Effect Of Chromium Underlayer On The Properties Of Nano-Crystalline Diamond Films

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

Garratt, Elias; AlFaify, Salem; Yoshitake, T.

2013-01-11

This paper investigated the effect of chromium underlayer on the structure, microstructure and composition of the nano-crystalline diamond films. Nano-crystalline diamond thin films were deposited at high temperature in microwave-induced plasma diluted with nitrogen, on silicon substrate with a thin film of chromium as an underlayer. The composition, structure and microstructure of the deposited layers were analyzed using non-Rutherford Backscattering Spectrometry, Raman Spectroscopy, Near-Edge X-Ray Absorption Fine Structure, X-ray Diffraction and Atomic Force Microscopy. Nanoindentation studies showed that the films deposited on chromium underlayer have higher hardness values compared to those deposited on silicon without an underlayer. Diamond and graphiticmore » phases of the films evaluated by x-ray and optical spectroscopic analysis determined consistency between sp2 and sp3 phases of carbon in chromium sample to that of diamond grown on silicon. Diffusion of chromium was observed using ion beam analysis which was correlated with the formation of chromium complexes by x-ray diffraction.« less

Submicron x-ray diffraction and its applications to problems in materials and environmental science

NASA Astrophysics Data System (ADS)

Tamura, N.; Celestre, R. S.; MacDowell, A. A.; Padmore, H. A.; Spolenak, R.; Valek, B. C.; Meier Chang, N.; Manceau, A.; Patel, J. R.

2002-03-01

The availability of high brilliance third generation synchrotron sources together with progress in achromatic focusing optics allows us to add submicron spatial resolution to the conventional century-old x-ray diffraction technique. The new capabilities include the possibility to map in situ, grain orientations, crystalline phase distribution, and full strain/stress tensors at a very local level, by combining white and monochromatic x-ray microbeam diffraction. This is particularly relevant for high technology industry where the understanding of material properties at a microstructural level becomes increasingly important. After describing the latest advances in the submicron x-ray diffraction techniques at the Advanced Light Source, we will give some examples of its application in material science for the measurement of strain/stress in metallic thin films and interconnects. Its use in the field of environmental science will also be discussed.

Study of microstructure and electroluminescence of zinc sulfide thin film

NASA Astrophysics Data System (ADS)

Zhao-hong, Liu; Yu-jiang, Wang; Mou-zhi, Chen; Zhen-xiang, Chen; Shu-nong, Sun; Mei-chun, Huang

1998-03-01

The electroluminscent zinc sulfide thin film doped with erbium, fabricated by thermal evaporation with two boats, are examined. The surface and internal electronic states of ZnS thin film are measured by means of x-ray diffraction and x-ray photoemission spectroscopy. The information on the relations between electroluminescent characteristics and internal electronic states of the film is obtained. And the effects of the microstructure of thin film doped with rare earth erbium on electroluminescence are discussed as well.

Single-shot full strain tensor determination with microbeam X-ray Laue diffraction and a two-dimensional energy-dispersive detector.

PubMed

Abboud, A; Kirchlechner, C; Keckes, J; Conka Nurdan, T; Send, S; Micha, J S; Ulrich, O; Hartmann, R; Strüder, L; Pietsch, U

2017-06-01

The full strain and stress tensor determination in a triaxially stressed single crystal using X-ray diffraction requires a series of lattice spacing measurements at different crystal orientations. This can be achieved using a tunable X-ray source. This article reports on a novel experimental procedure for single-shot full strain tensor determination using polychromatic synchrotron radiation with an energy range from 5 to 23 keV. Microbeam X-ray Laue diffraction patterns were collected from a copper micro-bending beam along the central axis (centroid of the cross section). Taking advantage of a two-dimensional energy-dispersive X-ray detector (pnCCD), the position and energy of the collected Laue spots were measured for multiple positions on the sample, allowing the measurement of variations in the local microstructure. At the same time, both the deviatoric and hydrostatic components of the elastic strain and stress tensors were calculated.

X-ray diffraction analysis of hydroxyapatite-coated in different plasma gas atmosphere on Ti and Ti-6Al-4V

PubMed Central

Kotian, Ravindra; Rao, P. Prasad; Madhyastha, Prashanthi

2017-01-01

Objective: The aim is to study the effect of plasma working gas on composition, crystallinity, and microstructure of hydroxyapatite (HA) coated on Ti and Ti-6Al-4V metal substrates. Materials and Methods: Ti and Ti-6Al-4V metal substrates were coated with HA by plasma spray using four plasma gas atmospheres of argon, argon/hydrogen, nitrogen, and nitrogen/hydrogen. The degree of crystallinity, the phases present, and microstructure of HA coating were characterized using X-ray diffraction and scanning electron microscopy. Results: Variation in crystallinity and the microstructure of HA coating on plasma gas atmosphere was observed. Micro-cracks due to thermal stresses and shift in the 2θ angle of HA compared to feedstock was seen. Conclusion: Plasma gas atmosphere has a significant influence on composition, crystallinity, and micro-cracks of HA-coated dental implants. PMID:29279668

Understanding self ion damage in FCC Ni-Cr-Fe based alloy using X-ray diffraction techniques

NASA Astrophysics Data System (ADS)

Halder Banerjee, R.; Sengupta, P.; Chatterjee, A.; Mishra, S. C.; Bhukta, A.; Satyam, P. V.; Samajdar, I.; Dey, G. K.

2018-04-01

Using X-ray diffraction line profile analysis (XRDLPA) approach the radiation response of FCC Ni-Cr-Fe based alloy 690 to 1.5 and 3 MeV Ni2+ ion damage was quantified in terms of its microstructural parameters. These microstructural parameters viz. average domain size, microstrain and dislocation density were found to vary anisotropically with fluence. The anisotropic behaviour is mainly attributable to presence of twins in pre-irradiated microstructure. After irradiation, surface roughness increases as a function of fluence attributable to change in surface and sub-surface morphology caused by displacement cascade, defects and sputtered atoms created by incident energetic ion. The radiation hardening in case of 1.5 MeV Ni2+ irradiated specimens too is a consequence of the increase in dislocation density formed by interaction of radiation induced defects with pre-existing dislocations. At highest fluence there is an initiation of saturation.

An x-ray diffraction study of microstructural deformation induced by cyclic loading of selected steel

NASA Astrophysics Data System (ADS)

Fourspring, Patrick Michael

X-ray double crystal diffractometry (XRDCD) and X-ray scanning diffractometry (XRSD) were used to assess cyclic microstructural deformation in a face centered cubic (fcc) steel (AISI304) and a body centered cubic (bcc) steel (SA508 class 2). The objectives of the investigation were to determine if X-ray diffraction could be used effectively to monitor cyclic microstructural deformation in polycrystalline Fe alloys and to study the distribution of the microstructural deformation induced by cyclic loading in these alloys. The approach used in the investigation was to induce fatigue damage in a material and to characterize the resulting microstructural deformation at discrete fractions of the fatigue life of the material. Also, characterization of microstructural deformation was carried out to identify differences in the accumulation of damage from the surface to the bulk, focusing on the following three regions: near surface (0-10 mum), subsurface (10-300 mum), and bulk. Characterization of the subsurface region was performed only on the AISI304 material because of the limited availability of the SA508 material. The results from the XRDCD data indicate a measurable change induced by fatigue from the initial state to subsequent states of both the AISI304 and the SA508 materials. The results from the XRSD data show similar but less coherent trends than the results from the XRDCD data. Therefore, the XRDCD technique was shown to be sensitive to the microstructural deformation caused by fatigue in steels; thus, the technique can be used to monitor fatigue damage in steels. In addition, for the AISI304 material, the level of cyclic microstructural deformation in the bulk material was found to be greater than the level in the near surface material. In contrast, previous investigations have shown that the deformation is greater in the near surface than the bulk for Al alloys and bcc Fe alloys.

Microstructure Analysis of Bismuth Absorbers for Transition-Edge Sensor X-ray Microcalorimeters

NASA Astrophysics Data System (ADS)

Yan, Daikang; Divan, Ralu; Gades, Lisa M.; Kenesei, Peter; Madden, Timothy J.; Miceli, Antonino; Park, Jun-Sang; Patel, Umeshkumar M.; Quaranta, Orlando; Sharma, Hemant; Bennett, Douglas A.; Doriese, William B.; Fowler, Joseph W.; Gard, Johnathon D.; Hays-Wehle, James P.; Morgan, Kelsey M.; Schmidt, Daniel R.; Swetz, Daniel S.; Ullom, Joel N.

2018-03-01

Given its large X-ray stopping power and low specific heat capacity, bismuth (Bi) is a promising absorber material for X-ray microcalorimeters and has been used with transition-edge sensors (TESs) in the past. However, distinct X-ray spectral features have been observed in TESs with Bi absorbers deposited with different techniques. Evaporated Bi absorbers are widely reported to have non-Gaussian low-energy tails, while electroplated ones do not show this feature. In this study, we fabricated Bi absorbers with these two methods and performed microstructure analysis using scanning electron microscopy and X-ray diffraction microscopy. The two types of material showed the same crystallographic structure, but the grain size of the electroplated Bi was about 40 times larger than that of the evaporated Bi. This distinction in grain size is likely to be the cause of their different spectral responses.

In Situ XRD Studies of the Process Dynamics During Annealing in Cold-Rolled Copper

NASA Astrophysics Data System (ADS)

Dey, Santu; Gayathri, N.; Bhattacharya, M.; Mukherjee, P.

2016-12-01

The dynamics of the release of stored energy during annealing along two different crystallographic planes, i.e., {111} and {220}, in deformed copper have been investigated using in situ X-ray diffraction measurements at 458 K and 473 K (185 °C and 200 °C). The study has been carried out on 50 and 80 pct cold-rolled Cu sheets. The microstructures of the rolled samples have been characterized using optical microscopy and electron backscattered diffraction measurements. The microstructural parameters were evaluated from the X-ray diffractogram using the Scherrer equation and the modified Rietveld method. The stored energy along different planes was determined using the modified Stibitz formula from the X-ray peak broadening, and the bulk stored energy was evaluated using differential scanning calorimetry. The process dynamics of recovery and recrystallization as observed through the release of stored energy have been modeled as the second-order and first-order processes, respectively.

Biaxial flexural strength and microstructure changes of two recycled pressable glass ceramics.

PubMed

Albakry, Mohammad; Guazzato, Massimiliano; Swain, Michael Vincent

2004-09-01

This study evaluated the biaxial flexural strength and identified the crystalline phases and the microstructural features of pressed and repressed materials of the glass ceramics, Empress 1 and Empress 2. Twenty pressed and 20 repressed disc specimens measuring 14 mm x 1 mm per material were prepared following the manufacturers' recommendations. Biaxial flexure (piston on 3-ball method) was used to assess strength. X-ray diffraction was performed to identify the crystalline phases, and a scanning electron microscope was used to disclose microstructural features. Biaxial flexural strength, for the pressed and repressed specimens, respectively, were E1 [148 (SD 18) and 149 (SD 35)] and E2 [340 (SD 40), 325 (SD 60)] MPa. There was no significant difference in strength between the pressed and the repressed groups of either material, Empress 1 and Empress 2 (p > 0.05). Weibull modulus values results were E1: (8, 4.7) and E2: (9, 5.8) for the same groups, respectively. X-ray diffraction revealed that leucite was the main crystalline phase for Empress 1 groups, and lithium disilicate for Empress 2 groups. No further peaks were observed in the X-ray diffraction patterns of either material after repressing. Dispersed leucite crystals and cracks within the leucite crystals and glass matrix were features observed in Empress 1 for pressed and repressed samples. Similar microstructure features--dense lithium disilicate crystals within a glass matrix--were observed in Empress 2 pressed and repressed materials. However, the repressed material showed larger lithium disilicate crystals than the singly pressed material. Second pressing had no significant effect on the biaxial flexural strength of Empress 1 or Empress 2; however, higher strength variations among the repressed samples of the materials may indicate less reliability of these materials after second pressing.

Strain and lattice orientation distribution in SiN/Ge complementary metal–oxide–semiconductor compatible light emitting microstructures by quick x-ray nano-diffraction microscopy

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

Chahine, G. A.; Schülli, T. U.; Zoellner, M. H.

2015-02-16

This paper presents a study of the spatial distribution of strain and lattice orientation in CMOS-fabricated strained Ge microstripes using high resolution x-ray micro-diffraction. The recently developed model-free characterization tool, based on a quick scanning x-ray diffraction microscopy technique can image strain down to levels of 10{sup −5} (Δa/a) with a spatial resolution of ∼0.5 μm. Strain and lattice tilt are extracted using the strain and orientation calculation software package X-SOCS. The obtained results are compared with the biaxial strain distribution obtained by lattice parameter-sensitive μ-Raman and μ-photoluminescence measurements. The experimental data are interpreted with the help of finite element modelingmore » of the strain relaxation dynamics in the investigated structures.« less

Control of the kerf size and microstructure in Inconel 738 superalloy by femtosecond laser beam cutting

NASA Astrophysics Data System (ADS)

Wei, J.; Ye, Y.; Sun, Z.; Liu, L.; Zou, G.

2016-05-01

Femtosecond laser beam cutting is becoming widely used to meet demands for increasing accuracy in micro-machining. In this paper, the effects of processing parameters in femtosecond laser beam cutting on the kerf size and microstructure in Inconel 738 have been investigated. The defocus, pulse width and scanning speed were selected to study the controllability of the cutting process. Adjusting and matching the processing parameters was a basic enhancement method to acquire well defined kerf size and the high-quality ablation of microstructures, which has contributed to the intensity clamping effect. The morphology and chemical compositions of these microstructures on the cut surface have been characterized by a scanning electron microscopy equipped with an energy dispersive X-ray spectroscopy, X-ray diffraction and X-ray photoelectron spectroscopy. Additionally, the material removal mechanism and oxidation mechanism on the Inconel 738 cut surface have also been discussed on the basis of the femtosecond laser induced normal vaporization or phase explosion, and trapping effect of the dangling bonds.

Applications of synchrotron radiation to materials science: Diffraction imaging (topography) and microradiography

NASA Technical Reports Server (NTRS)

Kuriyama, Masao

1988-01-01

Synchrotron radiation sources are now available throughout the world. The use of hard X-ray radiation from these sources for materials science is described with emphasis on diffraction imaging for material characterization. With the availability of synchrotron radiation, real-time in situ measurements of dynamic microstructural phenomena have been started. This is a new area where traditional application of X-rays has been superseded. Examples are chosen from limited areas and are by no means exhaustive. The new emerging information will, no doubt, have great impact on materials science and engineering.

Microstructural and micromechanical characterization of IN718 theta shaped specimens built with electron beam melting

DOE PAGES

Cakmak, Ercan; Kirka, Michael M.; Watkins, Thomas R.; ...

2016-02-23

Theta-shaped specimens were additively manufactured out of Inconel 718 powders using an electron beam melting technique, as a model complex load bearing structure. We employed two different build strategies; producing two sets of specimens. Microstructural and micro-mechanical characterizations were performed using electron back-scatter, synchrotron x-ray and in-situ neutron diffraction techniques. In particular, the cross-members of the specimens were the focus of the synchrotron x-ray and in-situ neutron diffraction measurements. The build strategies employed resulted in the formation of distinct microstructures and crystallographic textures, signifying the importance of build-parameter manipulation for microstructural optimization. Large strain anisotropy of the different lattice planesmore » was observed during in-situ loading. Texture was concluded to have a distinct effect upon both the axial and transverse strain responses of the cross-members. In particular, the (200), (220) and (420) transverse lattice strains all showed unexpected overlapping trends in both builds. This was related to the strong {200} textures along the build/loading direction, providing agreement between the experimental and calculated results.« less

Probing multi-scale mechanical damage in connective tissues using X-ray diffraction.

PubMed

Bianchi, Fabio; Hofmann, Felix; Smith, Andrew J; Thompson, Mark S

2016-11-01

The accumulation of microstructural collagen damage following repetitive loading is linked to painful and debilitating tendon injuries. As a hierarchical, semi-crystalline material, collagen mechanics can be studied using X-ray diffraction. The aim of the study was to describe multi-structural changes in tendon collagen following controlled plastic damage (5% permanent strain). We used small angle X-ray scattering (SAXS) to interrogate the spacing of collagen molecules within a fibril, and wide angle X-ray scattering (WAXS) to measure molecular strains under macroscopic loading. Simultaneous recordings of SAXS and WAXS patterns, together with whole-tissue strain in physiologically hydrated rat-tail tendons were made during increments of in situ tensile loading. Results showed that while tissue level modulus was unchanged, fibril modulus decreased significantly, and molecular modulus significantly increased. Further, analysis of higher order SAXS peaks suggested structural changes in the gap and overlap regions, possibly localising the damage to molecular cross-links. Our results provide new insight into the fundamental damage processes at work in collagenous tissues and point to new directions for their mitigation and repair. This article reports the first in situ loading synchrotron studies on mechanical damage in collagenous tissues. We provide new insight into the nano- and micro-structural mechanisms of damage processes. Pre-damaged tendons showed differential alteration of moduli at macro, micro and nano-scales as measured using X-ray scattering techniques. Detailed analysis of higher order diffraction peaks suggested damage is localised to molecular cross-links. The results are consistent with previous X-ray scattering studies of tendons and also with recent thermal stability studies on damaged material. Detailed understanding of damage mechanisms is essential in the development of new therapies promoting tissue repair. Copyright © 2016 Acta Materialia Inc. Published by Elsevier Ltd. All rights reserved.

The microstructures of SCS-6 and SCS-8 SiC reinforcing fibers

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

Sattler, M.L.; Kinney, J.H.; Zywicz, E.

The microstructures of SCS-6 and SCS-8 SiC fibers have been examined and analyzed using high resolution transmission electron microscopy (HRTEM), microdiffraction, parallel electron energy loss spectroscopy (PEELS), x-ray diffraction and x-ray spectroscopy. The results of the study confirm findings from earlier studies wherein the microstructure of the fibers have been described as consisting of {beta}-SiC grown upon a monofilament turbostratic carbon core. The present study, however, provides much more detail regarding this microstructure. For example, PEELS spectroscopy and x-ray microscopy indicate that the composition of the SiC varies smoothly from SiC plus free C near the carbon core to SiCmore » at the midradial boundary. The SiC stoichiometry is roughly preserved from the midradial boundary to the exterior interface. HRTEM, microdiffraction, and dark field images provide evidence that the excess carbon is amorphous free carbon which is most likely situated at the grain boundaries of the SiC. The x-ray microscopy results are also consistent with the presence of two phases near the core which consist of SiC and free carbon having density less than graphite (2.25 g/cc). This complex microstructure may explain the recent observations of nonplanar failure in composites fabricated with SCS fibers.« less

Phase-contrast x-ray imaging of microstructure and fatigue-crack propagation in single-crystal nickel-base superalloys

NASA Astrophysics Data System (ADS)

Husseini, Naji Sami

Single-crystal nickel-base superalloys are ubiquitous in demanding turbine-blade applications, and they owe their remarkable resilience to their dendritic, hierarchical microstructure and complex composition. During normal operations, they endure rapid low-stress vibrations that may initiate fatigue cracks. This failure mode in the very high-cycle regime is poorly understood, in part due to inadequate testing and diagnostic equipment. Phase-contrast imaging with coherent synchrotron x rays, however, is an emergent technique ideally suited for dynamic processes such as crack initiation and propagation. A specially designed portable ultrasonic-fatigue apparatus, coupled with x-ray radiography, allows real-time, in situ imaging while simulating service conditions. Three contrast mechanisms - absorption, diffraction, and phase contrast - span the immense breadth of microstructural features in superalloys. Absorption contrast is sensitive to composition and crack displacements, and diffraction contrast illuminates dislocation aggregates and crystallographic misorientations. Phase contrast enhances electron-density gradients and is particularly useful for fatigue-crack studies, sensitive to internal crack tips and openings less than one micrometer. Superalloy samples were imaged without external stresses to study microstructure and mosaicity. Maps of rhenium and tungsten concentrations revealed strong segregation to the center of dendrites, as manifested by absorption contrast. Though nominally single crystals, dendrites were misoriented from the bulk by a few degrees, as revealed by diffraction contrast. For dynamic studies of cyclic fatigue, superalloys were mounted in the portable ultrasonic-fatigue apparatus, subjected to a mean tensile stress of ˜50-150 MPa, and cycled in tension to initiate and propagate fatigue cracks. Radiographs were recorded every thousand cycles over the multimillion-cycle lifetime to measure micron-scale crack growth. Crack openings were very small, as determined by absorption and phase contrast, and suggested multiple fracture modes for propagation along {111} planes at room temperature, which was verified by finite element analysis. With increasing temperature, cracks became Mode I (perpendicular to the loading axis) in character and more sensitive to the microstructure. Advancing plastic zones ahead of crack tips altered the crystallographic quality, from which diffraction contrast anticipated initiation and propagation. These studies demonstrate the extreme sensitivity of x-ray radiography for detailed studies of superalloys and crack growth processes.

Microstructural characterization of Ti-6Al-4V alloy subjected to the duplex SMAT/plasma nitriding.

