction (EBSD) in order to confirm the microstructural alteration in terms of effective depth and refined grain size. The surface hardness measurement results, including depth profile, revealed that the hardness of the UNSM-treated specimens at both temperatures was increased in comparison with those of the untreated ones. The increase in UNSM treatment temperature led to a further increase in hardness. Moreover, both the UNSM-treated specimens with an increased hardness resulted in a higher resistance to wear in comparison with those of the untreated ones under dry conditions. The increase in hardness and induced compressive residual stress that depend on the formation of severe plastically deformed layer with the refined nano-grains are responsible for the enhancement in wear resistance. The findings of this study may be implemented in response to various industries that are related to strength improvement and wear enhancement issues of Ta.

Gradient Nanostructured Tantalum by Thermal-Mechanical Ultrasonic Impact Energy

PubMed Central

Chae, Jong-Min; Lee, Keun-Oh; Amanov, Auezhan

2018-01-01

Microstructural evolution and wear performance of Tantalum (Ta) treated by ultrasonic nanocrystalline surface modification (UNSM) at 25 and 1000 °C were reported. The UNSM treatment modified a surface along with subsurface layer with a thickness in the range of 20 to 150 µm, which depends on the UNSM treatment temperature, via the surface severe plastic deformation (S2PD) method. The cross-sectional microstructure of the specimens was observed by electron backscattered diffraction (EBSD) in order to confirm the microstructural alteration in terms of effective depth and refined grain size. The surface hardness measurement results, including depth profile, revealed that the hardness of the UNSM-treated specimens at both temperatures was increased in comparison with those of the untreated ones. The increase in UNSM treatment temperature led to a further increase in hardness. Moreover, both the UNSM-treated specimens with an increased hardness resulted in a higher resistance to wear in comparison with those of the untreated ones under dry conditions. The increase in hardness and induced compressive residual stress that depend on the formation of severe plastically deformed layer with the refined nano-grains are responsible for the enhancement in wear resistance. The findings of this study may be implemented in response to various industries that are related to strength improvement and wear enhancement issues of Ta. PMID:29558402

Effect of initial grain size on inhomogeneous plastic deformation and twinning behavior in high manganese austenitic steel with a polycrystalline microstructure

NASA Astrophysics Data System (ADS)

Ueji, R.; Tsuchida, N.; Harada, K.; Takaki, K.; Fujii, H.

2015-08-01

The grain size effect on the deformation twinning in a high manganese austenitic steel which is so-called TWIP (twining induced plastic deformation) steel was studied in order to understand how to control deformation twinning. The 31wt%Mn-3%Al-3% Si steel was cold rolled and annealed at various temperatures to obtain fully recrystallized structures with different mean grain sizes. These annealed sheets were examined by room temperature tensile tests at a strain rate of 10-4/s. The coarse grained sample (grain size: 49.6μm) showed many deformation twins and the deformation twinning was preferentially found in the grains in which the tensile axis is parallel near to [111]. On the other hand, the sample with finer grains (1.8 μm) had few grains with twinning even after the tensile deformation. The electron back scattering diffraction (EB SD) measurements clarified the relationship between the anisotropy of deformation twinning and that of inhomogeneous plastic deformation. Based on the EBSD analysis, the mechanism of the suppression of deformation twinning by grain refinement was discussed with the concept of the slip pattern competition between the slip system governed by a grain boundary and that activated by the macroscopic load.

Magnetostrictive performance of additively manufactured CoFe rods using the LENS (TM) system

DOE PAGES

Jones, Nicholas J.; Yoo, Jin-Hyeong; Ott, Ryan T.; ...

2018-05-01

Magnetostrictive materials exhibit a strain in the presence of a variable magnetic field. While they normally require large, highly oriented crystallographic grains for high strain values, metal additive manufacturing (3D printing) may be able to produce highly textured polycrystalline rods, with properties comparable to those manufactured using the more demanding free standing zone melting (FSZM) technique. Rods of Co 75.8Fe 24.2 and Co 63.7Fe 36.3 have been fabricated using the Laser engineered net shaping (LENS TM) system to evaluate the performance of additively manufactured magnetic and magnetostrictive materials. The 76% Co sample showed an average magnetostriction (λ) of 86 ppmmore » at a stress of 124 MPa; in contrast, the 64% Co sample showed only 27 ppm at the same stress. For direct comparison, a Co 67Fe 33 single crystal disk, also measured as part of this study, exhibited a magnetostriction value of 131 and 91 microstrain in the [100] and [111] directions, respectively, with a calculated polycrystalline value (λ s) of 107 microstrain. Electron back scattered diffraction (EBSD) has been used to qualitatively link the performance with crystallographic orientation and phase information, showing only the BCC phase in the 76% Co sample, but three different phases (BCC, FCC, and HCP) in the 64% Co sample.« less

Laser Cladding of Ultra-Thin Nickel-Based Superalloy Sheets.

PubMed

Gabriel, Tobias; Rommel, Daniel; Scherm, Florian; Gorywoda, Marek; Glatzel, Uwe

2017-03-10

Laser cladding is a well-established process to apply coatings on metals. However, on substrates considerably thinner than 1 mm it is only rarely described in the literature. In this work 200 µm thin sheets of nickel-based superalloy 718 are coated with a powder of a cobalt-based alloy, Co-28Cr-9W-1.5Si, by laser cladding. The process window is very narrow, therefore, a precisely controlled Yb fiber laser was used. To minimize the input of energy into the substrate, lines were deposited by setting single overlapping points. In a design of experiments (DoE) study, the process parameters of laser power, laser spot area, step size, exposure time, and solidification time were varied and optimized by examining the clad width, weld penetration, and alloying depth. The microstructure of the samples was investigated by optical microscope (OM) and scanning electron microscopy (SEM), combined with electron backscatter diffraction (EBSD) and energy dispersive X-ray spectroscopy (EDX). Similarly to laser cladding of thicker substrates, the laser power shows the highest influence on the resulting clad. With a higher laser power, the clad width and alloying depth increase, and with a larger laser spot area the weld penetration decreases. If the process parameters are controlled precisely, laser cladding of such thin sheets is manageable.

Laser Cladding of Ultra-Thin Nickel-Based Superalloy Sheets

PubMed Central

Gabriel, Tobias; Rommel, Daniel; Scherm, Florian; Gorywoda, Marek; Glatzel, Uwe

2017-01-01

Laser cladding is a well-established process to apply coatings on metals. However, on substrates considerably thinner than 1 mm it is only rarely described in the literature. In this work 200 µm thin sheets of nickel-based superalloy 718 are coated with a powder of a cobalt-based alloy, Co–28Cr–9W–1.5Si, by laser cladding. The process window is very narrow, therefore, a precisely controlled Yb fiber laser was used. To minimize the input of energy into the substrate, lines were deposited by setting single overlapping points. In a design of experiments (DoE) study, the process parameters of laser power, laser spot area, step size, exposure time, and solidification time were varied and optimized by examining the clad width, weld penetration, and alloying depth. The microstructure of the samples was investigated by optical microscope (OM) and scanning electron microscopy (SEM), combined with electron backscatter diffraction (EBSD) and energy dispersive X-ray spectroscopy (EDX). Similarly to laser cladding of thicker substrates, the laser power shows the highest influence on the resulting clad. With a higher laser power, the clad width and alloying depth increase, and with a larger laser spot area the weld penetration decreases. If the process parameters are controlled precisely, laser cladding of such thin sheets is manageable. PMID:28772639