PubMed

Pi, Y; Faure, J; Agoda-Tandjawa, G; Andreazza, C; Potiron, S; Levesque, A; Demangel, C; Retraint, D; Benhayoune, H

2013-09-01

In this study, microstructural characterization of Ti-6Al-4V alloy, subjected to the duplex surface mechanical attrition treatment (SMAT)/nitriding treatment, leading to improve its mechanical properties, was carried out through novel and original samples preparation methods. Instead of acid etching which is limited for morphological characterization by scanning electron microscopy (SEM), an original ion polishing method was developed. Moreover, for structural characterization by transmission electron microscopy (TEM), an ion milling method based with the use of two ions guns was also carried out for cross-section preparation. To demonstrate the efficiency of the two developed methods, morphological investigations were done by traditional SEM and field emission gun SEM. This was followed by structural investigations through selected area electron diffraction (SAED) coupled with TEM and X-ray diffraction techniques. The results demonstrated that ionic polishing allowed to reveal a variation of the microstructure according to the surface treatment that could not be observed by acid etching preparation. TEM associated to SAED and X-ray diffraction provided information regarding the nanostructure compositional changes induced by the duplex SMAT/nitriding process. Copyright © 2013 Wiley Periodicals, Inc.

Phase transformation in δ-Pu alloys at low temperature: An in situ microstructural characterization using X-ray diffraction

NASA Astrophysics Data System (ADS)

Ravat, B.; Platteau, C.; Texier, G.; Oudot, B.; Delaunay, F.

2009-09-01

In order to investigate the martensitic transformation, an isothermal hold at -130 °C for 48 h was performed on a highly homogenized PuGa alloy. The modifications of the microstructure were characterized in situ thanks to a specific tool. This device was developed at the CEA-Valduc to analyze the crystalline structure of plutonium alloys as a function of temperature and more especially at low temperature using X-ray diffraction. The analysis of the recorded diffraction patterns highlighted that the martensitic transformation for this alloy is the result of a direct δ → α' + δ phase transformation. Moreover, a significant Bragg's peaks broadening corresponding to the δ-phase was observed. A microstructural analysis was made to characterize anisotropic microstrain resulting from the stress induced by the unit cell volume difference between the δ and α' phases. The amount of α'-phase evolved was analyzed within the framework of the Avrami theory in order to characterize the nucleation process. The results suggested that the growth mechanism corresponded to a general mechanism where the nucleation sites were in the δ-grain edges and the α'-phase had a plate-like morphology.

Impurity incorporation, deposition kinetics, and microstructural evolution in sputtered Ta films

NASA Astrophysics Data System (ADS)

Whitacre, Jay Fredric

There is an increasing need to control the microstructure in thin sputtered Ta films for application as high-temperature coatings or diffusion barriers in microelectronic interconnect structures. To this end, the relationship between impurity incorporation, deposition kinetics, and microstructural evolution was examined for room-temperature low growth rate DC magnetron sputtered Ta films. Impurity levels present during deposition were controlled by pumping the chamber to various base pressures before growth. Ar pressures ranging from 2 to 20 mTorr were used to create contrasting kinetic environments in the sputter gas. This affected both the distribution of adatom kinetic energies at the substrate as well as the rate of impurity desorption from the chamber walls: at higher Ar pressures adatoms has lower kinetic energies, and there was an increase in impurity concentration. X-ray diffraction, high-resolution transmission electron microscopy (HREM), transmission electron diffraction (TED), scanning electron microscopy (SEM), secondary ion mass spectrometry (SIMS), and x-ray photoelectron. spectroscopy (XPS) were used to examine film crystallography, microstructure, and composition. A novel laboratory-based in-situ x-ray diffractometer was constructed. This new set-up allowed for the direct observation of microstructural evolution during growth. Films deposited at increasingly higher Ar pressures displayed a systematic decrease in grain size and degree of texturing, while surface morphology was found to vary from a nearly flat surface to a rough surface with several length scales of organization. In-situ x-ray results showed that the rate of texture evolution was found to be much higher in films grown using lower Ar pressures. These effects were studied in films less than 200 A thick using high resolution x-ray diffraction in conjunction with a synchrotron light source (SSRL B.L. 7-2). Films grown using higher Ar pressures (above 10 mTorr) with a pre-growth base pressure of 1 x 10--6 Torr had grains less than 10 nm in diameter and significant amorphous content Calculated radial distribution functions show a significant increase in average inter-atomic spacing in films grown using higher base pressures and Ar pressures. The amorphous content in the films was determined via comparison between ideal crystalline diffraction patterns and actual data. Thinner films grown at higher Ar pressures had relatively greater amorphous content. Real-time process control using the in-situ diffractometer was also demonstrated. The effects observed are discussed in the context of previous theories and experiments that document room-temperature sputter film growth. The changes in film microstructure observed were impurity mediated. Specifically, oxygen desorbed from the chamber walls during growth were incorporated into the film and subsequently limited grain development and texturing. A second phase consisting of amorphous Ta2O5 formed between the grain nuclei. Adatom kinetics played a role in determining surface morphology: at low Ar pressures (2 mTorr) significant adatom kinetic energies served to flattened the film surface, though impurity levels dominated grain development even in these conditions.

Dynamic fracture toughness of cellulose-fiber-reinforced polypropylene : preliminary investigation of microstructural effects

Treesearch

Craig M. Clemons; Daniel F. Caulfield; A. Jeffrey Giacomin

1999-10-01

In this study, the microstructure of injection-molded polypropylene reinforced with cellulose fiber was investigated. Scanning electron microscopy of the fracture surfaces and X-ray diffraction were used to investigate fiber orientation. The polypropylene matrix was removed by solvent extraction, and the lengths of the residual fibers were optically determined. Fiber...

Studies on densification, mechanical, micro-structural and structure–properties relationship of magnesium aluminate spinel refractory aggregates prepared from Indian magnesite

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

Ghosh, Chandrima; Ghosh, Arup; Haldar, Manas Kamal, E-mail: manashaldar@cgcri.res.in

The present work intends to study the development of magnesium aluminate spinel aggregates from Indian magnesite in a single firing stage. The raw magnesite has been evaluated in terms of chemical analysis, differential thermal analysis, thermogravimetric analysis, infrared spectroscopy, and X-ray diffraction. The experimental batch containing Indian magnesite and calcined alumina has been sintered in the temperature range of 1550 °C–1700 °C. The sintered material has been characterized in terms of physico-chemical properties like bulk density, apparent porosity, true density, relative density and thermo-mechanical/mechanical properties like hot modulus of rupture, thermal shock resistance, cold modulus of rupture and structural propertiesmore » by X-ray diffraction in terms of phase identification and evaluation of crystal structure parameters of corresponding phases by Rietveld analysis. The microstructures developed at different temperatures have been analyzed by field emission scanning electron microscope study and compositional analysis of the developed phase has been carried out by energy dispersive X-ray study. - Highlights: • The studies have been done to characterize the developed magnesium aluminate spinel. • The studies reveal correlation between refractory behavior of spinel and developed microstructures. • The studies show the values of lattice parameters of developed phases.« less

Crystallographic Characterization on Polycrystalline Ni-Mn-Ga Alloys with Strong Preferred Orientation.

PubMed

Li, Zongbin; Yang, Bo; Zou, Naifu; Zhang, Yudong; Esling, Claude; Gan, Weimin; Zhao, Xiang; Zuo, Liang

2017-04-27

Heusler type Ni-Mn-Ga ferromagnetic shape memory alloys can demonstrate excellent magnetic shape memory effect in single crystals. However, such effect in polycrystalline alloys is greatly weakened due to the random distribution of crystallographic orientation. Microstructure optimization and texture control are of great significance and challenge to improve the functional behaviors of polycrystalline alloys. In this paper, we summarize our recent progress on the microstructure control in polycrystalline Ni-Mn-Ga alloys in the form of bulk alloys, melt-spun ribbons and thin films, based on the detailed crystallographic characterizations through neutron diffraction, X-ray diffraction and electron backscatter diffraction. The presented results are expected to offer some guidelines for the microstructure modification and functional performance control of ferromagnetic shape memory alloys.

Synthesis of nanocrystalline CdS thin film by SILAR and their characterization

NASA Astrophysics Data System (ADS)

Mukherjee, A.; Satpati, B.; Bhattacharyya, S. R.; Ghosh, R.; Mitra, P.

2015-01-01

Cadmium sulphide (CdS) thin film was prepared by successive ion layer adsorption and reaction (SILAR) technique using ammonium sulphide as anionic precursor. Characterization techniques of XRD, SEM, TEM, FTIR and EDX were utilized to study the microstructure of the films. Structural characterization by x-ray diffraction reveals the polycrystalline nature of the films. Cubic structure is revealed from X-ray diffraction and selected area diffraction (SAD) patterns. The particle size estimated using X-ray line broadening method is approximately 7 nm. Instrumental broadening was taken into account while particle size estimation. TEM shows CdS nanoparticles in the range 5-15 nm. Elemental mapping using EFTEM reveals good stoichiometric composition of CdS. Characteristic stretching vibration mode of CdS was observed in the absorption band of FTIR spectrum. Optical absorption study exhibits a distinct blue shift in band gap energy value of about 2.56 eV which confirms the size quantization.

Density of bunched threading dislocations in epitaxial GaN layers as determined using X-ray diffraction

NASA Astrophysics Data System (ADS)

Barchuk, M.; Holý, V.; Rafaja, D.

2018-04-01

X-ray diffraction is one of the most popular experimental methods employed for determination of dislocation densities, as it can recognize both the strain fields and the local lattice rotations produced by dislocations. The main challenge of the quantitative analysis of the dislocation density is the formulation of a suitable microstructure model, which describes the dislocation arrangement and the effect of the interactions between the strain fields from neighboring dislocations reliably in order to be able to determine the dislocation densities precisely. The aim of this study is to prove the capability of X-ray diffraction and two computational methods, which are frequently used for quantification of the threading dislocation densities from X-ray diffraction measurements, in the special case of partially bunched threading dislocations. The first method is based on the analysis of the dislocation-controlled crystal mosaicity, and the other one on the analysis of diffuse X-ray scattering from threading dislocations. The complementarity of both methods is discussed. Furthermore, it is shown how the complementarity of these methods can be used to improve the results of the quantitative analysis of bunched and thus inhomogeneously distributed threading dislocations and to get a better insight into the dislocation arrangement.

In-situ investigation of stress-induced martensitic transformation in Ti–Nb binary alloys with low Young's modulus [In-situ high-energy X-ray diffraction investigation on stress-induced martensitic transformation in Ti-Nb binary alloys

DOE PAGES

Chang, L. L.; Wang, Y. D.; Ren, Y.

2015-11-04

Microstructure evolution, mechanical behaviors of cold rolled Ti-Nb alloys with different Nb contents subjected to different heat treatments were investigated. Here, optical microstructure and phase compositions of Ti-Nb alloys were characterized using optical microscopy and X-ray diffractometre, while mechanical behaviors of Ti-Nb alloys were examined by using tension tests. Stress-induced martensitic transformation in a Ti-30. at%Nb binary alloy was in-situ explored by synchrotron-based high-energy X-ray diffraction (HE-XRD). The results obtained suggested that mechanical behavior of Ti-Nb alloys, especially Young's modulus was directly dependent on chemical compositions and heat treatment process. According to the results of HE-XRD, α"-V1 martensite generated priormore » to the formation of α"-V2 during loading and a partial reversible transformation from α"-V1 to β phase was detected while α"-V2 tranformed to β completely during unloading.« less

Dislocation structure in textured zirconium tensile-deformed along rolling and transverse directions determined by X-ray diffraction line profile analysis

NASA Astrophysics Data System (ADS)

Fan, Zhijian; Jóni, Bertalan; Xie, Lei; Ribárik, Gábor; Ungár, Tamás

2018-04-01

Specimens of cold-rolled zirconium were tensile-deformed along the rolling (RD) and the transverse (TD) directions. The stress-strain curves revealed a strong texture dependence. High resolution X-ray line profile analysis was used to determine the prevailing active slip-systems in the specimens with different textures. The reflections in the X-ray diffraction patterns were separated into two groups. One group corresponds to the major and the other group to the random texture component, respectively. The dislocation densities, the subgrain size and the prevailing active slip-systems were evaluated by using the convolutional multiple whole profile (CMWP) procedure. These microstructure parameters were evaluated separately in the two groups of reflections corresponding to the two different texture components. Significant differences were found in both, the evolution of dislocation densities and the development of the fractions of and type slip systems in the RD and TD specimens during tensile deformation. The differences between the RD and TD stress-strain curves are discussed in terms of the differences of the microstructure evolution.

Impurity precipitation in atomized particles evidenced by nano x-ray diffraction computed tomography

NASA Astrophysics Data System (ADS)

Bonnin, Anne; Wright, Jonathan P.; Tucoulou, Rémi; Palancher, Hervé

2014-08-01

Performances and physical properties of high technology materials are influenced or even determined by their initial microstructure and by the behavior of impurity phases. Characterizing these impurities and their relations with the surrounding matrix is therefore of primary importance but it unfortunately often requires a destructive approach, with the risk of misinterpreting the observations. The improvement we have done in high resolution X-ray diffraction computed tomography combined with the use of an X-ray nanoprobe allows non-destructive crystallographic description of materials with microscopic heterogeneous microstructure (with a grain size between 10 nm and 10 μm). In this study, the grain localization in a 2D slice of a 20 μm solidified atomized γU-Mo particle is shown and a minority U(C,O) phase (1 wt. %) with sub-micrometer sized grains was characterized inside. Evidence is presented showing that the onset of U(C,O) grain crystallization can be described by a precipitation mechanism since one single U-Mo grain has direct orientation relationship with more than one surrounding U(C,O) grains.

International Conference (4th) on Nanostructured Materials Held in Stockholm, Sweden on 14-19 June 1998. Special Volume - Part A. Volume 12, Numbers 1-4, 1999

DTIC Science & Technology

1998-06-19

correlation was found between the X - ray grain size and the TEM grain size. Table 2 contains the hardness and density data for the nanocrystalline 5083...temperature with a Neophot hardness tester and a load of 0.2 N. RESULTS AND DISCUSSION X - ray diffraction and transmission electron microscopy combined with...For Single- Wall Carbon Nanotubes by Raman Scattering Technique Microstructure Change in Co46AI19035 Granular Thin Films by Annealing X - Ray

An instrument for in situ time-resolved X-ray imaging and diffraction of laser powder bed fusion additive manufacturing processes

NASA Astrophysics Data System (ADS)

Calta, Nicholas P.; Wang, Jenny; Kiss, Andrew M.; Martin, Aiden A.; Depond, Philip J.; Guss, Gabriel M.; Thampy, Vivek; Fong, Anthony Y.; Weker, Johanna Nelson; Stone, Kevin H.; Tassone, Christopher J.; Kramer, Matthew J.; Toney, Michael F.; Van Buuren, Anthony; Matthews, Manyalibo J.

2018-05-01

In situ X-ray-based measurements of the laser powder bed fusion (LPBF) additive manufacturing process produce unique data for model validation and improved process understanding. Synchrotron X-ray imaging and diffraction provide high resolution, bulk sensitive information with sufficient sampling rates to probe melt pool dynamics as well as phase and microstructure evolution. Here, we describe a laboratory-scale LPBF test bed designed to accommodate diffraction and imaging experiments at a synchrotron X-ray source during LPBF operation. We also present experimental results using Ti-6Al-4V, a widely used aerospace alloy, as a model system. Both imaging and diffraction experiments were carried out at the Stanford Synchrotron Radiation Lightsource. Melt pool dynamics were imaged at frame rates up to 4 kHz with a ˜1.1 μm effective pixel size and revealed the formation of keyhole pores along the melt track due to vapor recoil forces. Diffraction experiments at sampling rates of 1 kHz captured phase evolution and lattice contraction during the rapid cooling present in LPBF within a ˜50 × 100 μm area. We also discuss the utility of these measurements for model validation and process improvement.

An instrument for in situ time-resolved X-ray imaging and diffraction of laser powder bed fusion additive manufacturing processes.

PubMed

Calta, Nicholas P; Wang, Jenny; Kiss, Andrew M; Martin, Aiden A; Depond, Philip J; Guss, Gabriel M; Thampy, Vivek; Fong, Anthony Y; Weker, Johanna Nelson; Stone, Kevin H; Tassone, Christopher J; Kramer, Matthew J; Toney, Michael F; Van Buuren, Anthony; Matthews, Manyalibo J

2018-05-01

In situ X-ray-based measurements of the laser powder bed fusion (LPBF) additive manufacturing process produce unique data for model validation and improved process understanding. Synchrotron X-ray imaging and diffraction provide high resolution, bulk sensitive information with sufficient sampling rates to probe melt pool dynamics as well as phase and microstructure evolution. Here, we describe a laboratory-scale LPBF test bed designed to accommodate diffraction and imaging experiments at a synchrotron X-ray source during LPBF operation. We also present experimental results using Ti-6Al-4V, a widely used aerospace alloy, as a model system. Both imaging and diffraction experiments were carried out at the Stanford Synchrotron Radiation Lightsource. Melt pool dynamics were imaged at frame rates up to 4 kHz with a ∼1.1 μm effective pixel size and revealed the formation of keyhole pores along the melt track due to vapor recoil forces. Diffraction experiments at sampling rates of 1 kHz captured phase evolution and lattice contraction during the rapid cooling present in LPBF within a ∼50 × 100 μm area. We also discuss the utility of these measurements for model validation and process improvement.

An instrument for in situ time-resolved X-ray imaging and diffraction of laser powder bed fusion additive manufacturing processes

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

Calta, Nicholas P.; Wang, Jenny; Kiss, Andrew M.

In situ X-ray-based measurements of the laser powder bed fusion (LPBF) additive manufacturing process produce unique data for model validation and improved process understanding. Synchrotron X-ray imaging and diffraction provide high resolution, bulk sensitive information with sufficient sampling rates to probe melt pool dynamics as well as phase and microstructure evolution. Here, we describe a laboratory-scale LPBF test bed designed to accommodate diffraction and imaging experiments at a synchrotron X-ray source during LPBF operation. We also present experimental results using Ti-6Al-4V, a widely used aerospace alloy, as a model system. Both imaging and diffraction experiments were carried out at themore » Stanford Synchrotron Radiation Lightsource. Melt pool dynamics were imaged at frame rates up to 4 kHz with a ~1.1 μm effective pixel size and revealed the formation of keyhole pores along the melt track due to vapor recoil forces. Diffraction experiments at sampling rates of 1 kHz captured phase evolution and lattice contraction during the rapid cooling present in LPBF within a ~50 × 100 μm area. In conclusion, we also discuss the utility of these measurements for model validation and process improvement.« less

An instrument for in situ time-resolved X-ray imaging and diffraction of laser powder bed fusion additive manufacturing processes

DOE PAGES

Calta, Nicholas P.; Wang, Jenny; Kiss, Andrew M.; ...

2018-05-01

In situ X-ray-based measurements of the laser powder bed fusion (LPBF) additive manufacturing process produce unique data for model validation and improved process understanding. Synchrotron X-ray imaging and diffraction provide high resolution, bulk sensitive information with sufficient sampling rates to probe melt pool dynamics as well as phase and microstructure evolution. Here, we describe a laboratory-scale LPBF test bed designed to accommodate diffraction and imaging experiments at a synchrotron X-ray source during LPBF operation. We also present experimental results using Ti-6Al-4V, a widely used aerospace alloy, as a model system. Both imaging and diffraction experiments were carried out at themore » Stanford Synchrotron Radiation Lightsource. Melt pool dynamics were imaged at frame rates up to 4 kHz with a ~1.1 μm effective pixel size and revealed the formation of keyhole pores along the melt track due to vapor recoil forces. Diffraction experiments at sampling rates of 1 kHz captured phase evolution and lattice contraction during the rapid cooling present in LPBF within a ~50 × 100 μm area. In conclusion, we also discuss the utility of these measurements for model validation and process improvement.« less

Evaluation of Argon ion irradiation hardening of ferritic/martensitic steel-T91 using nanoindentation, X-ray diffraction and TEM techniques

NASA Astrophysics Data System (ADS)

Naveen Kumar, N.; Tewari, R.; Mukherjee, P.; Gayathri, N.; Durgaprasad, P. V.; Taki, G. S.; Krishna, J. B. M.; Sinha, A. K.; Pant, P.; Revally, A. K.; Dutta, B. K.; Dey, G. K.

2017-08-01

In the present study, microstructures of Ferritic-martensitic T-91 steel irradiated at room temperature for 5, 10 and 20 dpa using 315 KeV Ar+9 ions have been characterized by grazing incident X-ray diffraction (GIXRD) and by transmission electron microscopy (TEM). Line profiles of GIXRD patterns have shown that the size of domain continuously reduced with increasing dose of radiation. TEM investigations of irradiated samples have shown the presence of black dots, the number density of which decreases with increasing dose. Microstructures of irradiated samples have also revealed the presence of point defect clusters, such as dislocation loops and bubbles. In addition, dissolution of precipitates due to irradiation was also observed. Nano-indentation studies on the irradiated samples have shown saturation behavior in hardness as a function of dose which could be correlated with the changes in the yield strength of the alloy.

Mechanical properties of MEMS materials: reliability investigations by mechanical- and HRXRD-characterization related to environmental testing

NASA Astrophysics Data System (ADS)

Bandi, T.; Shea, H.; Neels, A.

2014-06-01

The performance and aging of MEMS often rely on the stability of the mechanical properties over time and under harsh conditions. An overview is given on methods to investigate small variations of the mechanical properties of structural MEMS materials by functional characterization, high-resolution x-ray diffraction methods (HR-XRD) and environmental testing. The measurement of the dynamical properties of micro-resonators is a powerful method for the investigation of elasticity variations in structures relevant to microtechnology. X-ray diffraction techniques are used to analyze residual strains and deformations with high accuracy and in a non-destructive manner at surfaces and in buried micro-structures. The influence of elevated temperatures and radiation damage on the performance of resonant microstructures with a focus on quartz and single crystal silicon is discussed and illustrated with examples including work done in our laboratories at CSEM and EPFL.

The microstructural characterization of an in situ grown Si{sub 3}N{sub 4} whisker-reinforced BAS glass-ceramic matrix composite

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

Yu, Feng; Ortiz-Longo, C.R.; White, K.W.

The microstructure of barium aluminum silicate (BAS)/silicon nitride in situ whisker reinforced ceramic matrix composite was examined by X-ray diffraction, transmission electron microscopy, electron diffraction and energy-dispersive X-ray microanalysis. Although the authors can not conclusively exclude the presence of orthorhombic BAS, hexagonal BAS and both {alpha}-Si{sub 3}N{sub 4} and {beta}-Si{sub 3}N{sub 4} were identified in this material. The {beta}-Si{sub 3}N{sub 4} whiskers nucleate and grow in random directions in the nearly continuous matrix of metastable hexacelsian. The crystallization process of the glass phase can be taken almost to completion but a small proportion of residual glass phase is present atmore » the interface and grains-junction. Both whisker-like and equiaxed {beta}-Si{sub 3}N{sub 4} exist in this material.« less

Twin density of aragonite in molluscan shells characterized using X-ray diffraction and transmission electron microscopy

NASA Astrophysics Data System (ADS)

Kogure, Toshihiro; Suzuki, Michio; Kim, Hyejin; Mukai, Hiroki; Checa, Antonio G.; Sasaki, Takenori; Nagasawa, Hiromichi

2014-07-01

{110} twin density in aragonites constituting various microstructures of molluscan shells has been characterized using X-ray diffraction (XRD) and transmission electron microscopy (TEM), to find the factors that determine the density in the shells. Several aragonite crystals of geological origin were also investigated for comparison. The twin density is strongly dependent on the microstructures and species of the shells. The nacreous structure has a very low twin density regardless of the shell classes. On the other hand, the twin density in the crossed-lamellar (CL) structure has large variation among classes or subclasses, which is mainly related to the crystallographic direction of the constituting aragonite fibers. TEM observation suggests two types of twin structures in aragonite crystals with dense {110} twins: rather regulated polysynthetic twins with parallel twin planes, and unregulated polycyclic ones with two or three directions for the twin planes. The former is probably characteristic in the CL structures of specific subclasses of Gastropoda. The latter type is probably related to the crystal boundaries dominated by (hk0) interfaces in the microstructures with preferred orientation of the c-axis, and the twin density is mainly correlated to the crystal size in the microstructures.

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.

Quantitative microstructural imaging by scanning Laue x-ray micro- and nanodiffraction

DOE PAGES

Chen, Xian; Dejoie, Catherine; Jiang, Tengfei; ...

2016-06-08

We present that local crystal structure, crystal orientation, and crystal deformation can all be probed by Laue diffraction using a submicron x-ray beam. This technique, employed at a synchrotron facility, is particularly suitable for fast mapping the mechanical and microstructural properties of inhomogeneous multiphase polycrystalline samples, as well as imperfect epitaxial films or crystals. As synchrotron Laue x-ray microdiffraction enters its 20th year of existence and new synchrotron nanoprobe facilities are being built and commissioned around the world, we take the opportunity to overview current capabilities as well as the latest technical developments. Fast data collection provided by state-of-the-art areamore » detectors and fully automated pattern indexing algorithms optimized for speed make it possible to map large portions of a sample with fine step size and obtain quantitative images of its microstructure in near real time. Lastly, we extrapolate how the technique is anticipated to evolve in the near future and its potential emerging applications at a free-electron laser facility.« less

The microstructural changes of Ge2Sb2Te5 thin film during crystallization process

NASA Astrophysics Data System (ADS)

Xu, Jingbo; Qi, Chao; Chen, Limin; Zheng, Long; Xie, Qiyun

2018-05-01

Phase change memory is known as the most promising candidate for the next generation nonvolatile memory technology. In this paper, the microstructural changes of Ge2Sb2Te5 film, which is the most common choice of phase change memory material, has been carefully studied by the combination of several characterization techniques. The combination of resistance measurements, X-ray diffraction, Raman spectroscopy and X-ray reflectivity allows us to simultaneously extract the characteristics of microstructural changes during crystallization process. The existence of surface/interface Ge2Sb2Te5 layer has been proposed here based on X-ray reflectivity measurements. Although the total film thickness decreases, as a result of the phase transition from amorphous to metastable crystalline cubic and then to the stable hexagonal phase, the surface/interface thickness increases after crystallization. Moreover, the increase of average grain size, density and surface roughness has been confirmed during thermal annealing process.

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.

Crystallographic Characterization on Polycrystalline Ni-Mn-Ga Alloys with Strong Preferred Orientation

PubMed Central

Li, Zongbin; Yang, Bo; Zou, Naifu; Zhang, Yudong; Esling, Claude; Gan, Weimin; Zhao, Xiang; Zuo, Liang

2017-01-01

Heusler type Ni-Mn-Ga ferromagnetic shape memory alloys can demonstrate excellent magnetic shape memory effect in single crystals. However, such effect in polycrystalline alloys is greatly weakened due to the random distribution of crystallographic orientation. Microstructure optimization and texture control are of great significance and challenge to improve the functional behaviors of polycrystalline alloys. In this paper, we summarize our recent progress on the microstructure control in polycrystalline Ni-Mn-Ga alloys in the form of bulk alloys, melt-spun ribbons and thin films, based on the detailed crystallographic characterizations through neutron diffraction, X-ray diffraction and electron backscatter diffraction. The presented results are expected to offer some guidelines for the microstructure modification and functional performance control of ferromagnetic shape memory alloys. PMID:28772826

Determining Individual Phase Flow Properties in a Quench and Partitioning Steel with In Situ High-Energy X-Ray Diffraction and Multiphase Elasto-Plastic Self-Consistent Method

NASA Astrophysics Data System (ADS)

Hu, Xiaohua; Choi, Kyoo Sil; Sun, Xin; Ren, Yang; Wang, Yangdong

2016-12-01

The micromechanical properties of the constituent phases were characterized for advanced high-strength steels (AHSS) produced by a quenching and partitioning (Q&P) process with in situ tensile loading under synchrotron-based, high-energy X-ray diffraction. The constituent phases present are retained austenite and three martensites (tempered, untampered, and freshly formed martensites). For the material investigated, the 200 and 220 lattice strains of the retained austenite phase were calculated by examining the changes of the X-ray diffraction peak positions during deformation. The 200 and 211 lattice strains of the various martensitic phases with similar crystal structures were determined by separating their overlapped diffraction peaks. Apart from tempered and untempered martensite, the diffraction peaks of freshly formed martensite as a result of austenite-to-martensite transformation can also be separated due to a high initial austenite volume fraction. The phase stresses are first estimated with an empirical relationship through the X-ray diffraction elastic constants. A multiphase elasto-plastic self-consistent model is next used for more accurate determination of the constitutive behaviors of the various phases by comparing the predicted lattice strain distributions and global stress-strain curves with the measured ones. The determined constitutive laws will be used for microstructure-based modeling for sheet formability of the Q&P AHSS steel.

Influence of nanogold additives on phase formation, microstructure and dielectric properties of perovskite BaTiO3 ceramics

NASA Astrophysics Data System (ADS)

Nonkumwong, Jeeranan; Ananta, Supon; Srisombat, Laongnuan

2015-06-01

The formation of perovskite phase, microstructure and dielectric properties of nanogold-modified barium titanate (BaTiO3) ceramics was examined as a function of gold nanoparticle contents by employing a combination of X-ray diffraction, scanning electron microscopy, energy-dispersive X-ray, Archimedes principle and dielectric measurement techniques. These ceramics were fabricated from a simple mixed-oxide method. The amount of gold nanoparticles was found to be one of the key factors controlling densification, grain growth and dielectric response in BaTiO3 ceramics. It was found that under suitable amount of nanogold addition (4 mol%), highly dense perovskite BaTiO3 ceramics with homogeneous microstructures of refined grains (~0.5-3.1 μm) and excellence dielectric properties can be produced.

Synthesis of Novel Sea-Urchin-Like CdS and Their Optical Properties.

PubMed

Kamran, Muhammad Arshad; Liu, Ruibin; Shi, Li-Jie; Bukhtiar, Arfan; Li, Jing; Zou, Bingsuo

2015-06-01

A novel morphology of CdS sea-urchin-like microstructures is synthesized by simple thermal evaporation process. Microstructures with average size of 20-50 μm are composed of single crystalline CdS nanobelts. The structural, compositional, morphological characterization of the product were examined by X-ray diffraction, energy dispersive X-ray spectroscopy, Raman spectroscopy, scanning electron microscope, transmission electron microscopy and selected area electron diffraction while optical properties are investigated by Photoluminescence spectroscopy and time-resolved Photoluminescence measurements. The tentative growth mechanism for the growth of sea-urchin-like CdS is proposed and described briefly. A strong green emission with a maximum around 517 nm was observed from the individual CdS microstructure at room temperature, which was attributed to band-edge emission of CdS. These Novel structures exhibit excellent lasing (stimulated emission) with low threshold (9.07 μJ cm(-2)) at room temperature. We analyze the physical mechanism of stimulated emission. These results are important in the design of green luminescence, low-threshold laser and display devices in the future.

Relationships Between the Phase Transformation Kinetics, Texture Evolution, and Microstructure Development in a 304L Stainless Steel Under Biaxial Loading Conditions: Synchrotron X-ray and Electron Backscatter Diffraction Studies

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

Cakmak, Ercan; Choo, Hahn; Kang, Jun-Yun

2015-02-11

The relationships between the martensitic phase transformation kinetics, texture evolution, and the microstructure development in the parent austenite phase were studied for a 304L stainless steel that exhibits the transformation-induced plasticity effect under biaxial loading conditions at ambient temperature. The applied loading paths included: pure torsion, simultaneous biaxial torsion/tension, simultaneous biaxial torsion/compression, and stepwise loading of tension followed by torsion (i.e., first loading by uniaxial tension and then by pure torsion in sequence). Synchrotron X-ray and electron backscatter diffraction techniques were used to measure the evolution of the phase fractions, textures, and microstructures as a function of the applied strains.more » The influence of loading character and path on the changes in martensitic phase transformation kinetics is discussed in the context of (1) texture-transformation relationship and the preferred transformation of grains belonging to certain texture components over the others, (2) effects of axial strains on shear band evolutions, and (3) volume changes associated with martensitic transformation.« less

Mesoscale evolution of voids and microstructural changes in HMX-based explosives during heating through the β-δ phase transition

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

Willey, Trevor M., E-mail: willey1@llnl.gov; Lauderbach, Lisa; Gagliardi, Franco

HMX-based explosives LX-10 and PBX-9501 were heated through the β-δ phase transition. Ultra-small angle x-ray scattering (USAXS) and molecular diffraction were simultaneously recorded as the HMX was heated. Mesoscale voids and structure dramatically change promptly with the β-δ phase transition, rather than with other thermal effects. Also, x-ray induced damage, observed in the USAXS, occurs more readily at elevated temperatures; as such, the dose was reduced to mitigate this effect. Optical microscopy performed during a similar heating cycle gives an indication of changes on longer length scales, while x-ray microtomography, performed before and after heating, shows the character of extensivemore » microstructural damage resulting from the temperature cycle and solid-state phase transition.« less

Mesoscale evolution of voids and microstructural changes in HMX-based explosives during heating through the β-δ phase transition

DOE PAGES

Willey, Trevor M.; Lauderbach, Lisa; Gagliardi, Franco; ...

2015-08-07

HMX-based explosives LX-10 and PBX-9501 were heated through the β-δ phase transition. Ultra-small angle x-ray scattering (USAXS) and molecular diffraction were simultaneously recorded as the HMX was heated. Mesoscale voids and structure dramatically change promptly with the β-δ phase transition, rather than with other thermal effects. Also, x-ray induced damage, observed in the USAXS, occurs more readily at elevated temperatures; as such, the dose was reduced to mitigate this effect. Optical microscopy performed during a similar heating cycle gives an indication of changes on longer length scales, while x-ray microtomography, performed before and after heating, shows the character of extensivemore » microstructural damage resulting from the temperature cycle and solid-state phase transition.« less

Synchrotron X-ray diffraction investigations on strains in the oxide layer of an irradiated Zircaloy fuel cladding

NASA Astrophysics Data System (ADS)

Chollet, Mélanie; Valance, Stéphane; Abolhassani, Sousan; Stein, Gene; Grolimund, Daniel; Martin, Matthias; Bertsch, Johannes

2017-05-01

For the first time the microstructure of the oxide layer of a Zircaloy-2 cladding after 9 cycles of irradiation in a boiling water reactor has been analyzed with synchrotron micro-X-ray diffraction. Crystallographic strains of the monoclinic and to some extent of the tetragonal ZrO2 are depicted through the thick oxide layer. Thin layers of sub-oxide at the oxide-metal interface as found for autoclave-tested samples and described in the literature, have not been observed in this material maybe resulting from irradiation damage. Shifts of selected diffraction peaks of the monoclinic oxide show that the uniform strain produced during oxidation is orientated in the lattice and displays variations along the oxide layer. Diffraction peaks and their shifts from families of diffracting planes could be translated into a virtual tensor. This virtual tensor exhibits changes through the oxide layer passing by tensile or compressive components.

Simulations of in situ x-ray diffraction from uniaxially compressed highly textured polycrystalline targets

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

McGonegle, David, E-mail: d.mcgonegle1@physics.ox.ac.uk; Wark, Justin S.; Higginbotham, Andrew

2015-08-14

A growing number of shock compression experiments, especially those involving laser compression, are taking advantage of in situ x-ray diffraction as a tool to interrogate structure and microstructure evolution. Although these experiments are becoming increasingly sophisticated, there has been little work on exploiting the textured nature of polycrystalline targets to gain information on sample response. Here, we describe how to generate simulated x-ray diffraction patterns from materials with an arbitrary texture function subject to a general deformation gradient. We will present simulations of Debye-Scherrer x-ray diffraction from highly textured polycrystalline targets that have been subjected to uniaxial compression, as maymore » occur under planar shock conditions. In particular, we study samples with a fibre texture, and find that the azimuthal dependence of the diffraction patterns contains information that, in principle, affords discrimination between a number of similar shock-deformation mechanisms. For certain cases, we compare our method with results obtained by taking the Fourier transform of the atomic positions calculated by classical molecular dynamics simulations. Illustrative results are presented for the shock-induced α–ϵ phase transition in iron, the α–ω transition in titanium and deformation due to twinning in tantalum that is initially preferentially textured along [001] and [011]. The simulations are relevant to experiments that can now be performed using 4th generation light sources, where single-shot x-ray diffraction patterns from crystals compressed via laser-ablation can be obtained on timescales shorter than a phonon period.« less

Simulations of in situ x-ray diffraction from uniaxially compressed highly textured polycrystalline targets

DOE PAGES

McGonegle, David; Milathianaki, Despina; Remington, Bruce A.; ...

2015-08-11

A growing number of shock compression experiments, especially those involving laser compression, are taking advantage of in situ x-ray diffraction as a tool to interrogate structure and microstructure evolution. Although these experiments are becoming increasingly sophisticated, there has been little work on exploiting the textured nature of polycrystalline targets to gain information on sample response. Here, we describe how to generate simulated x-ray diffraction patterns from materials with an arbitrary texture function subject to a general deformation gradient. We will present simulations of Debye-Scherrer x-ray diffraction from highly textured polycrystalline targets that have been subjected to uniaxial compression, as maymore » occur under planar shock conditions. In particular, we study samples with a fibre texture, and find that the azimuthal dependence of the diffraction patterns contains information that, in principle, affords discrimination between a number of similar shock-deformation mechanisms. For certain cases, we compare our method with results obtained by taking the Fourier transform of the atomic positions calculated by classical molecular dynamics simulations. Illustrative results are presented for the shock-induced α–ϵ phase transition in iron, the α–ω transition in titanium and deformation due to twinning in tantalum that is initially preferentially textured along [001] and [011]. In conclusion, the simulations are relevant to experiments that can now be performed using 4th generation light sources, where single-shot x-ray diffraction patterns from crystals compressed via laser-ablation can be obtained on timescales shorter than a phonon period.« less

Synthesis of nanostructured vanadium powder by high-energy ball milling: X-ray diffraction and high-resolution electron microscopy characterization

NASA Astrophysics Data System (ADS)

Krishnan, Vinoadh Kumar; Sinnaeruvadi, Kumaran

2016-10-01

Vanadium metal powders, ball milled with different surfactants viz., stearic acid, KCl and NaCl, have been studied by X-ray diffraction and transmission electron microscopy. The surfactants alter the microstructural and morphological characteristics of the powders. Ball milling with stearic acid results in solid-state amorphization, while powders milled with KCl yield vanadium-tungsten carbide nanocomposite mixtures. NaCl proved to be an excellent surfactant for obtaining nanostructured fusion-grade vanadium powders. In order to understand the reaction mechanism behind any interstitial addition in the ball-milled powders, CHNOS analysis was performed.

3D Microstructural Architectures for Metal and Alloy Components Fabricated by 3D Printing/Additive Manufacturing Technologies

NASA Astrophysics Data System (ADS)

Martinez, E.; Murr, L. E.; Amato, K. N.; Hernandez, J.; Shindo, P. W.; Gaytan, S. M.; Ramirez, D. A.; Medina, F.; Wicker, R. B.

The layer-by-layer building of monolithic, 3D metal components from selectively melted powder layers using laser or electron beams is a novel form of 3D printing or additive manufacturing. Microstructures created in these 3D products can involve novel, directional solidification structures which can include crystallographically oriented grains containing columnar arrays of precipitates characteristic of a microstructural architecture. These microstructural architectures are advantageously rendered in 3D image constructions involving light optical microscopy and scanning and transmission electron microscopy observations. Microstructural evolution can also be effectively examined through 3D image sequences which, along with x-ray diffraction (XRD) analysis in the x-y and x-z planes, can effectively characterize related crystallographic/texture variances. This paper compares 3D microstructural architectures in Co-base and Ni-base superalloys, columnar martensitic grain structures in 17-4 PH alloy, and columnar copper oxides and dislocation arrays in copper.

Effect of processing on the microstructure of finger millet by X-ray diffraction and scanning electron microscopy.

PubMed

Dharmaraj, Usha; Parameswara, P; Somashekar, R; Malleshi, Nagappa G

2014-03-01

Finger millet is one of the important minor cereals, and carbohydrates form its major chemical constituent. Recently, the millet is processed to prepare hydrothermally treated (HM), decorticated (DM), expanded (EM) and popped (PM) products. The present research aims to study the changes in the microstructure of carbohydrates using X-ray diffraction and scanning electron microscopy. Processing the millet brought in significant changes in the carbohydrates. The native millet exhibited A-type pattern of X-ray diffraction with major peaks at 2θ values of 15.3, 17.86 and 23.15°, whereas, all other products showed V-type pattern with single major peak at 2θ values ranging from 19.39 to 19.81°. The corresponding lattice spacing and the number of unit cells in a particular direction of reflection also reduced revealing that crystallinity of starch has been decreased depending upon the processing conditions. Scanning electron microscopic studies also revealed that the orderly pattern of starch granules changed into a coherent mass due to hydrothermal treatment, while high temperature short time treatment rendered a honey-comb like structure to the product. However, the total carbohydrates and non-starch polysaccharide contents almost remained the same in all the products except for DM and EM, but the individual carbohydrate components changed significantly depending on the type of processing.

Effect of annealing conditions on the microstructure and magnetic properties of sintered Nd-Fe-B magnets as seen by magnetic small-angle neutron scattering

NASA Astrophysics Data System (ADS)

Périgo, Élio A.; Titov, Ivan; Weber, Raoul; Mettus, Denis; Peral, Inma; Vallcorba, Oriol; Honecker, Dirk; Feoktystov, Artem; Michels, Andreas

2018-03-01

We have investigated the effect of the annealing conditions (heating rate and temperature) on the magnetic microstructure of sintered Nd-Fe-B magnets by means of magnetometry, scanning electron microscopy, high-energy synchrotron x-ray diffraction, and small-angle neutron scattering (SANS). While the temperature treatment has a strong effect on the coercivity (reduction by about 50% on annealing), the associated changes in the microstructure do surprisingly not show up (or at best only very weakly) in the neutron-scattering signal, which probes a mesoscopic real-space length scale ranging between about 1–300 nm. On the other hand, the x-ray data reveal microstructural changes in the Nd-rich phases, presumably due to modifications in grain-boundary regions. Moreover, we observe an unusual diamond-shaped angular anisotropy in the SANS cross section, which strongly points towards the existence of texture in the nuclear microstructure.

Impact load-induced micro-structural damage and micro-structure associated mechanical response of concrete made with different surface roughness and porosity aggregates

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

Erdem, Savas, E-mail: evxse1@nottingham.ac.uk; Dawson, Andrew Robert; Thom, Nicholas Howard

2012-02-15

The relationship between the nature of micro damage under impact loading and changes in mechanical behavior associated with different microstructures is studied for concretes made with two different coarse aggregates having significant differences mainly in roughness and porosity - sintered fly ash and uncrushed gravel. A range of techniques including X-ray diffraction, digital image analysis, mercury porosimetry, X-ray computed tomography, laser surface profilometry and scanning electron microscopy were used to characterize the aggregates and micro-structures. The concrete prepared with lightweight aggregates was stronger in compression than the gravel aggregate concrete due to enhanced hydration as a result of internal curing.more » In the lightweight concrete, it was deduced that an inhomogeneous micro-structure led to strain incompatibilities and consequent localized stress concentrations in the mix, leading to accelerated failure. The pore structure, compressibility, and surface texture of the aggregates are of paramount importance for the micro-cracking growth.« less

Microstructural evolution of neutron irradiated 3C-SiC

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

Sprouster, David J.; Koyanagi, Takaaki; Dooryhee, Eric

The microstructural response of neutron irradiated 3C-SiC have been investigated over a wide irradiation temperature and fluence range via qualitative and quantitative synchrotron-based X-ray diffraction characterization. Here, we identify several neutron fluence- and irradiation temperature-dependent changes in the microstructure, and directly highlight the specific defects introduced through the course of irradiation. By quantifying the microstructure, we aim to develop a more detailed understanding of the radiation response of SiC. Such studies are important to build mechanistic models of material performance and to understand the susceptibility of various microstructures to radiation damage for advanced energy applications.

Microstructural evolution of neutron irradiated 3C-SiC

DOE PAGES

Sprouster, David J.; Koyanagi, Takaaki; Dooryhee, Eric; ...

2017-03-18

The microstructural response of neutron irradiated 3C-SiC have been investigated over a wide irradiation temperature and fluence range via qualitative and quantitative synchrotron-based X-ray diffraction characterization. Here, we identify several neutron fluence- and irradiation temperature-dependent changes in the microstructure, and directly highlight the specific defects introduced through the course of irradiation. By quantifying the microstructure, we aim to develop a more detailed understanding of the radiation response of SiC. Such studies are important to build mechanistic models of material performance and to understand the susceptibility of various microstructures to radiation damage for advanced energy applications.

X-ray diffraction and Raman investigations of thickness dependent stress effects on Pb(ZrxTi1-x)O3 thin films

NASA Astrophysics Data System (ADS)

Lappalainen, Jyrki; Lantto, Vilho; Frantti, Johannes; Hiltunen, Jussi

2006-06-01

Microstructure, film orientation, and optical transmission spectra of polycrystalline Nd-modified Pb(ZrxTi1-x)O3 films were studied as a function of film thickness. Pulsed laser deposition was used for the fabrication of films with thickness from 80to465nm on single-crystal MgO(100) substrates. Raman spectroscopy, x-ray diffraction, and spectrophotometry measurements were utilized in the film characterization. With the decreasing film thickness, films first oriented with c axis perpendicular to film surface, and then, after some critical thickness, changed to a-axis orientation. At the same time, compressive stress increased up to 1.3GPa and a clear blueshift of the optical absorption edge was found in transmission spectra.

Evolution processes of the corrosion behavior and structural characteristics of plasma electrolytic oxidation coatings on AZ31 magnesium alloy

NASA Astrophysics Data System (ADS)

Chen, Dong; Wang, Ruiqiang; Huang, Zhiquan; Wu, Yekang; Zhang, Yi; Wu, Guorui; Li, Dalong; Guo, Changhong; Jiang, Guirong; Yu, Shengxue; Shen, Dejiu; Nash, Philip

2018-03-01

Evolution processes of the corrosion behavior and structural characteristics of the plasma electrolytic oxidation (PEO) coated AZ31 magnesium alloy were investigated by using scanning electron microscope (SEM) equipped with energy dispersive X-ray spectroscopy (EDS), X-ray diffraction (XRD), potentio-dynamic polarization curves and electrochemical impedance spectroscopy (EIS) measurements. Detached coating samples were fabricated by an electrochemical method and more details of the internal micro-structure of coatings were clearly observed on the fractured cross-section morphologies of the samples compared to general polished cross-section morphologies. Evolution mechanisms of the coating corrosion behavior in relation to the evolution of micro-structural characteristics were discussed in detail.

Effect of chromium underlayer on the properties of nano-crystalline diamond films

NASA Astrophysics Data System (ADS)

Garratt, E.; AlFaify, S.; Yoshitake, T.; Katamune, Y.; Bowden, M.; Nandasiri, M.; Ghantasala, M.; Mancini, D. C.; Thevuthasan, S.; Kayani, A.

2013-01-01

This paper investigated the effect of chromium underlayer on the structure, microstructure, and composition of the nano-crystalline diamond films. Nano-crystalline diamond thin films were deposited at high temperature in microwave-induced plasma diluted with nitrogen, on single crystal silicon substrate with a thin film of chromium as an underlayer. Characterization of the film was implemented using non-Rutherford backscattering spectrometry, Raman spectroscopy, near-edge x-ray absorption fine structure, x-ray diffraction, and atomic force microscopy. Nanoindentation studies showed that the films deposited on chromium underlayer have higher hardness values compared to those deposited on silicon without an underlayer. Diamond and graphitic phases of the films evaluated by x-ray and optical spectroscopic analyses determined consistency between the sp2 and sp3 phases of carbon in chromium sample to that of diamond grown on silicon. Diffusion of chromium was observed using ion beam analysis which was correlated with the formation of chromium complexes by x-ray diffraction.

Microstructure and Properties of Fe3Al-Fe3AlC x Composite Prepared by Reactive Liquid Processing

NASA Astrophysics Data System (ADS)

Verona, Maria Nalu; Setti, Dalmarino; Paredes, Ramón Sigifredo Cortés

2018-04-01

A Fe3Al-Fe3AlC x composite was prepared using reactive liquid processing (RLP) through controlled mixture of carbon steel and aluminum in the liquid state. The microstructure and phases of the composite were assessed using X-ray diffraction, scanning electron microscopy, energy-dispersive X-ray spectroscopy, optical microscopy, and differential scanning calorimetry. In addition, the density, hardness, microhardness, and elastic modulus were evaluated. The Fe3Al-Fe3AlC x composite consisted of 65 vol pct Fe3Al and 35 vol pct Fe3AlC x ( κ). The κ phase contained 10.62 at. pct C, resulting in the stoichiometry Fe3AlC0.475. The elastic modulus of the Fe3Al-Fe3AlC0.475 composite followed the rule of mixtures. The RLP technique was shown to be capable of producing Fe3Al-Fe3AlC0.475 with a microstructure and properties similar to those achieved using other processing techniques reported in the literature.

Optical properties of cerium oxide (CeO2) nanoparticles synthesized by hydroxide mediated method

NASA Astrophysics Data System (ADS)

Ali, Mawlood Maajal; Mahdi, Hadeel Salih; Parveen, Azra; Azam, Ameer

2018-05-01

The nanoparticles of cerium oxide have been successfully synthesized by hydroxide mediated method, using cerium nitrate and sodium hydroxide as precursors. The microstructural properties were analyzed by X-ray diffraction technique (XRD). The X-ray diffraction results show that the cerium oxide nanoparticles were in cubic structure. The optical absorption spectra of cerium oxide were recorded by UV-VIS spectrophotometer in the range of 320 to 600 nm and photoluminescence spectra in the range of 400-540 nm and have been presented. The energy band gap was determined by Tauc relationship. The crystallite size was determined from Debye-Scherer equation and came out to be 6.4 nm.

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

X-ray investigation of cross-breed silk in cocoon, yarn and fabric forms

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

Radhalakshmi, Y. C.; Kariappa,; Siddaraju, G. N.

2012-06-05

Recently Central Sericulture Research and Training Institute, Mysore developed many improved cross breeds and bivoltine hybrids. Newly developed cross breeds recorded fibre characteristics which are significantly superior over existing control hybrids. This aspect has been investigated using X-ray diffraction technique. We have employed line profile analysis to compute microstructural parameters. These parameters are compared with physical parameters of newly developed cross breed silk fibers for a better understanding of structure-property relation in these samples.

Relationships Between the Phase Transformation Kinetics, Texture Evolution, and Microstructure Development in a 304L Stainless Steel Under Biaxial Loading Conditions: Synchrotron X-ray and Electron Backscatter Diffraction Studies

DOE PAGES

Cakmak, Ercan; Choo, Hahn; Kang, Jun-Yun; ...

2015-02-11

Here we report that the relationships between the martensitic phase transformation kinetics, texture evolution, and the microstructure development in the parent austenite phase were studied for a 304L stainless steel that exhibits the transformation-induced plasticity effect under biaxial loading conditions at ambient temperature. The applied loading paths included: pure torsion, simultaneous biaxial torsion/tension, simultaneous biaxial torsion/compression, and stepwise loading of tension followed by torsion (i.e., first loading by uniaxial tension and then by pure torsion in sequence). Synchrotron X-ray and electron backscatter diffraction techniques were used to measure the evolution of the phase fractions, textures, and microstructures as a functionmore » of the applied strains. The influence of loading character and path on the changes in martensitic phase transformation kinetics is discussed in the context of (1) texture-transformation relationship and the preferred transformation of grains belonging to certain texture components over the others, (2) effects of axial strains on shear band evolutions, and (3) volume changes associated with martensitic transformation.« less

Structural, microstructural and magnetic evolution in cryo milled carbon doped MnAl.

PubMed

Fang, Hailiang; Cedervall, Johan; Hedlund, Daniel; Shafeie, Samrand; Deledda, Stefano; Olsson, Fredrik; von Fieandt, Linus; Bednarcik, Jozef; Svedlindh, Peter; Gunnarsson, Klas; Sahlberg, Martin

2018-02-06

The low cost, rare earth free τ-phase of MnAl has high potential to partially replace bonded Nd 2 Fe 14 B rare earth permanent magnets. However, the τ-phase is metastable and it is experimentally difficult to obtain powders suitable for the permanent magnet alignment process, which requires the fine powders to have an appropriate microstructure and high τ-phase purity. In this work, a new method to make high purity τ-phase fine powders is presented. A high purity τ-phase Mn 0.55 Al 0.45 C 0.02 alloy was synthesized by the drop synthesis method. The drop synthesized material was subjected to cryo milling and  followed by a flash heating process. The crystal structure and microstructure of the drop synthesized, cryo milled and flash heated samples were studied by X-ray in situ powder diffraction, scanning electron microscopy, X-ray energy dispersive spectroscopy and electron backscatter diffraction. Magnetic properties and magnetic structure of the drop synthesized, cryo milled, flash heated  samples were characterized by magnetometry and neutron powder diffraction, respectively. The results reveal that the 2 and 4 hours cryo milled and flash heated samples both exhibit high τ-phase purity and micron-sized round particle shapes. Moreover, the flash heated samples display high saturation magnetization as well as increased coercivity.

Effects of the Tempering and High-Pressure Torsion Temperatures on Microstructure of Ferritic/Martensitic Steel Grade 91

PubMed Central

Ganeev, Artur; Nikitina, Marina; Sitdikov, Vil; Islamgaliev, Rinat; Hoffman, Andrew; Wen, Haiming

2018-01-01

Grade 91 (9Cr-1Mo) steel was subjected to various heat treatments and then to high-pressure torsion (HPT) at different temperatures. Its microstructure was studied using transmission electron microscopy (TEM) and X-ray diffraction (XRD). Effects of the tempering temperature and the HPT temperature on the microstructural features and microhardness in the ultrafine-grained (UFG) Grade 91 steel were researched. The study of the UFG structure formation takes into account two different microstructures observed: before HPT in both samples containing martensite and in fully ferritic samples. PMID:29671761

Microstructural characteristics of Hadfield steel solidified under high pressure

NASA Astrophysics Data System (ADS)

Zhang, Yuzi; Li, Yanguo; Han, Bo; Zhang, Fucheng; Qian, Lihe

2011-12-01

Samples of Hadfield steel, high manganese austenite steel with 13 wt% manganese and 1.2 wt% carbon, were solidified under a pressure of 6 GPa. The microstructures of the samples were analyzed by metallography and X-ray diffraction. The results indicate that the solidification microstructure of the Hadfield steel was remarkably refined under high pressure. Additionally, the carbide of M23C6 was obtained in the Hadfield steel solidified under high pressure was different from the carbide of M3C obtained by solidification under normal pressure. Furthermore, high pressure promoted the formation of orientational solidified microstructure of the Hadfield steel.

Computation of Bragg Reflection for Layered Microstructures

NASA Technical Reports Server (NTRS)

Underwood, J. W.; Barbee, T. W.

1984-01-01

Bragg diffractors analyzed for use in X-ray mirrors and other applications. SLM tailored to specific applications by varying layer thicknesses and number of layers to control reflectivity diffraction width, and wavelength resolution. Applications as glancing incidence mirrors or filters for wavelengths of few to few hundred angstroms.

Nanocrystalline ferroelectric BaTiO3/Pt/fused silica for implants synthetized by pulsed laser deposition method

NASA Astrophysics Data System (ADS)

Jelínek, Miroslav; Drahokoupil, Jan; Jurek, Karel; Kocourek, Tomáš; Vaněk, Přemysl

2017-09-01

The thin-films of BaTiO3 (BTO)/Pt were prepared to test their potential as coatings for titanium-alloy implants. The nanocrystalline BTO/Pt bi-layers were successfully synthesized using fused silica as substrates. The bi-layers were prepared using KrF excimer laser ablation at substrate temperatures (Ts) ranging from 650 °C to 750 °C. The microstructure and composition of the deposits were investigated by scanning electron microscope, x-ray diffraction and wavelength dispersive x-ray spectroscopy methods. The electrical characterization of the Pt/BTO/Pt capacitors indicated ferroelectric-type response in BTO films containing (40-140) nm-sized grains. The technology, microstructure, and functional response of the layers are presented in detail.

Evolution of Microstructure in a Nickel-based Superalloy as a Function of Ageing Time

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

Chen, Wei-Ren; Smith, Gregory Scott; Porcar, L.

2011-01-01

An experimental investigation, combining synchrotron X-ray powder diffraction, small-angle neutron-scattering, and transmission electron microscopy, has been undertaken to study the microstructure of nanoprecipitates in a nickel-based superalloy. Upon increasing the ageing time during a heat-treatment process, the average size of the precipitates first decreases before changing to a monotonical growth stage. Possible reasons for this observed structural evolution, which is predicted thermodynamically, are suggested.

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

Sicupira, Felipe Lucas; Sandim, Maria José R.; Sandim, Hugo R.Z.

The good performance of supermartensitic stainless steels is strongly dependent on the volume fraction of retained austenite at room temperature. The present work investigates the effect of secondary tempering temperatures on this phase transformation and quantifies the amount of retained austenite by X-ray diffraction and saturation magnetization. The steel samples were tempered for 1 h within a temperature range of 600–800 °C. The microstructure was characterized using scanning electron microscopy and electron backscatter diffraction. Results show that the amount of retained austenite decreased with increasing secondary tempering temperature in both quantification methods. - Highlights: • The phase transformation during secondarymore » tempering temperatures was observed. • Phases were quantified by X-ray diffraction and DC-saturation magnetization. • More retained austenite forms with increasing secondary tempering temperature. • The retained austenite is mainly located at the grain and lath boundaries.« less

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

Microstructure and properties of laser-clad high-temperature wear-resistant alloys

NASA Astrophysics Data System (ADS)

Yang, Yongqiang

1999-02-01

A 2-kW CO 2 laser with a powder feeder was used to produce alloy coatings with high temperature-wear resistance on the surface of steel substrates. To analyze the microstructure and microchemical composition of the laser-clad layers, a scanning electron microscope (SEM) equipped with an energy dispersive X-ray microanalysis system was employed. X-ray diffraction techniques were applied to characterize the phases formed during the cladding process. The results show that the microstructure of the cladding alloy consists mainly of many dispersed particles (W 2C, (W,Ti)C 1- x, WC), a lamellar eutectic carbide M 12C, and an (f.c.c) matrix. Hardness tested at room and high temperature showed that the laser-clad zone has a moderate room temperature hardness and relatively higher elevated temperature hardness. The application of the laser-clad layer to a hot tool was very successful, and its operational life span was prolonged 1 to 4 times.

Correlation between microstructure and thermionic electron emission from Os-Ru thin films on dispenser cathodes

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

Swartzentruber, Phillip D.; John Balk, Thomas, E-mail: john.balk@uky.edu; Effgen, Michael P.

2014-07-01

Osmium-ruthenium films with different microstructures were deposited onto dispenser cathodes and subjected to 1000 h of close-spaced diode testing. Tailored microstructures were achieved by applying substrate biasing during deposition, and these were evaluated with scanning electron microscopy, x-ray diffraction, and energy dispersive x-ray spectroscopy before and after close-spaced diode testing. Knee temperatures determined from the close-spaced diode test data were used to evaluate cathode performance. Cathodes with a large (10-11) Os-Ru film texture possessed comparatively low knee temperatures. Furthermore, a low knee temperature correlated with a low effective work function as calculated from the close-spaced diode data. It is proposedmore » that the formation of strong (10-11) texture is responsible for the superior performance of the cathode with a multilayered Os-Ru coating.« less

High temperature oxidation behavior of austenitic stainless steel AISI 304 in steam of nanofluids contain nanoparticle ZrO2

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

Prajitno, Djoko Hadi, E-mail: djokohp@batan.go.id; Syarif, Dani Gustaman, E-mail: djokohp@batan.go.id

2014-03-24

The objective of this study is to evaluate high temperature oxidation behavior of austenitic stainless steel SS 304 in steam of nanofluids contain nanoparticle ZrO{sub 2}. The oxidation was performed at high temperatures ranging from 600 to 800°C. The oxidation time was 60 minutes. After oxidation the surface of the samples was analyzed by different methods including, optical microscope, scanning electron microscope (SEM) and X-ray diffraction (XRD). X-ray diffraction examination show that the oxide scale formed during oxidation of stainless steel AISI 304 alloys is dominated by iron oxide, Fe{sub 2}O{sub 3}. Minor element such as Cr{sub 2}O{sub 3} ismore » also appeared in the diffraction pattern. Characterization by optical microscope showed that cross section microstructure of stainless steel changed after oxidized with the oxide scale on the surface stainless steels. SEM and x-ray diffraction examination show that the oxide of ZrO{sub 2} appeared on the surface of stainless steel. Kinetic rate of oxidation of austenite stainless steel AISI 304 showed that increasing oxidation temperature and time will increase oxidation rate.« 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.

Irradiation effects and micro-structural changes in large grain uranium dioxide fuel investigated by micro-beam X-ray diffraction

NASA Astrophysics Data System (ADS)

Mieszczynski, C.; Kuri, G.; Degueldre, C.; Martin, M.; Bertsch, J.; Borca, C. N.; Grolimund, D.; Delafoy, Ch.; Simoni, E.

2014-01-01

Microstructural changes in a set of commercial grade UO2 fuel samples have been investigated using synchrotron based micro-focused X-ray fluorescence (μ-XRF) and X-ray diffraction (μ-XRD) techniques. The results are associated with conventional UO2 materials and relatively larger grain chromia-doped UO2 fuels, irradiated in a commercial light water reactor plant (average burn-up: 40 MW d kg-1). The lattice parameters of UO2 in fresh and irradiated specimens have been measured and compared with theoretical predictions. In the pristine state, the doped fuel has a somewhat smaller lattice parameter than the standard UO2 as a result of chromia doping. Increase in micro-strain and lattice parameter in irradiated materials is highlighted. All irradiated samples behave in a similar manner with UO2 lattice expansion occurring upon irradiation, where any Cr induced effect seems insignificant and accumulated lattice defects prevail. Elastic strain energy densities in the irradiated fuels are also evaluated based on the UO2 crystal lattice strain and non-uniform strain. The μ-XRD patterns further allow the evaluation of the crystalline domain size and sub-grain formation at different locations of the irradiated UO2 pellets.

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.

Diffraction and imaging study of imperfections of crystallized lysozyme with coherent X-rays

NASA Technical Reports Server (NTRS)

Hu, Z. W.; Chu, Y. S.; Lai, B.; Thomas, B. R.; Chernov, A. A.

2004-01-01

Phase-contrast X-ray diffraction imaging and high-angular-resolution diffraction combined with phase-contrast radiographic imaging were employed to characterize defects and perfection of a uniformly grown tetragonal lysozyme crystal in the symmetric Laue case. The full-width at half-maximum (FWHM) of a 4 4 0 rocking curve measured from the original crystal was approximately 16.7 arcsec and imperfections including line defects, inclusions and other microdefects were observed in the diffraction images of the crystal. The observed line defects carry distinct dislocation features running approximately along the <1 1 0> growth front and have been found to originate mostly in a central growth area and occasionally in outer growth regions. Inclusions of impurities or formations of foreign particles in the central growth region are resolved in the images with high sensitivity to defects. Slow dehydration led to the broadening of a fairly symmetric 4 4 0 rocking curve by a factor of approximately 2.6, which was primarily attributed to the dehydration-induced microscopic effects that are clearly shown in X-ray diffraction images. The details of the observed defects and the significant change in the revealed microstructures with drying provide insight into the nature of imperfections, nucleation and growth, and the properties of protein crystals.

Microstructure and Mechanical Properties of Laves Phase-strengthened Fe-Cr-Zr Alloys

DOE PAGES

Tan, Lizhen; Yang, Ying

2014-12-05

Laves phase-reinforced alloys have shown some preliminary promising performance at room temperatures. This paper aims at evaluating mechanical properties of Laves phase-strengthened alloys at elevated temperatures. Three Fe-Cr-Zr alloys were designed to favor the formation of eutectic microstructures containing Laves and body-centered cubic phases with the aid of thermodynamic calculations. Microstructural characterization was carried out on the alloys in as-processed and aged states using optical microscopy, scanning electron microscopy, energy-dispersive X-ray spectroscopy, and X-ray diffraction. The effect of thermal aging and alloy composition on microstructure has been discussed based on microstructural characterization results. Mechanical properties have been evaluated by meansmore » of Vickers microhardness measurements, tensile testing at temperatures up to 973.15 K (700.15 °C), and creep testing at 873.15 K (600.15 °C) and 260 MPa. Alloys close to the eutectic composition show significantly superior strength and creep resistance compared to P92. Finally, however, their low tensile ductility may limit their applications at relatively low temperatures.« less

Modulated structures and associated microstructures in the ferroelectric phase of Ba1-xSrxAl2O4 for 0.7 ≤ x ≤ 1.0

NASA Astrophysics Data System (ADS)

Tsukasaki, Hirofumi; Ishii, Yui; Tanaka, Eri; Kurushima, Kosuke; Mori, Shigeo

2016-01-01

In order to understand the ferroelectric and ferroelastic phases in Ba1-xSrxAl2O4 for 0.7 ≤ x ≤ 1.0, we have investigated the crystal structures and their associated microstructures of the ferroelectric and ferroelastic phases mainly by transmission electron microscopy (TEM) and scanning transmission electron microscopy-high-angle angular dark-field (STEM-HAADF) experiments, combined with powder X-ray diffraction experiments. Electron diffraction experiments showed that the ferroelectric and ferroelastic phases of Ba1-xSrxAl2O4 for 0.7 ≤ x ≤ 1.0 should be characterized as a modulated structure with the modulation vector of \\boldsymbol{{q}} = 0,1/2,0, whose space group should be monoclinic P21. High-resolution TEM experiments revealed that the microstructures in the monoclinic phase can be characterized as twin structures and nanometer-sized planar defects due to the monoclinic structure with the modulated structures, which are responsible for anomalous elastic behaviors and mechanoelectro-optical properties. In addition, subatomic-resolution STEM-HAADF images clearly indicated that the displacement of Al3+ ions involved in the AlO4 tetrahedra should play a crucial role in the formation of the modulated structures and twin structures.

Texture and microstructure evolution in single-phase Ti{sub x}Ta{sub 1-x}N alloys of rocksalt structure

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

Koutsokeras, L. E.; Department of Materials Science and Engineering, University of Ioannina, GR-45100 Ioannina; Abadias, G.

2011-08-15

The mechanisms controlling the structural and morphological features (texture and microstructure) of ternary transition metal nitride thin films of the Ti{sub x}Ta{sub 1-x}N system, grown by various physical vapor deposition techniques, are reported. Films deposited by pulsed laser deposition, dual cathode magnetron sputtering, and dual ion beam sputtering have been investigated by means of x-ray diffraction in various geometries and scanning electron microscopy. We studied the effects of composition, energetic, and kinetics in the evolution of the microstructure and texture of the films. We obtain films with single and mixed texture as well as films with columnar ''zone-T'' and globularmore » type morphology. The results have shown that the texture evolution of ternary transition metal nitrides as well as the microstructural features of such films can be well understood in the framework of the kinetic mechanisms proposed for their binary counterparts, thus giving these mechanisms a global application.« less

Microstructures in rapidly solidified Ni-Mo alloys

NASA Technical Reports Server (NTRS)

Jayaraman, N.; Tewari, S. N.; Hemker, K. J.; Glasgow, T. K.

1985-01-01

Ni-Mo alloys of compositions ranging from pure Ni to Ni-40 at % Mo were rapidly solidified by Chill Block Melt Spinning in vacuum and were examined by optical metallography, X-ray diffraction and transmission electron microscopy. Rapid solidification resulted in an extension of molybdenum solubility in nickel from 28 to 37.5 at %. A number of different phases and microstructures were seen at different depths (solidification conditions) from the quenched surface of the melt spun ribbons.

Broadening and shifting of Bragg reflections of nanoscale-microtwinned LT-Ni3Sn2

NASA Astrophysics Data System (ADS)

Leineweber, Andreas; Krumeich, Frank

2013-12-01

The effect of nanoscale microtwinning of long-range ordered domains in LT-Ni3Sn2 on its diffraction behaviour was studied by X-ray powder diffraction and electron microscopy. LT-Ni3Sn2 exhibits a Ni2In/NiAs-type structure with a superstructure breaking the symmetry relative to the hexagonal high-temperature (HT) to the orthorhombic low-temperature (LT) phase, implying three different twin-domain orientations. The microstructure was generated by annealing HT-Ni3Sn2 considerably below the order-disorder transition temperature, establishing the LT phase avoiding too much domain coarsening. High-resolution electron microscopy reveals domain sizes of 100-200 Å compatible with the Scherrer broadening of the superstructure reflections recorded by X-ray diffraction. Whereas the orthorhombic symmetry of the LT phase leads in powder-diffraction patterns from coarse-domain size material to splitting of the fundamental reflections, this splitting does not occur for the LT-Ni3Sn2 with nanoscale domains. Instead, a (pseudo)hexagonal indexing is possible giving hexagonal lattice parameters, which are, however, incompatible with the positions of the superstructure reflections. This can be attributed to interference between X-rays scattered by the differently oriented, truly orthorhombic domains leading to merging of the fundamental reflections. These show pronounced anisotropic microstrain-like broadening, where the integral breadths ? on the reciprocal d-spacing scale of a series of higher order reflection increase in a non-linear fashion with upward curvature with the reciprocal d-spacings ? of these reflections. Such a type of unusual microstrain broadening appears to be typical for microstructures which are inhomogeneous on the nanoscale, and in which the structural inhomogeneities lead to small phase shifts of the scattered radiation from different locations (e.g. domains).

Investigation of the Microstructure Evolution in a Fe-17Mn-1.5Al-0.3C Steel via In Situ Synchrotron X-ray Diffraction during a Tensile Test

PubMed Central

Song, Wenwen; Bleck, Wolfgang

2017-01-01

The quantitative characterization of the microstructure evolution in high-Mn steel during deformation is of great importance to understanding its strain-hardening behavior. In the current study, in situ high-energy synchrotron X-ray diffraction was employed to characterize the microstructure evolution in a Fe-17Mn-1.5Al-0.3C steel during a tensile test. The microstructure at different engineering strain levels—in terms of ε-martensite and α’-martensite volume fractions, the stacking fault probability, and the twin fault probability—was analyzed by the Rietveld refinement method. The Fe-17Mn-1.5Al-0.3C steel exhibits a high ultimate tensile strength with a superior uniform elongation and a high strain-hardening rate. The remaining high strain-hardening rate at the strain level about 0.025 to 0.35 results from ε-martensite dominant transformation-induced-plasticity (TRIP) effect. The increase in the strain-hardening rate at the strain level around 0.35 to 0.43 is attributed to the synergetic α’-martensite dominant TRIP and twinning-induced-plasticity (TWIP) effects. An evaluation of the stacking fault energy (SFE) of the Fe-17Mn-1.5Al-0.3C steel by the synchrotron measurements shows good agreement with the thermodynamic calculation of the SFE. PMID:28946692

Investigation of the Microstructure Evolution in a Fe-17Mn-1.5Al-0.3C Steel via In Situ Synchrotron X-ray Diffraction during a Tensile Test.

PubMed

Ma, Yan; Song, Wenwen; Bleck, Wolfgang

2017-09-25

The quantitative characterization of the microstructure evolution in high-Mn steel during deformation is of great importance to understanding its strain-hardening behavior. In the current study, in situ high-energy synchrotron X-ray diffraction was employed to characterize the microstructure evolution in a Fe-17Mn-1.5Al-0.3C steel during a tensile test. The microstructure at different engineering strain levels-in terms of ε-martensite and α'-martensite volume fractions, the stacking fault probability, and the twin fault probability-was analyzed by the Rietveld refinement method. The Fe-17Mn-1.5Al-0.3C steel exhibits a high ultimate tensile strength with a superior uniform elongation and a high strain-hardening rate. The remaining high strain-hardening rate at the strain level about 0.025 to 0.35 results from ε-martensite dominant transformation-induced-plasticity (TRIP) effect. The increase in the strain-hardening rate at the strain level around 0.35 to 0.43 is attributed to the synergetic α'-martensite dominant TRIP and twinning-induced-plasticity (TWIP) effects. An evaluation of the stacking fault energy (SFE) of the Fe-17Mn-1.5Al-0.3C steel by the synchrotron measurements shows good agreement with the thermodynamic calculation of the SFE.

Combining operando synchrotron X-ray tomographic microscopy and scanning X-ray diffraction to study lithium ion batteries

PubMed Central

Pietsch, Patrick; Hess, Michael; Ludwig, Wolfgang; Eller, Jens; Wood, Vanessa

2016-01-01

We present an operando study of a lithium ion battery combining scanning X-ray diffraction (SXRD) and synchrotron radiation X-ray tomographic microscopy (SRXTM) simultaneously for the first time. This combination of techniques facilitates the investigation of dynamic processes in lithium ion batteries containing amorphous and/or weakly attenuating active materials. While amorphous materials pose a challenge for diffraction techniques, weakly attenuating material systems pose a challenge for attenuation-contrast tomography. Furthermore, combining SXRD and SRXTM can be used to correlate processes occurring at the atomic level in the crystal lattices of the active materials with those at the scale of electrode microstructure. To demonstrate the benefits of this approach, we investigate a silicon powder electrode in lithium metal half-cell configuration. Combining SXRD and SRXTM, we are able to (i) quantify the dissolution of the metallic lithium electrode and the expansion of the silicon electrode, (ii) better understand the formation of the Li15Si4 phase, and (iii) non-invasively probe kinetic limitations within the silicon electrode. A simple model based on the 1D diffusion equation allows us to qualitatively understand the observed kinetics and demonstrates why high-capacity electrodes are more prone to inhomogeneous lithiation reactions. PMID:27324109

Combining operando synchrotron X-ray tomographic microscopy and scanning X-ray diffraction to study lithium ion batteries

NASA Astrophysics Data System (ADS)

Pietsch, Patrick; Hess, Michael; Ludwig, Wolfgang; Eller, Jens; Wood, Vanessa

2016-06-01

We present an operando study of a lithium ion battery combining scanning X-ray diffraction (SXRD) and synchrotron radiation X-ray tomographic microscopy (SRXTM) simultaneously for the first time. This combination of techniques facilitates the investigation of dynamic processes in lithium ion batteries containing amorphous and/or weakly attenuating active materials. While amorphous materials pose a challenge for diffraction techniques, weakly attenuating material systems pose a challenge for attenuation-contrast tomography. Furthermore, combining SXRD and SRXTM can be used to correlate processes occurring at the atomic level in the crystal lattices of the active materials with those at the scale of electrode microstructure. To demonstrate the benefits of this approach, we investigate a silicon powder electrode in lithium metal half-cell configuration. Combining SXRD and SRXTM, we are able to (i) quantify the dissolution of the metallic lithium electrode and the expansion of the silicon electrode, (ii) better understand the formation of the Li15Si4 phase, and (iii) non-invasively probe kinetic limitations within the silicon electrode. A simple model based on the 1D diffusion equation allows us to qualitatively understand the observed kinetics and demonstrates why high-capacity electrodes are more prone to inhomogeneous lithiation reactions.

Effects of limestone petrography and calcite microstructure on OPC clinker raw meals burnability

NASA Astrophysics Data System (ADS)

Galimberti, Matteo; Marinoni, Nicoletta; Della Porta, Giovanna; Marchi, Maurizio; Dapiaggi, Monica

2017-10-01

Limestone represents the main raw material for ordinary Portland cement clinker production. In this study eight natural limestones from different geological environments were chosen to prepare raw meals for clinker manufacturing, aiming to define a parameter controlling the burnability. First, limestones were characterized by X-Ray Fluorescence, X-Ray Powder Diffraction and Optical Microscopy to assess their suitability for clinker production and their petrographic features. The average domains size and the microstrain of calcite were also determined by X-Ray Powder Diffraction line profile analysis. Then, each limestone was admixed with clay minerals to achieve the adequate chemical composition for clinker production. Raw meals were thermally threated at seven different temperatures, from 1000 to 1450 °C, to evaluate their behaviour on heating by ex situ X-Ray Powder Diffraction and to observe the final clinker morphology by Scanning Electron Microscopy. Results indicate the calcite microstrain is a reliable parameter to predict the burnability of the raw meals, in terms of calcium silicates growth and lime consumption. In particular, mixtures prepared starting from high-strained calcite exhibit a better burnability. Later, when the melt appears this correlation vanishes; however differences in the early burnability still reflect on the final clinker composition and texture.

Low Temperature Synthesis, Chemical and Electrochemical Characterization of LiNi(x)Co(1-x)O2 (0 less than x less than 1)

NASA Technical Reports Server (NTRS)

Nanjundaswamy, K. S.; Standlee, D.; Kelly, C. O.; Whiteley, R. V., Jr.

1997-01-01

A new method of synthesis for the solid solution cathode materials LiNi(x)Co(1-x)O2 (0 less than x less than 1) involving enhanced reactions at temperatures less than or equal to 700 deg. C, between metal oxy-hydroxide precursors MOOH (M = Ni, Co) and Li-salts (Li2CO3, LiOH, and LiNO3) has been investigated. The effects of synthesis conditions and sources of Li, on phase purity, microstructure, and theoretical electrochemical capacity (total M(3+) content) are characterized by powder X-ray diffraction analysis, scanning electron microscopy, chemical analysis and room temperature magnetic susceptibility. An attempt has been made to correlate the electrochemical properties with the synthesis conditions and microstructure.

Anisotropic pyrochemical microetching of poly(tetrafluoroethylene) initiated by synchrotron radiation-induced scission of molecule bonds

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

Yamaguchi, Akinobu, E-mail: yamaguti@lasti.u-hyogo.ac.jp, E-mail: utsumi@lasti.u-hyogo.ac.jp; Kido, Hideki; Utsumi, Yuichi, E-mail: yamaguti@lasti.u-hyogo.ac.jp, E-mail: utsumi@lasti.u-hyogo.ac.jp

2016-02-01

We developed a process for micromachining polytetrafluoroethylene (PTFE): anisotropic pyrochemical microetching induced by synchrotron X-ray irradiation. X-ray irradiation was performed at room temperature. Upon heating, the irradiated PTFE substrates exhibited high-precision features. Both the X-ray diffraction peak and Raman signal from the irradiated areas of the substrate decreased with increasing irradiation dose. The etching mechanism is speculated as follows: X-ray irradiation caused chain scission, which decreased the number-average degree of polymerization. The melting temperature of irradiated PTFE decreased as the polymer chain length decreased, enabling the treated regions to melt at a lower temperature. The anisotropic pyrochemical etching process enabledmore » the fabrication of PTFE microstructures with higher precision than simultaneously heating and irradiating the sample.« less

Preliminary in situ and real-time study of directional solidification of metallic alloys by x-ray imaging techniques

NASA Astrophysics Data System (ADS)

Nguyen Thi, H.; Jamgotchian, H.; Gastaldi, J.; Härtwig, J.; Schenk, T.; Klein, H.; Billia, B.; Baruchel, J.; Dabo, Y.

2003-05-01

During directional solidification of a binary alloy, the solid-liquid interface exhibits a variety of patterns that are due to the Mullins-Sekerka instability and governed by the growth conditions. It is well known that properties of the grown material are largely controlled by the microstructures left in the solid during processing. Thus, a precise mastering of the solidification is essential to tailor products in a reproducible fashion to a specified quality. One major difficulty for this study is the real-time and in situ observation of the interface, especially for metallic alloys. A possibility is to use an intense and coherent third generation x-ray beam. By combining different x-ray imaging techniques (absorption/phase contrast radiography and diffraction topography), we have studied the directional melting and solidification of aluminium-based alloys. The preliminary results show the great potential of these techniques for the study of the coupling between stress effects and microstructure formation in solidification processing.

Microscopic stress characterisation of functional iron-based alloys by white X-ray microbeam diffraction

NASA Astrophysics Data System (ADS)

Kwon, E. P.; Sato, S.; Fujieda, S.; Shinoda, K.; Kajiwara, K.; Sato, M.; Suzuki, S.

2018-01-01

Microscopic residual stress evolution in an austenite (γ) grain during a shape-memory process in an Fe-Mn-Si-Cr alloy was investigated using the white X-ray microbeam diffraction technique. The stresses were measured on a coarse grain, which had an orientation near <144>, parallel to the tensile loading direction with a high Schmid factor for a martensitic transformation. The magnitude of the residual stresses in a grain of the sample, which was subjected to a 23 % tensile strain and subsequent shape-recovery heating, was found to be very small and comparable to that prior to tensile deformation. Measurements of the recovery strain and microstructural analyses using electron backscatter diffraction suggested that the low residual stresses could be attributed to the significant shape recovery caused by a highly reversible martensitic transformation in the grain with a particular orientation.

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

Willey, Trevor M.; Lauderbach, Lisa; Gagliardi, Franco

HMX-based explosives LX-10 and PBX-9501 were heated through the β-δ phase transition. Ultra-small angle x-ray scattering (USAXS) and molecular diffraction were simultaneously recorded as the HMX was heated. Mesoscale voids and structure dramatically change promptly with the β-δ phase transition, rather than with other thermal effects. Also, x-ray induced damage, observed in the USAXS, occurs more readily at elevated temperatures; as such, the dose was reduced to mitigate this effect. Optical microscopy performed during a similar heating cycle gives an indication of changes on longer length scales, while x-ray microtomography, performed before and after heating, shows the character of extensivemore » microstructural damage resulting from the temperature cycle and solid-state phase transition.« less

Microstructure and Corrosion Resistance of Laser Additively Manufactured 316L Stainless Steel

NASA Astrophysics Data System (ADS)

Trelewicz, Jason R.; Halada, Gary P.; Donaldson, Olivia K.; Manogharan, Guha

2016-03-01

Additive manufacturing (AM) of metal alloys to produce complex part designs via powder bed fusion methods such as laser melting promises to be a transformative technology for advanced materials processing. However, effective implementation of AM processes requires a clear understanding of the processing-structure-properties-performance relationships in fabricated components. In this study, we report on the formation of micro and nanoscale structures in 316L stainless steel samples printed by laser AM and their implications for general corrosion resistance. A variety of techniques including x-ray diffraction, optical, scanning and transmission electron microscopy, x-ray fluorescence, and energy dispersive x-ray spectroscopy were employed to characterize the microstructure and chemistry of the laser additively manufactured 316L stainless steel, which are compared with wrought 316L coupons via electrochemical polarization. Apparent segregation of Mo has been found to contribute to a loss of passivity and an increased anodic current density. While porosity will also likely impact the environmental performance (e.g., facilitating crevice corrosion) of AM alloys, this work demonstrates the critical influence of microstructure and heterogeneous solute distributions on the corrosion resistance of laser additively manufactured 316L stainless steel.

Characterization of high energy Xe ion irradiation effects in single crystal molybdenum with depth-resolved synchrotron microbeam diffraction

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

Yun, Di; Miao, Yinbin; Xu, Ruqing

2016-04-01

Microbeam X-ray diffraction experiments were conducted at beam line 34-ID of the Advanced Photon Source (APS) on fission fragment energy Xe heavy ion irradiated single crystal Molybdenum (Mo). Lattice strain measurements were obtained with a depth resolution of 0.7 mu m, which is critical in resolving the peculiar heterogeneity of irradiation damage associated with heavy ion irradiation. Q-space diffraction peak shift measurements were correlated with lattice strain induced by the ion irradiations. Transmission electron microscopy (TEM) characterizations were performed on the as-irradiated materials as well. Nanometer sized Xe bubble microstructures were observed via TEM. Molecular Dynamics (MD) simulations were performedmore » to help interpret the lattice strain measurement results from the experiment. This study showed that the irradiation effects by fission fragment energy Xe ion irradiations can be collaboratively understood with the depth resolved X-ray diffraction and TEM measurements under the assistance of MD simulations. (c) 2015 Elsevier B.V. All rights reserved.« less

Effect of iron doping on structural and microstructural properties of nanocrystalline ZnSnO3 thin films prepared by spray pyrolysis techniques

NASA Astrophysics Data System (ADS)

Pathan, Idris G.; Suryawanshi, Dinesh N.; Bari, Anil R.; Patil, Lalchand A.

2018-05-01

This work presents the effect of iron doping having different volume ratios (1 ml, 2.5 ml and 5 ml) on the structural, microstructural and electrical properties of zinc stannate thin films, prepared by spray pyrolysis method. These properties were characterized with X-ray diffraction (XRD) and Transmission Electron Microscope (TEM). In our study, XRD pattern indicates that ZnSnO3 has a perovskite phase with face exposed hexahedron structure. The electron diffraction fringes observed are in consistent with the peak observed in XRD patterns. Moreover the sensor reported in our study is cost-effective, user friendly and easy to fabricate.

Effects of vanadium ion implantation on microstructure, mechanical and tribological properties of TiN coatings

NASA Astrophysics Data System (ADS)

Deng, Bin; Tao, Ye; Guo, Deliang

2012-09-01

TiN coatings were deposited on the substrates of cemented carbide (WC-TiC-Co) by Magnetic Filter Arc Ion Plating (MFAIP) and then implanted with vanadium through Metal Vacuum Vapor Arc (MEVVA) ion source with the doses of 1 × 1017 and 5 × 1017 ions/cm2 at 40 kV. The microstructures and chemical compositions of the V-implanted TiN coatings were investigated using Glancing Incidence X-ray Diffraction (GIXRD) and X-ray Photoelectron Spectroscopy (XPS), together with the mechanical and tribological properties of coatings were characterized using nano-indentation and ball-on-disk tribometer. It was found that the diffraction peaks of the V-implanted TiN coatings at the doses of 5 × 1017 ions/cm2 shifted to higher angles and became broader. The hardness and elastic modulus of TiN coatings increased after V ion implantation. The wear mechanism for both un-implanted and V-implanted TiN coatings against GCr15 steel ball was adhesive wear, and the V-implanted TiN coatings had a lower friction coefficient as well as a better wear resistance

Rapid microwave assisted synthesis of YIn1-xMnxO3 blue pigments: Synthesis, microstructure and optical properties

NASA Astrophysics Data System (ADS)

Zhou, Yuncheng; Jiang, Peng; Kuang, Jianlei; Yang, Xueshan; Cao, Wenbin

2018-07-01

The YIn1-xMnxO3 (0.1 ≤x ≤ 0.5) blue pigment samples are successfully prepared through a sol-gel process followed by microwave assisted sintering process. All the samples are shown single phases in the X-ray diffraction results. In the morphology study from scanning electronic microscope, the samples are composed of loosely connected small particles. The oxidation state of Mn is confirmed to be 3 + from the results of X-ray photonelectronic scan. The optical properties are characterized by UV-Visible spectrum and UV-visible-NIR spectrum. The samples exhibit intense blue color and they show small absorption in infrared region.

In search of the elusive IrB{sub 2}: Can mechanochemistry help?

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

Xie, Zhilin; Blair, Richard G.; Department of Physics, University of Central Florida, Orlando, FL 32816

The previously unknown hexagonal ReB{sub 2}-type IrB{sub 2} diboride and orthorhombic IrB monoboride phases were produced by mechanochemical syntheses. High energy ball milling of elemental Ir and B powder for 30 h, followed by annealing of the powder at 1050 °C for 48 h, resulted in the formation of the desired phases. Both traditional laboratory and high resolution synchrotron X-ray diffraction (XRD) analyses were used for phase identification of the synthesized powder. In addition to XRD, scanning electron microscopy and transmission electron microscopy were employed to further characterize the microstructure of the phases produced. - Graphical abstract: ReB{sub 2}-type IrB{submore » 2} and a new IrB have been successfully synthesized for the first time using mechanochemical method. Crystal structures of IrB{sub 2} and IrB were studied by synchrotron X-ray diffraction. Microstructures of the new phases were characterized by SEM and TEM. - Highlights: • ReB{sub 2}-type IrB{sub 2} and a new IrB have been synthesized by mechanochemical method. • Crystal structures of IrB{sub 2} and IrB were studied by synchrotron XRD. • Microstructures of the new phases were characterized by SEM and TEM.« less

Effect of niobium content on the microstructure and thermal properties of fluorapatite glass-ceramics.

PubMed

Denry, I L; Holloway, J A; Nakkula, R J; Walters, J D

2005-10-01

Niobium oxide has been shown to improve biocompatibility and promote bioactivity. The purpose of this study was to evaluate the effect of niobium oxide additions on the microstructure and thermal properties of fluorapatite glass-ceramics for biomedical applications. Four glass-ceramic compositions with increasing amounts of niobium oxide from 0 to 5 wt % were prepared. The glass compositions were melted at 1,525 degrees C for 3 h, quenched, ground, melted again at 1,525 degrees C for 3 h and furnace cooled. The coefficient of thermal expansion was measured by dilatometry. The crystallization behavior was evaluated by differential thermal analysis. The nature of the crystalline phases was investigated by X-ray diffraction. The microstructure was studied by SEM. In addition, the cytotoxicity of the ceramics was evaluated according to the ASTM standard F895--84. The results from X-ray diffraction analyses showed that fluorapatite was the major crystalline phase in all glass-ceramics. Differential thermal analyses revealed that fluorapatite crystallization occurred between 800 and 934 degrees C depending on the composition. The coefficient of thermal expansion varied from 7.6 to 9.4 x 10(-6)/ degrees C. The microstructure after heat treatment at 975 degrees C for 30 min consisted of submicroscopic fluorapatite crystals (200--300 nm) for all niobium-containing glass-ceramics, whereas the niobium-free glass-ceramic contained needle-shaped fluorapatite crystals, 2 microm in length. None of the glass-ceramics tested exhibited any cytotoxic activity as tested by ASTM standard F895--84. (c) 2005 Wiley Periodicals, Inc. J Biomed Mater Res Part B: Appl Biomater, 2005.

A comparative study of a (0-3) connectivity type composite and core-shell structure of CoFe2O4 - BaTiO3 based on microstructure and magnetic property

NASA Astrophysics Data System (ADS)

Das, Avisek; Gorige, Venkataiah

2018-04-01

In this work CoFe2O4 (CFO)-BaTiO3 (BTO) composite and core-shell CFO-BTO have been prepared to investigate the effect of microstructure on the magnetic properties. Detailed microstructure analysis has been carried out using X-ray diffraction, field emission scanning electron microscope and transmission electron microscope. Although uniform distribution of CFO is found in BTO matrix for the composite sample, magnetization and coercivity values are more enhanced in core-shell CFO-BTO.

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

Jana, S.; Devaraj, A.; Kovarik, L.

Transformation kinetics of metastable body-centered cubic γ-UMo phase in U-10 wt.percent Mo alloy during annealing at sub-eutectoid temperatures of 500C and 400C has been determined as a function of time using detailed microstructural characterization by scanning electron microscopy, X-ray diffraction analysis, scanning transmission electron microscopy, and atom probe tomography. Based on the results, we found that the phase transformation is initiated by cellular transformation at both the temperatures, which results in formation of a lamellar microstructure along prior γ-UMo grain boundaries.

Multilayer diffraction grating

DOEpatents

Barbee, T.W. Jr.

1990-04-10

This invention is for a reflection diffraction grating that functions at X-ray to VUV wavelengths and at normal angles of incidence. The novel grating is comprised of a laminar grating of period D with flat-topped grating bars. A multiplicity of layered synthetic microstructures, of period d and comprised of alternating flat layers of two different materials, are disposed on the tops of the grating bars of the laminar grating. In another embodiment of the grating, a second multiplicity of layered synthetic microstructures are also disposed on the flat faces, of the base of the grating, between the bars. D is in the approximate range from 3,000 to 50,000 Angstroms, but d is in the approximate range from 10 to 400 Angstroms. The laminar grating and the layered microstructures cooperatively interact to provide many novel and beneficial instrumentational advantages. 2 figs.

Multilayer diffraction grating

DOEpatents

Barbee, Jr., Troy W.

1990-01-01

This invention is for a reflection diffraction grating that functions at X-ray to VUV wavelengths and at normal angles of incidence. The novel grating is comprised of a laminar grating of period D with flat-topped grating bars. A multiplicity of layered synthetic microstructures, of period d and comprised of alternating flat layers of two different materials, are disposed on the tops of the grating bars of the laminar grating. In another embodiment of the grating, a second multiplicity of layered synthetic microstructures are also disposed on the flat faces, of the base of the grating, between the bars. D is in the approximate range from 3,000 to 50,000 Angstroms, but d is in the approximate range from 10 to 400 Angstroms. The laminar grating and the layered microstructures cooperatively interact to provide many novel and beneficial instrumentational advantages.

Evolution of microstructure and residual stress during annealing of austenitic and ferritic steels

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

Wawszczak, R.; Baczmański, A., E-mail: Andrzej.Baczmanski@fis.agh.edu.pl; Marciszko, M.

2016-02-15

In this work the recovery and recrystallization processes occurring in ferritic and austenitic steels were studied. To determine the evolution of residual stresses during material annealing the nonlinear sin{sup 2}ψ diffraction method was used and an important relaxation of the macrostresses as well as the microstresses was found in the cold rolled samples subjected to heat treatment. Such relaxation occurs at the beginning of recovery, when any changes of microstructure cannot be detected using other experimental techniques. Stress evolution in the annealed steel samples was correlated with the progress of recovery process, which significantly depends on the value of stackingmore » fault energy. - Highlights: • X-ray diffraction was used to determine the first order and second order stresses. • Diffraction data were analyzed using scale transition elastoplastic models model. • Stress relaxation in annealed ferritic and austenitic steels was correlated with evolution of microstructure. • Influence of stacking fault energy on thermally induced processes was discussed.« less

Mechanism of the α -ɛ phase transformation in iron

NASA Astrophysics Data System (ADS)

Dewaele, A.; Denoual, C.; Anzellini, S.; Occelli, F.; Mezouar, M.; Cordier, P.; Merkel, S.; Véron, M.; Rausch, E.

2015-05-01

The α -Fe↔ɛ -Fe pressure-induced transformation under pure hydrostatic static compression has been characterized with in situ x-ray diffraction using α -Fe single crystals as starting samples. The forward transition starts at 14.9 GPa, and the reverse at 12 GPa, with a width of α -ɛ coexistence domain of the order of 2 GPa. The elastic stress in the sample increases in this domain, and partially relaxes after completion of the transformation. Orientation relations between parent α -Fe and child ɛ -Fe have been determined, which definitely validates the Burgers path for the direct transition. On the reverse transition, an unexpected variant selection is observed. X-ray diffraction data, complemented with ex situ microstructural observations, suggest that this selection is caused by defects and stresses accumulated during the direct transition.

Effect of Co2+ and Y3+ ions insertion on the microstructure development and magnetic properties of Ni0.5Zn0.5Fe2O4 powders synthesized using Co-precipitation method

NASA Astrophysics Data System (ADS)

Rashad, M. M.; Rayan, D. A.; Turky, A. O.; Hessien, M. M.

2015-01-01

Nanocrystalline Ni0.5Zn0.5-xCoxFe2-zYzO4 powders (x=0-0.3 and z from 0 to 0.3) have been synthesized via a facile co-precipitation technique. X-ray diffraction (XRD), scanning electron microscopy (SEM) and vibrating sample magnetometer (VSM) are utilized in order to study the effect of variation of cobalt and yttrium substitutions and its impact on crystalline size, lattice parameter, X-ray density, microstructure and magnetic properties of the formed powders. X-ray diffraction data indicated that, after doping, all samples consisted of the main spinel phase for the formed precursors precipitated at pH 10 annealed at 1000 oC for 2 h. The lattice parameter and the unit cell were decreased linearly with increasing Co content whereas they were increased with increasing the Y incorporation. Additionally, the porosity was increased with increasing Co concentration while it was decreased with increasing the Y insertion. The mean ionic radii and hopping and bond lengths was decreased with the value of Co2+ and they were increased with the value of Y3+ ion as well as both of Y3+ and Co2+ ions. The microstructures of the produced powders were found to be cubic like structure. The addition of Y3+ ion suppressed the grain size whereas addition of Co2+ ion enhanced the grain growth availably. An examination of the magnetic properties revealed an increase in saturation magnetization with increasing Co and Y concentrations incorporation up to x=0.3. Meanwhile, the formed powders exhibited superparamagnetic characteristics. A high saturation magnetization (77.0 emu/g) was achieved for Ni0.5Zn0.2Co0.3Fe2O4 sample annealed at 1000 oC for 2 h.

Metallurgical characterization of experimental Ag-based soldering alloys.

PubMed

Ntasi, Argyro; Al Jabbari, Youssef S; Silikas, Nick; Al Taweel, Sara M; Zinelis, Spiros

2014-10-01

To characterize microstructure, hardness and thermal properties of experimental Ag-based soldering alloys for dental applications. Ag12Ga (AgGa) and Ag10Ga5Sn (AgGaSn) were fabricated by induction melting. Six samples were prepared for each alloy and microstructure, hardness and their melting range were determined by, scanning electron microscopy, energy dispersive X-ray (EDX) microanalysis, X-ray diffraction (XRD), Vickers hardness testing and differential scanning calorimetry (DSC). Both alloys demonstrated a gross dendritic microstructure while according to XRD results both materials consisted predominately of a Ag-rich face centered cubic phase The hardness of AgGa (61 ± 2) was statistically lower than that of AgGaSn (84 ± 2) while the alloys tested showed similar melting range of 627-762 °C for AgGa and 631-756 °C for AgGaSn. The experimental alloys tested demonstrated similar microstructures and melting ranges. Ga and Sn might be used as alternative to Cu and Zn to modify the selected properties of Ag based soldering alloys.

Metallurgical characterization of experimental Ag-based soldering alloys

PubMed Central

Ntasi, Argyro; Al Jabbari, Youssef S.; Silikas, Nick; Al Taweel, Sara M.; Zinelis, Spiros

2014-01-01

Aim To characterize microstructure, hardness and thermal properties of experimental Ag-based soldering alloys for dental applications. Materials and methods Ag12Ga (AgGa) and Ag10Ga5Sn (AgGaSn) were fabricated by induction melting. Six samples were prepared for each alloy and microstructure, hardness and their melting range were determined by, scanning electron microscopy, energy dispersive X-ray (EDX) microanalysis, X-ray diffraction (XRD), Vickers hardness testing and differential scanning calorimetry (DSC). Results Both alloys demonstrated a gross dendritic microstructure while according to XRD results both materials consisted predominately of a Ag-rich face centered cubic phase The hardness of AgGa (61 ± 2) was statistically lower than that of AgGaSn (84 ± 2) while the alloys tested showed similar melting range of 627–762 °C for AgGa and 631–756 °C for AgGaSn. Conclusion The experimental alloys tested demonstrated similar microstructures and melting ranges. Ga and Sn might be used as alternative to Cu and Zn to modify the selected properties of Ag based soldering alloys. PMID:25382945

The power of in situ pulsed laser deposition synchrotron characterization for the detection of domain formation during growth of Ba0.5Sr0.5TiO3 on MgO.

PubMed

Bauer, Sondes; Lazarev, Sergey; Molinari, Alan; Breitenstein, Andreas; Leufke, Philipp; Kruk, Robert; Hahn, Horst; Baumbach, Tilo

2014-03-01

A highly sophisticated pulsed laser deposition (PLD) chamber has recently been installed at the NANO beamline at the synchrotron facility ANKA (Karlsruhe, Germany), which allows for comprehensive studies on the PLD growth process of dielectric, ferroelectric and ferromagnetic thin films in epitaxial oxide heterostructures or even multilayer systems by combining in situ reflective high-energy diffraction with the in situ synchrotron high-resolution X-ray diffraction and surface diffraction methods. The modularity of the in situ PLD chamber offers the opportunity to explore the microstructure of the grown thin films as a function of the substrate temperature, gas pressure, laser fluence and target-substrate separation distance. Ba0.5Sr0.5TiO3 grown on MgO represents the first system that is grown in this in situ PLD chamber and studied by in situ X-ray reflectivity, in situ two-dimensional reciprocal space mapping of symmetric X-ray diffraction and acquisition of time-resolved diffraction profiles during the ablation process. In situ PLD synchrotron investigation has revealed the occurrence of structural distortion as well as domain formation and misfit dislocation which all depend strongly on the film thickness. The microstructure transformation has been accurately detected with a time resolution of 1 s. The acquisition of two-dimensional reciprocal space maps during the PLD growth has the advantage of simultaneously monitoring the changes of the crystalline structure as well as the formation of defects. The stability of the morphology during the PLD growth is demonstrated to be remarkably affected by the film thickness. A critical thickness for the domain formation in Ba0.5Sr0.5TiO3 grown on MgO could be determined from the acquisition of time-resolved diffraction profiles during the PLD growth. A splitting of the diffraction peak into two distinguishable peaks has revealed a morphology change due to modification of the internal strain during growth.

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

Effect of gas flow ratio on the microstructure and mechanical properties of boron phosphide films prepared by reactive magnetron sputtering

NASA Astrophysics Data System (ADS)

Jia, Z. C.; Zhu, J. Q.; Jiang, C. Z.; Shen, W. X.; Han, J. C.; Chen, R. R.

2011-10-01

Boron phosphide films were grown on silicon substrate by radio frequency reactive magnetron sputtering using boron target and hydrogen phosphine at different gas flow ratios (PH 3/Ar) at lower temperature. The chemical composition, microstructure and mechanical properties were characterized by X-ray photoelectron spectroscopy, X-ray diffraction, Raman spectrum, FTIR spectrum, surface profilometer and nano-indenter. The results indicate that the atomic ratio (P/B) rises from 1.06 up to 1.52 with the gas flow ratio increasing from 3/50 to 15/50. Simultaneously, the hardness and Young's modulus decrease from 25.4 GPa to 22.5 GPa, and 250.4 GPa to 238.4 GPa, respectively. Microstructure transforms from microcrystalline state to amorphous state along with the gas flow ratio increasing. Furthermore higher gas flow ratio leads to lower stress. The BP film prepared at the gas flow ratio of 3/50 can be contributed with the best properties.

The influence of surface microstructure and chemical composition on corrosion behaviour in fuel-grade bio-ethanol of low-alloy steel modified by plasma nitro-carburizing and post-oxidizing

NASA Astrophysics Data System (ADS)

Boniatti, Rosiana; Bandeira, Aline L.; Crespi, Ângela E.; Aguzzoli, Cesar; Baumvol, Israel J. R.; Figueroa, Carlos A.

2013-09-01

The interaction of bio-ethanol on steel surfaces modified by plasma-assisted diffusion technologies is studied for the first time. The influence of surface microstructure and chemical composition on corrosion behaviour of AISI 4140 low-alloy steel in fuel-grade bio-ethanol was investigated. The steel surfaces were modified by plasma nitro-carburizing followed plasma oxidizing. X-ray diffraction, scanning electron microscopy, optical microscopy, X-ray dispersive spectroscopy, and glow-discharge optical emission spectroscopy were used to characterize the modified surface before and after immersion tests in bio-ethanol up to 77 days. The main corrosion mechanism is pit formation. The pit density and pit size were measured in order to quantify the corrosion resistance which was found to depend more strongly on microstructure and morphology of the oxide layer than on its thickness. The best corrosion protection was observed for samples post-oxidized at 480 °C and 90 min.

Microstructural evolution and grain growth kinetics of GZ31 magnesium alloy

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

Roostaei, M., E-mail: miladroustaei68@ut.ac.ir

2016-08-15

Grain growth behavior of Mg–3Gd–1Zn (GZ31) magnesium alloy was studied in a wide range of annealing time and temperature to clarify the kinetics of grain growth, microstructural evolution and related metallurgical phenomena. This material exhibited typical normal grain growth mode under annealing conditions with annealing temperature of lower than 300 °C and soaking time of lower than 240 min. However, the abnormality in grain growth was also evident at annealing temperature of 400 °C and 500 °C. The dependence of abnormal grain growth (AGG) at mentioned annealing temperatures upon microstructural features such as dispersed precipitates, which were rich in Znmore » and Gd, was investigated by optical micrographs, X-ray diffraction patterns, scanning electron microscopy images, and energy dispersive X-ray analysis spectra. The bimodality in grain-size distribution histograms also signified the occurrence of AGG. Based on the experimental data on grain growth obtained by annealing treatments, the grain growth exponent and the activation energy were also figured out.« less

Effect of Ar{sup +} ion irradiation on the microstructure of pyrolytic carbon

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

Feng, Shanglei; Zhang, Dongsheng; Yang, Xinmei

2015-03-21

Pyrolytic carbon (PyC) coatings prepared by chemical vapor deposition were irradiated by 300 keV Ar{sup +} ions. Then, atomic force microscopy, synchrotron-based grazing incidence X-ray diffraction, Raman spectroscopy, X-ray photoemission spectroscopy, and transmission electron microscopy were employed to study how Ar{sup +} irradiation affects the microstructure of PyC, including the microstructural damage mechanisms and physics driving these phenomena. The 300 keV Ar{sup +} ion irradiation deteriorated the structure along the c-axis, which increased the interlayer spacing between graphene layers. With increasing irradiation dose, the density of defect states on the surface of PyC coating increases, and the basal planes gradually loses theirmore » initial ordering resulting in breaks in the lattice and turbulence at the peak damage dose reaches 1.58 displacement per atom (dpa). Surprisingly, the PyC becomes more textured as it becomes richer in structural defects with increasing irradiation dose.« less

Metallurgical characterization of a new nickel-titanium wire for rotary endodontic instruments.

PubMed

Alapati, Satish B; Brantley, William A; Iijima, Masahiro; Clark, William A T; Kovarik, Libor; Buie, Caesar; Liu, Jie; Ben Johnson, William

2009-11-01

A novel thermomechanical processing procedure has been developed that yields a superelastic (SE) nickel-titanium (NiTi) wire (M-Wire) that laboratory testing shows has improved mechanical properties compared with conventional SE austenitic NiTi wires used for manufacture of rotary instruments. The objective of this study was to determine the origin of the improved mechanical properties. Specimens from 2 batches of M-Wire prepared under different processing conditions and from 1 batch of standard-processed SE wire for rotary instruments were examined by scanning transmission electron microscopy, temperature-modulated differential scanning calorimetry, micro-x-ray diffraction, and scanning electron microscopy with x-ray energy-dispersive spectrometric analyses. The processing for M-Wire yields a microstructure containing martensite, that the proportions of NiTi phases depend on processing conditions, and that the microstructure exhibits pronounced evidence of alloy strengthening. The presence of Ti(2)Ni precipitates in both microstructures indicates that M-Wire and the conventional SE wire for rotary instruments are titanium-rich.

Magnetic and microstructural characterisation of FeNi: Insight into the formation and impact history of the IAB parent body

NASA Astrophysics Data System (ADS)

Nichols, C. I. O.; Krakow, R.; Herrero-Albillos, J.; Kronast, F.; Northwood-Smith, G.; Harrison, R. J.

2017-12-01

The IABs represent one of only two groups of iron meteorites that did not form by fractional crystallization of liquid Fe-Ni in the core of a differentiated planetesimal. Instead, they are believed to originate from a partially differentiated body that was severely disrupted by one or more impacts during its early history. Paleomagnetic signals from two IABs, Toluca and Odessa, were investigated using X-ray magnetic circular dichroism (XMCD) and X-ray photoemission electron microscopy (X-PEEM) to image the magnetisation of the cloudy zone. The IABs do not appear to have experienced a magnetic field, consistent with the lack of a metallic core on the parent body. We also present a detailed microstructural and magnetic study of the observed FeNi microstructures, characterising their properties using XMCD and X-PEEM. The crystallographic architecture of the microstructures was analysed using electron backscatter diffraction (EBSD). Odessa and Toluca both exhibit a complex series of microstructures, requiring an unusual evolution during slow cooling. A conventional Widmanstätten sequence of kamacite, tetrataenite rim and cloudy zone developed via slow cooling to temperatures below 400 ºC. Subsequent modification of the microstructures resulted in the formation of pearlitic plessite and spheroidized plessite. Compositional and crystallographic analysis suggests that pearlitic and spheroidized plessite formed by impact modification of the cloudy zone and martensite, respectively. This study highlights the importance of characterising microstructures in order to corroborate paleomagnetic observations, as well as improving our understanding of the processes effecting planetary formation and evolution.

Transition metal-substituted cobalt ferrite nanoparticles for biomedical applications.

PubMed

Sanpo, Noppakun; Berndt, Christopher C; Wen, Cuie; Wang, James

2013-03-01

Transition metals of copper, zinc, chromium and nickel were substituted into cobalt ferrite nanoparticles via a sol-gel route using citric acid as a chelating agent. The microstructure and elemental composition were characterized using scanning electron microscopy combined with energy-dispersive X-ray spectroscopy. Phase analysis of transition metal-substituted cobalt ferrite nanoparticles was performed via X-ray diffraction. Surface wettability was measured using the water contact angle technique. The surface roughness of all nanoparticles was measured using profilometry. Moreover, thermogravimetric analysis and differential scanning calorimetry were performed to determine the temperature at which the decomposition and oxidation of the chelating agents took place. Results indicated that the substitution of transition metals influences strongly the microstructure, crystal structure and antibacterial property of the cobalt ferrite nanoparticles. Copyright © 2012 Acta Materialia Inc. Published by Elsevier Ltd. All rights reserved.

Relationship of microstructure properties to oxygen impurities in nanocrystalline silicon photovoltaic materials

NASA Astrophysics Data System (ADS)

Xu, H.; Wen, C.; Liu, H.; Li, Z. P.; Shen, W. Z.

2013-03-01

We have fully investigated the correlation of microstructure properties and oxygen impurities in hydrogenated nanocrystalline silicon photovoltaic films. The achievement has been realized through a series of different hydrogen dilution ratio treatment by plasma enhanced chemical vapor deposition system. Raman scattering, x-ray diffraction, and ultraviolet-visible transmission techniques have been employed to characterize the physical structural characterization and to elucidate the structure evolution. The bonding configuration of the oxygen impurities was investigated by x-ray photoelectron spectroscopy and the Si-O stretching mode of infrared-transmission, indicating that the films were well oxidized in SiO2 form. Based on the consistence between the proposed structure factor and the oxygen content, we have demonstrated that there are two dominant disordered structure regions closely related to the post-oxidation contamination: plate-like configuration and clustered microvoids.

High spatial resolution grain orientation and strain mapping in thin films using polychromatic submicron x-ray diffraction

NASA Astrophysics Data System (ADS)

Tamura, N.; MacDowell, A. A.; Celestre, R. S.; Padmore, H. A.; Valek, B.; Bravman, J. C.; Spolenak, R.; Brown, W. L.; Marieb, T.; Fujimoto, H.; Batterman, B. W.; Patel, J. R.

2002-05-01

The availability of high brilliance synchrotron sources, coupled with recent progress in achromatic focusing optics and large area two-dimensional detector technology, has allowed us to develop an x-ray synchrotron technique that is capable of mapping orientation and strain/stress in polycrystalline thin films with submicron spatial resolution. To demonstrate the capabilities of this instrument, we have employed it to study the microstructure of aluminum thin film structures at the granular and subgranular levels. Due to the relatively low absorption of x-rays in materials, this technique can be used to study passivated samples, an important advantage over most electron probes given the very different mechanical behavior of buried and unpassivated materials.

Improved microstructure of cement-based composites through the addition of rock wool particles

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

Lin, Wei-Ting; Institute of Nuclear Energy Research, Atomic Energy Council, Taoyuan 32546, Taiwan; Cheng, An, E-mail: ancheng@niu.edu.tw

2013-10-15

Rock wool is an inorganic fibrous substance produced by steam blasting and cooling molten glass. As with other industrial by-products, rock wool particles can be used as cementitious materials or ultra fine fillers in cement-based composites. This study investigated the microstructure of mortar specimens produced with cement-based composites that include various forms of rock wool particles. It conducted compressive strength testing, rapid chloride penetration tests, X-ray diffraction analysis, thermo-gravimetric analysis, and scanning electronic microscopy to evaluate the macro- and micro-properties of the cement-based composites. Test results indicate that inclusion of rock wool particles in composites improved compressive strength and reducedmore » chloride ion penetration at the age of 91 days due to the reduction of calcium hydroxide content. Microscopic analysis confirms that the use of rock wool particles contributed to the formation of a denser, more compact microstructure within the hardened paste. In addition, X-ray diffraction analysis shows few changes in formation of pozzolanic reaction products and no new hydrations are formed with incorporating rock wool particles. - Highlights: • We report the microstructural characterization of cement-based composites. • Different mixes produced with various rock wool particles have been tested. • The influence of different mixes on macro and micro properties has been discussed. • The macro properties are included compressive strength and permeability. • XRD and SEM observations confirm the pozzolanic reaction in the resulting pastes.« less

Microstructure, Porosity and Mechanical Property Relationships of Calcium-Silicate-Hydrate

DTIC Science & Technology

1991-02-15

feasibility of producing S ,,zeolite-cement composites . calcium silicate hydrate (C-S-H) structure, NAS NMR, C3S, pH, zeolites, aluminosilicate hydrate...3 S pH- Composition Plots......................................... 6 X-ray Diffraction...6 The System CaO-A1203-SiO 2 -H2 0................................. 8 pH- Composition Plots......................................... 8 MASNMR

Synthesis of ZnO nanoparticles by a green process and the investigation of their physical properties

NASA Astrophysics Data System (ADS)

Nethavhanani, T.; Diallo, A.; Madjoe, R.; Kotsedi, L.; Maaza, M.

2018-05-01

This contribution reports on the synthesis and the physical properties of ZnO nanoparticles prepared using a green chemistry process. Aspalathus Linearis's extract was used as an effective chelating agent. The whole reaction process for the ZnO nanoparticle was conducted at room temperature. The microstructural properties of ZnO was investigated using X-ray diffraction, furthermore Electron Dispersive X-rays Spectroscopy was employed as quantitative elemental analysis. From the Transmission Electron Microscopy results, the ZnO nanoparticles were found to be highly crystalline with an average diameter of 23.7 nm.

Microstructural characterization of high-manganese austenitic steels with different stacking fault energies

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

Sato, Shigeo, E-mail: s.sato@imr.tohoku.ac.jp; Kwon, Eui-Pyo; Imafuku, Muneyuki

Microstructures of tensile-deformed high-manganese austenitic steels exhibiting twinning-induced plasticity were analyzed by electron backscatter diffraction pattern observation and X-ray diffraction measurement to examine the influence of differences in their stacking fault energies on twinning activity during deformation. The steel specimen with the low stacking fault energy of 15 mJ/m{sup 2} had a microstructure with a high population of mechanical twins than the steel specimen with the high stacking fault energy (25 mJ/m{sup 2}). The <111> and <100> fibers developed along the tensile axis, and mechanical twinning occurred preferentially in the <111> fiber. The Schmid factors for slip and twinning deformationsmore » can explain the origin of higher twinning activity in the <111> fiber. However, the high stacking fault energy suppresses the twinning activity even in the <111> fiber. A line profile analysis based on the X-ray diffraction data revealed the relationship between the characteristics of the deformed microstructures and the stacking fault energies of the steel specimens. Although the variation in dislocation density with the tensile deformation is not affected by the stacking fault energies, the effect of the stacking fault energies on the crystallite size refinement becomes significant with a decrease in the stacking fault energies. Moreover, the stacking fault probability, which was estimated from a peak-shift analysis of the 111 and 200 diffractions, was high for the specimen with low stacking fault energy. Regardless of the difference in the stacking fault energies of the steel specimens, the refined crystallite size has a certain correlation with the stacking fault probability, indicating that whether the deformation-induced crystallite-size refinement occurs depends directly on the stacking fault probability rather than on the stacking fault energies in the present steel specimens. - Highlights: {yields} We studied effects of stacking fault energies on deformed microstructures of steels. {yields} Correlations between texture and occurrence of mechanical twinning are discussed. {yields} Evolutions of dislocations and crystallite are analyzed by line profile analysis.« less

Shape-Controlled Synthesis of NiCo2 O4 Microstructures and Their Application in Supercapacitors.

PubMed

Xiang, Nannan; Ni, Yonghong; Ma, Xiang

2015-09-01

The shape-controlled synthesis of NiCo2 O4 microstructures through a facile hydrothermal method and subsequent calcinations was explored. By employing CoSO4 , NiSO4 , and urea as the starting reactants, flower-like NiCo2 O4 microstructures were obtained at 100 °C after 5 h without the assistance of any additive and subsequent calcination at 300 °C for 2 h; dumbbell-like NiCo2 O4 microstructures were prepared at 150 °C after 5 h in the presence of trisodium citrate and subsequent calcination at 300 °C for 2 h. The as-prepared NiCo2 O4 microstructures were characterized by X-ray powder diffraction, field-emission scanning electron microscopy, energy-dispersive X-ray spectroscopy, and (high-resolution) transmission electron microscopy. Both the flower-like and dumbbell-like NiCo2 O4 microstructures could be used as electrode materials for supercapacitors, and they exhibited excellent electrochemical performance, including high specific capacitance, good rate capability, and excellent long-term cycle stability. Simultaneously, the shape-dependent electrochemical properties of the product were investigated. © 2015 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Microstructures and Mechanical Properties of Co-Cr Dental Alloys Fabricated by Three CAD/CAM-Based Processing Techniques

PubMed Central

Kim, Hae Ri; Jang, Seong-Ho; Kim, Young Kyung; Son, Jun Sik; Min, Bong Ki; Kim, Kyo-Han; Kwon, Tae-Yub

2016-01-01

The microstructures and mechanical properties of cobalt-chromium (Co-Cr) alloys produced by three CAD/CAM-based processing techniques were investigated in comparison with those produced by the traditional casting technique. Four groups of disc- (microstructures) or dumbbell- (mechanical properties) specimens made of Co-Cr alloys were prepared using casting (CS), milling (ML), selective laser melting (SLM), and milling/post-sintering (ML/PS). For each technique, the corresponding commercial alloy material was used. The microstructures of the specimens were evaluated via X-ray diffractometry, optical and scanning electron microscopy with energy-dispersive X-ray spectroscopy, and electron backscattered diffraction pattern analysis. The mechanical properties were evaluated using a tensile test according to ISO 22674 (n = 6). The microstructure of the alloys was strongly influenced by the manufacturing processes. Overall, the SLM group showed superior mechanical properties, the ML/PS group being nearly comparable. The mechanical properties of the ML group were inferior to those of the CS group. The microstructures and mechanical properties of Co-Cr alloys were greatly dependent on the manufacturing technique as well as the chemical composition. The SLM and ML/PS techniques may be considered promising alternatives to the Co-Cr alloy casting process. PMID:28773718

Non-Destructive Characterization of UO2+x Nuclear Fuels

DOE PAGES

Pokharel, Reeju; Brown, Donald W.; Clausen, Bjørn; ...

2017-10-27

This article describes the effect of fabrication conditions on as-sintered microstructures of various stoichiometric ratios of uranium dioxide, UO 2+x, with the aim of enhancing the understanding of fabrication process and developing and validating a predictive microstructurebased model for fuel performance. We demonstrate the ability of novel, non-destructive methods such as near-field high-energy X-ray diffraction microscopy (nf-HEDM) and micro-computed tomography (μ-CT) to probe bulk samples of high-Z materials by non-destructively characterizing three samples: UO 2.00, UO 2.11, and UO 2.16, which were sintered at 1450°C for 4 hours. The measured 3D microstructures revealed that grain size and porosity were influencedmore » by deviation from stoichiometry.« less

Comparison Study on Additive Manufacturing (AM) and Powder Metallurgy (PM) AlSi10Mg Alloys

NASA Astrophysics Data System (ADS)

Chen, B.; Moon, S. K.; Yao, X.; Bi, G.; Shen, J.; Umeda, J.; Kondoh, K.

2018-02-01

The microstructural and mechanical properties of AlSi10Mg alloys fabricated by additive manufacturing (AM) and powder metallurgy (PM) routes were investigated and compared. The microstructures were examined by scanning electron microscopy assisted with electron-dispersive spectroscopy. The crystalline features were studied by x-ray diffraction and electron backscatter diffraction. Room-temperature tensile tests and Vickers hardness measurements were performed to characterize the mechanical properties. It was found that the AM alloy had coarser Al grains but much finer Si precipitates compared with the PM alloy. Consequently, the AM alloy showed more than 100% increment in strength and hardness compared with the PM alloy due to the presence of ultrafine forms of Si, while exhibiting moderate ductility.

Ferromagnetic Mn-Implanted GaP: Microstructures vs Magnetic Properties.

PubMed

Yuan, Ye; Hübner, René; Liu, Fang; Sawicki, Maciej; Gordan, Ovidiu; Salvan, G; Zahn, D R T; Banerjee, D; Baehtz, Carsten; Helm, Manfred; Zhou, Shengqiang

2016-02-17

Ferromagnetic GaMnP layers were prepared by ion implantation and pulsed laser annealing (PLA). We present a systematic investigation on the evolution of microstructure and magnetic properties depending on the pulsed laser annealing energy. The sample microstructure was analyzed by high-resolution X-ray diffraction (HR-XRD), transmission electron microscopy (TEM), Rutherford backscattering spectrometry (RBS), ultraviolet Raman spectroscopy (UV-RS), and extended X-ray absorption fine structure (EXAFS) spectroscopy. The presence of X-ray Pendellösung fringes around GaP (004) and RBS channeling prove the epitaxial structure of the GaMnP layer annealed at the optimized laser energy density (0.40 J/cm(2)). However, a forbidden TO vibrational mode of GaP appears and increases with annealing energy, suggesting the formation of defective domains inside the layer. These domains mainly appear in the sample surface region and extend to almost the whole layer with increasing annealing energy. The reduction of the Curie temperature (TC) and of the uniaxial magnetic anisotropy gradually happens when more defects and the domains appear as increasing the annealing energy density. This fact univocally points to the decisive role of the PLA parameters on the resulting magnetic characteristics in the processed layers, which eventually determine the magnetic (or spintronics) figure of merit.

Characterization of a cold-rolled 2101 lean duplex stainless steel.

PubMed

Bassani, Paola; Breda, Marco; Brunelli, Katya; Mészáros, Istvan; Passaretti, Francesca; Zanellato, Michela; Calliari, Irene

2013-08-01

Duplex stainless steels (DSS) may be defined as a category of steels with a two-phase ferritic-austenitic microstructure, which combines good mechanical and corrosion properties. However, these steels can undergo significant microstructural modification as a consequence of either thermo-mechanical treatments (ferrite decomposition, which causes σ- and χ-phase formation and nitride precipitation) or plastic deformation at room temperature [austenite transformation into strain-induced martensite (SIM)]. These secondary phases noticeably affect the properties of DSS, and therefore are of huge industrial interest. In the present work, SIM formation was investigated in a 2101 lean DSS. The material was subjected to cold rolling at various degrees of deformation (from 10 to 80% thickness reduction) and the microstructure developed after plastic deformation was investigated by electron backscattered diffraction, X-ray diffraction measurements, and hardness and magnetic tests. It was observed that SIM formed as a consequence of deformations higher than ~20% and residual austenite was still observed at 80% of thickness reduction. Furthermore, a direct relationship was found between microstructure and magnetic properties.

Effect of the microstructure on the thermoelectric properties of polycrystalline lanthanum chalcogenides

NASA Technical Reports Server (NTRS)

Lockwood, A.; Wood, C.; Vandersande, J.; Zoltan, A.; Parker, J.; Danielson, L.; Alexander, M.; Whittenberger, D.

1987-01-01

Small amounts of second phase materials can have important effects on the thermoelectric properties of polycrystalline gamma-La(3-x)X4 (X-S, Te; X in the range of 0 to 1/3). Microscopic examination by SEM of hot pressed La(3-x)Te4 samples has revealed from 1-5 vol. pct of La2O2Te, an amount which is not detected by X-ray powder diffraction measurements. This amount of La2O2Te resulting from oxygen contamination can reduce the concentration of electrons by as much as 10 to 75 percent below the electron concentration calculated for single phase La(3-x)Te4 in the composition range of greatest interest. Small amounts of second phase materials can also lower the lattice thermal conductivity by scattering low frequency phonons. These results indicate that microstructural effects should be considered when electrical and thermal properties of polycrystalline materials are analyzed.

Multi-scale mechanics of granular solids from grain-resolved X-ray measurements

NASA Astrophysics Data System (ADS)

Hurley, R. C.; Hall, S. A.; Wright, J. P.

2017-11-01

This work discusses an experimental technique for studying the mechanics of three-dimensional (3D) granular solids. The approach combines 3D X-ray diffraction and X-ray computed tomography to measure grain-resolved strains, kinematics and contact fabric in the bulk of a granular solid, from which continuum strains, grain stresses, interparticle forces and coarse-grained elasto-plastic moduli can be determined. We demonstrate the experimental approach and analysis of selected results on a sample of 1099 stiff, frictional grains undergoing multiple uniaxial compression cycles. We investigate the inter-particle force network, elasto-plastic moduli and associated length scales, reversibility of mechanical responses during cyclic loading, the statistics of microscopic responses and microstructure-property relationships. This work serves to highlight both the fundamental insight into granular mechanics that is furnished by combined X-ray measurements and describes future directions in the field of granular materials that can be pursued with such approaches.

The substitution of aluminum for cobalt in nanostructured bainitic steels

NASA Astrophysics Data System (ADS)

Yang, Jing; Qiu, Hui; Xu, Pudong; Yu, Hui; Wang, Yuchen

2018-06-01

Two kinds of new steels are designed, in which the only difference is the use of the alloy element aluminum instead of cobalt. The effect of cobalt and aluminum addition on the microstructure and mechanical properties of high-carbon nanostructured bainitic steels was studied. The microstructure and mechanical properties achieved by a low temperature au tempering treatment were investigated by optical microscopy, X-ray diffraction, scanning and transmission electron microscopy and hardness, tension, impact tests. The experimental results show that better mechanical properties were achieved in the high-carbon Al-contained steel.

The comparison of microstructures and mechanical properties between 14Cr-Al and 14Cr-Ti ferritic ODS alloys

DOE PAGES

Zhang, Guangming; Zhou, Zhangjian; Mo, Kun; ...

2016-03-03

In this study, two kinds of 14Cr ODS alloys (14Cr-Al and 14Cr-Ti) were investigated to reveal the different effects between Al and Ti on the microstructures and mechanical properties of 14Cr ferritic ODS alloys. The microstructure information such as grains, minor phases of these two alloys has been investigated by high-energy X-ray diffraction and transmission electron microscopy (TEM). The in situ synchrotron X-ray diffraction tensile test was applied to investigate the mechanical properties of these two alloys. The lattice strains of different phases through the entire tensile deformation process in these two alloys were analyzed to calculate their elastic stresses.more » From the comparison of elastic stress, the strengthening capability of Y 2Ti 2O 7 is better than TiN in 14Cr-Ti, and the strengthening capability of YAH is much better than YAM and AlN in 14Cr-Al ODS. The dislocation densities of 14Cr-Ti and 14Cr-Al ODS alloys during tensile deformation were also examined by modified Williamson-Hall analyses of peak broadening, respectively. In conclusion, the different increasing speed of dislocation density with plastic deformation reveals the better strengthening effect of Y-Ti-O particles in 14Cr-Ti ODS than that of Y-Al-O particles in 14Cr-Al ODS alloy.« less

Cross-sectional transmission electron microscopic study of irradiation induced nano-crystallization of nickel in a W/Ni multilayer.

PubMed

Bagchi, Sharmistha; Lalla, N P

2008-06-11

The present study reports the cross-sectional transmission electron microscopic investigations of swift heavy ion-irradiation induced nano-size recrystallization of Ni in a nearly immiscible W/Ni multilayer structure. Multilayer structures (MLS) of [W(25 Å)/Ni(25 Å)](10BL) were grown on Si-(100) substrate by the ion-beam sputtering technique. The as-synthesized MLS were subjected to 120 MeV-Au(9+) ion-irradiation to a fluence of ∼5 × 10(13) ions cm(-2). Wide-angle x-ray diffraction studies of pristine as well as irradiated W/Ni multilayers show deterioration of the superlattice structure, whereas x-ray reflectivity (XRR) measurement reveals a nearly unaffected microstructure after irradiation. Analysis of the XRR data using 'Parratt's formalism' does show a significant increase of W/Ni interface roughness. Cross-sectional transmission electron microscopy (TEM) studies carried out in diffraction and imaging modes (including bright-field and dark-field imaging), show that at high irradiation dose the intralayer microstructure of Ni becomes nano-crystalline (1-2 nm). During these irradiation induced changes of the intralayer microstructure, the interlayer definition of the W and Ni layers still remains intact. The observed nano-recrystallization of Ni has been attributed to competition between low miscibility of the W/Ni interface and the ion-beam induced mixing kinetics.

Progress in development of tapes and magnets made from Bi-2223 superconductors

NASA Technical Reports Server (NTRS)

Balachandran, U.; Iyer, A. N.; Haldar, P.; Hoehn, J. G., Jr.; Motowidlo, L. R.

1995-01-01

Long lengths of (Bi,Pb)2Sr2Ca2Cu3O(x) tapes made by powder-in-tube processing have been wound into coils. Performance of the coils has been measured at temperatures of 4.2 to 77 K, and microstructures have been examined by x-ray diffraction and electron microscopy and then related to superconducting properties. A summary of recent results and an overview of future goals are presented.

Graphene nanoplate-MnO2 composites for supercapacitors: a controllable oxidation approach

NASA Astrophysics Data System (ADS)

Huang, Huajie; Wang, Xin

2011-08-01

Graphene nanoplate-MnO2 composites have been synthesized by oxidising part of the carbon atoms in the framework of graphene nanoplates at ambient temperature. The composites were characterized by means of X-ray diffraction (XRD), Raman spectroscopy, scanning electron microscopy (SEM), transmission electron microscopy (TEM), X-ray photoelectron spectroscopy (XPS) and cyclic voltammetry (CV). It was found that the oxidation extent of the carbon atoms in the graphene framework in these composites was dependent on the reaction time, which also influenced their microstructure, morphology and electrochemical properties. Compared with MnO2 nanolamellas, the nanocomposite prepared with a reaction time of 3 h reveals better electrochemical properties as a supercapacitor electrode material.Graphene nanoplate-MnO2 composites have been synthesized by oxidising part of the carbon atoms in the framework of graphene nanoplates at ambient temperature. The composites were characterized by means of X-ray diffraction (XRD), Raman spectroscopy, scanning electron microscopy (SEM), transmission electron microscopy (TEM), X-ray photoelectron spectroscopy (XPS) and cyclic voltammetry (CV). It was found that the oxidation extent of the carbon atoms in the graphene framework in these composites was dependent on the reaction time, which also influenced their microstructure, morphology and electrochemical properties. Compared with MnO2 nanolamellas, the nanocomposite prepared with a reaction time of 3 h reveals better electrochemical properties as a supercapacitor electrode material. Electronic supplementary information (ESI) available: Fig. S1, AFM image (5 μm × 5 μm) of graphene nanoplate-MnO2 composite obtained at 3 h; Fig. S2, nitrogen adsorption/desorption isotherm of graphene nanoplate-MnO2 composite obtained at 3 h. See DOI: 10.1039/c1nr10229j

Characterization of Microstructure and Mechanical Properties of Mg-8Li-3Al-1Y Alloy Subjected to Different Rolling Processes

NASA Astrophysics Data System (ADS)

Zhou, Xiao; Liu, Qiang; Liu, Ruirui; Zhou, Haitao

2018-06-01

The mechanical properties and microstructure evolution of Mg-8Li-3Al-1Y alloy undergoing different rolling processes were systematically investigated. X-ray diffraction, optical microscope, scanning electron microscopy, transmission electron microscopy as well as electron backscattered diffraction were used for tracking the microstructure evolution. Tensile testing was employed to characterize the mechanical properties. After hot rolling, the MgLi2Al precipitated in β-Li matrix due to the transformation reaction: β-Li → β-Li + MgLi2Al + α-Mg. As for the alloy subjected to annealed hot rolling, β-Li phase was clearly recrystallized while recrystallization rarely occurred in α-Mg phase. With regard to the microstructure undergoing cold rolling, plenty of dislocations and dislocation walls were easily observed. In addition, the microstructure of alloys subjected to annealed cold rolling revealed the formation of new fresh α-Mg grains in β-Li phase due to the precipitation reaction. The mechanical properties and fracture modes of Mg-8Li-3Al-1Y alloys can be effectively tuned by different rolling processes.

ON MEASUREMENT OF CARBON CONTENT IN RETAINED AUSTENITE IN A NANOSTRUCTURED BAINITIC STEEL

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

Garcia-Mateo, C.; Caballero, Francesca G.; Miller, Michael K

2012-01-01

In this study, the carbon content of retained austenite in a nanostructured bainitic steel was measured by atom probe tomography and compared with data derived from the austenite lattice parameter determined by X-ray diffraction. The results provide new evidence about the heterogeneous distribution of carbon in austenite, a fundamental issue controlling ductility in this type of microstructure.

Texture measurement of shaped material by impulse acoustic microscopy

PubMed

Eyraud; Nadal; Gondard

2000-03-01

All the microstructural parameters involved in metallurgical processes are difficult to determine directly on a shaped material. The aim of this paper is to use an impulse line-focus acoustic microscope (LFAM) as a non-destructive alternative to X-ray diffraction for measuring texture of slightly anisotropic materials. We apply it to characterize the rolling and annealing texture for tantalum sheets.

Influence of Annealing on the Depth Microstructure of the Shot Peened Duplex Stainless Steel at Elevated Temperature

NASA Astrophysics Data System (ADS)

Feng, Qiang; She, Jia; Xiang, Yong; Wu, Xianyun; Wang, Chengxi; Jiang, Chuanhai

The depth profiles of residual stresses and lattice parameters in the surface layers of shot peened duplex stainless steel at elevated temperature were investigated utilizing X-ray diffraction analysis. At each deformation depth, residual stress distributions in both ferrite and austenite were studied by X-ray diffraction stress analysis which is performed on the basis of the sin2ψ method and the lattice parameters were explored by Rietveld method. The results reveal that difference changes of depth residual compressive stress profiles between ferrite and austenite under the same annealing condition are resulted from the diverse coefficient of thermal expansion, dislocation density, etc. for different phases in duplex stainless steel. The relaxations of depth residual stresses in austenite are more obvious than those in ferrite. The lattice parameters decrease in the surface layer with the extending of annealing time, however, they increase along the depth after annealing for 16min. The change of the depth lattice parameters can be ascribed to both thermal expansion and the relaxation of residual stress. The different changes of microstructure at elevated temperature between ferrite and austenite are discussed.

Determination of 200 °C Isothermal Section of Al-Ag-Ga Phase Diagram by Microanalysis, X-ray Diffraction, Hardness and Electrical Conductivity Measurements

NASA Astrophysics Data System (ADS)

Premović, Milena; Tomović, Milica; Minić, Duško; Manasijević, Dragan; Živković, Dragana; Ćosović, Vladan; Grković, Vladan; Đorđević, Aleksandar

2017-04-01

Ternary Al-Ag-Ga system at 200 °C was experimentally and thermodynamically assessed. Isothermal section was extrapolated using optimized thermodynamic parameters for constitutive binary systems. Microstructure and phase composition of the selected alloy samples were analyzed using light microscopy, scanning electron microscopy combined with energy-dispersive spectrometry and x-ray powder diffraction technique. The obtained experimental results were found to be in a close agreement with the predicted phase equilibria. Hardness and electrical conductivity of the alloy samples from four vertical sections Al-Ag80Ga20, Al-Ag60Ga40, Ag-Al80Ga20 and Ag-Al60Ga40 of the ternary Al-Ag-Ga system at 200 °C were experimentally determined using Brinell method and eddy current measurements. Additionally, hardness of the individual phases present in the microstructure of the studied alloy samples was determined using Vickers microhardness test. Based on experimentally obtained results, isolines of Brinell hardness and electrical conductivity were calculated for the alloys from isothermal section of the ternary Al-Ag-Ga system at 200 °C.

Effect of laser welding parameters on the austenite and martensite phase fractions of NiTi

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

Oliveira, J.P., E-mail: jp.oliveira@campus.fct.unl

Although laser welding is probably the most used joining technique for NiTi shape memory alloys there is still a lack of understanding about the effects of laser welding parameters on the microstructural induced changes: in both the heat affected and fusion zones martensite may be present, while the base material is fully austenitic. Synchrotron X-ray diffraction was used for fine probing laser welded NiTi joints. Through Rietveld refinement the martensite and austenite phase fractions were determined and it was observed that the martensite content increases towards the weld centreline. This is related to a change of the local transformation temperaturesmore » on these regions, which occurs due to compositional variation in those regions. The martensite phase fraction in the thermally affected regions may have significant implications on functional properties on these joints. - Highlights: •Synchrotron X-ray diffraction was used for fine probing of the microstructure in laser welded NiTi joints. •Rietveld refinement allowed to determine the content of martensite along the heat affected and fusion zones. •The martensite content increases from the base material towards the weld centreline.« less

Investigation on surface layer characteristics of shot peened graphene reinforced Al composite by X-ray diffraction method

NASA Astrophysics Data System (ADS)

Zhan, Ke; Wu, Yihao; Li, Jiongli; Zhao, Bin; Yan, Ya; Xie, Lechun; Wang, Lianbo; Ji, V.

2018-03-01

Graphene reinforced Al composite with high mechanical property was successfully reported. However, there are quite limited studies about shot peening effect on this new type material. Here, 1.0 wt% graphene reinforced Al composite was produced by powder metallurgy and treated by shot peening. The surface layer characteristics of shot peened composite was investigated by X-ray diffraction line profile analysis. The microstructure including domain size, micro-strain, dislocation density and crystalline texture were analyzed. The results showed that after surface shot-peening, the domain size were refined, the dislocation density of the composite was increased sharply to 9.0 × 1011/cm2 at the top surface. The original strong texture was diminished after shot peening. Based on the calculated results, the microstructure variation of composite was more severe than that of Al without graphene reinforcement after shot peening. Besides, the micro-hardness of composite at the top surface increased up to 75HV one time higher than that of matrix. It is concluded that shot peening can be considered as an essential process of improving the surface properties of graphene reinforced Al composite.

Structural and microstructural description of the glacial state in triphenyl phosphite from powder synchrotron X-ray diffraction data and Raman scattering investigations

NASA Astrophysics Data System (ADS)

Derollez, P.; Hernandez, O.; Hédoux, A.; Guinet, Y.; Masson, O.; Lefebvre, J.; Descamps, M.

2004-06-01

The structure and microstructure (refinement of the isotropic size and microstrain parameters) of the glacial state in triphenyl phosphite (TPP, P(OC 6H 5) 3) transformed at 222K have been determined from powder synchrotron X-ray diffraction data through a Rietveld and a Le Bail refinement, respectively. It is shown that the glacial state is composed of crystallites of the stable crystal phase coexisting with non-transformed supercooled liquid, the apparent size of the crystallites—depending on the aging temperature at which the glacial state is isothermally formed, [Phys. Rev. B 60 (1999) 9390]—being equal to 329.2(2) Å at 222K. The molecular conformation is slightly less mirror-symmetric than the one in the crystal state, and correlatively only one of the two unusual weak intermolecular C-H⋯O hydrogen bonds already observed in the latter state is encountered in the glacial one. Additional Raman scattering investigations confirm the previous result and reveal in addition that no hydrogen bonding interaction is observed neither in the glass nor in the liquid states.

Microstructural Characterization and Modeling of SLM Superalloy 718

NASA Technical Reports Server (NTRS)

Smith, Tim M.; Sudbrack, Chantal K.; Bonacuse, Pete; Rogers, Richard

2017-01-01

Superalloy 718 is an excellent candidate for selective laser melting (SLM) fabrication due to a combination of excellent mechanical properties and workability. Predicting and validating the microstructure of SLM-fabricated Superalloy 718 after potential post heat-treatment paths is an important step towards producing components comparable to those made using conventional methods. At present, obtaining accurate volume fraction and size measurements of gamma-double-prime, gamma-prime and delta precipitates has been challenging due to their size, low volume fractions, and similar chemistries. A technique combining high resolution distortion corrected SEM imaging and with x-ray energy dispersive spectroscopy has been developed to accurately and independently measure the size and volume fractions of the three precipitates. These results were further validated using x-ray diffraction and phase extraction methods and compared to the precipitation kinetics predicted by PANDAT and JMatPro. Discrepancies are discussed in context of materials properties, model assumptions, sampling, and experimental errors.

Synthesis and Characterization of Multi Wall Carbon Nanotubes (MWCNT) Reinforced Sintered Magnesium Matrix Composites

NASA Astrophysics Data System (ADS)

Vijaya Bhaskar, S.; Rajmohan, T.; Palanikumar, K.; Bharath Ganesh Kumar, B.

2016-04-01

Metal matrix composites (MMCs) reinforced with ceramic nano particles (less than 100 nm), termed as metal matrix nano composites (MMNCs), can overcome those disadvantages associated with the conventional MMCs. MMCs containing carbon nanotubes are being developed and projected for diverse applications in various fields of engineering like automotive, avionic, electronic and bio-medical sectors. The present investigation deals with the synthesis and characterization of hybrid magnesium matrix reinforced with various different wt% (0-0.45) of multi wall carbon nano tubes (MWCNT) and micro SiC particles prepared through powder metallurgy route. Microstructure and mechanical properties such as micro hardness and density of the composites were examined. Microstructure of MMNCs have been investigated by scanning electron microscope, X-ray diffraction and energy dispersive X-ray spectroscopy (EDS) for better observation of dispersion of reinforcement. The results indicated that the increase in wt% of MWCNT improves the mechanical properties of the composite.

Qualification of Ti6Al4V ELI Alloy Produced by Laser Powder Bed Fusion for Biomedical Applications

NASA Astrophysics Data System (ADS)

Yadroitsev, I.; Krakhmalev, P.; Yadroitsava, I.; Du Plessis, A.

2018-03-01

Rectangular Ti6Al4V extralow interstitials (ELI) samples were manufactured by laser powder bed fusion (LPBF) in vertical and horizontal orientations relative to the build platform and subjected to various heat treatments. Detailed analyses of porosity, microstructure, residual stress, tensile properties, fatigue, and fracture surfaces were performed based on x-ray micro-computed tomography, scanning electron microscopy, and x-ray diffraction methods. The types of fracture and the tensile fracture mechanisms of the LPBF Ti6Al4V ELI alloy were also studied. Detailed analysis of the microstructure and the corresponding mechanical properties were compared against standard specifications for conventional Ti6Al4V alloy for use in surgical implant applications. Conclusions regarding the mechanical properties and heat treatment of LPBF Ti6Al4V ELI for biomedical applications are made.

Microstructure and Properties of Zircon-Added Carbon Refractories for Blast Furnace

NASA Astrophysics Data System (ADS)

Zhu, Tianbin; Li, Yawei; Sang, Shaobai; Chen, Xilai; Zhao, Lei; Li, Yuanbing; Li, Shujing

2012-11-01

Microstructure and properties of zircon-added carbon refractory specimens for blast furnace (BF) were investigated with the aid of X-ray diffraction (XRD), a scanning electron microscope (SEM), energy-dispersive X-ray, mercury porosimetry, and a laser thermal conductivity (TC) meter. Additives could influence the matrix structures and improve the properties of specimens. With the increase of zircon powder content, the amount of SiC whiskers formed increased and their aspect ratio became larger, and the SiC whiskers tended to be distributed homogeneously. Zircon powder additions decreased the mean pore diameter and increased <1- μm pore volume by filling in pores via SiC, improved the TC and the cold crushing strength (CCS) due to the in-situ formation of the more well-developed SiC whiskers with high TC, and significantly reduced the molten iron attack to carbon specimens.

Effect of Heat Treatment on Microstructure and Magnetostrictive Property of Melt-Spun Fe85Ga15 Ribbons

NASA Astrophysics Data System (ADS)

Liu, Hao; Wang, Haiou; Cao, Mengxiong; Tan, Weishi; Shi, Yangguang; Chen, Yu; Huang, Yuying

2013-09-01

In order to study the microstructure of Fe-Ga alloy, Fe85Ga15 ribbons prepared with different wheel velocity were studied by high resolution X-ray diffraction (HRXRD) and extend X-ray absorption fine structure (EXAFS). HRXRD patterns showed that only disordered A2 phase was observed in as-cast Fe85Ga15 alloy. A modified-DO3 phase was detected in all of the melt spun samples. The HRXRD associated with EXAFS results indicated that Ga atoms were located as second-nearest neighbor along [100] orientation. A little DO3 phase was found in ribbons annealed at 1000°C under 0.06 MPa Ar atmosphere. The result of magnetostriction measurement revealed that in the ribbon prepared with higher wheel velocity, more modified-DO3 phase will enhance the magnetostriction. DO3 phase in the annealed sample will deteriorate the magnetostrictive properties of Fe-Ga ribbons.

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

Chang, L. L.; Wang, Y. D.; Ren, Y.

Microstructure evolution, mechanical behaviors of cold rolled Ti-Nb alloys with different Nb contents subjected to different heat treatments were investigated. Here, optical microstructure and phase compositions of Ti-Nb alloys were characterized using optical microscopy and X-ray diffractometre, while mechanical behaviors of Ti-Nb alloys were examined by using tension tests. Stress-induced martensitic transformation in a Ti-30. at%Nb binary alloy was in-situ explored by synchrotron-based high-energy X-ray diffraction (HE-XRD). The results obtained suggested that mechanical behavior of Ti-Nb alloys, especially Young's modulus was directly dependent on chemical compositions and heat treatment process. According to the results of HE-XRD, α"-V1 martensite generated priormore » to the formation of α"-V2 during loading and a partial reversible transformation from α"-V1 to β phase was detected while α"-V2 tranformed to β completely during unloading.« less

Synthesis, microstructure, and magnetic properties of monosized Mn x Zn y Fe3 − x − y O4 ferrite nanocrystals

PubMed Central

2013-01-01

We report the synthesis and characterization of ferrite nanocrystals which exhibit high crystallinity and narrow size distributions. The three types of samples including Zn ferrite, Mn ferrite, and Mn-Zn ferrite were prepared via a non-aqueous nanoemulsion method. The structural, chemical, and magnetic properties of the nanocrystals are analyzed by transmission electron microscopy, X-ray diffraction, X-ray fluorescence, and physical property measurement system. The characterization indicates that the three types of ferrite nanocrystals were successfully produced, which show well-behaved magnetic properties, ferrimagnetism at 5 K and superparamagnetism at 300 K, respectively. In addition, the magnetization value of the ferrites increases with the increasing concentration of Mn. PMID:24344630

Analyse de l'état mécanique et microstructural de films minces supraconducteurs YBa_2 Cu_3O_7 par diffraction des rayons X

NASA Astrophysics Data System (ADS)

Auzary, S.; Badawi, K. F.; Bimbault, L.; Rabier, J.; Gaboriaud, R. J.; Goudeau, Ph.

1997-01-01

Mechanical and microstructural analysis in a 100nm thin film is presented in this study. Using X-ray diffraction with a tensorial approach, we have determined stresses, strains, stress-free lattice parameters, microdistorsions and diffracting coherent domains size. Stress-free lattice parameters are higher than the bulk values. A high value of stresses is explained as a combination of coherent stresses, thermal stresses and intrinsic ones. Diffraction peaks line profiles analysis suggests grain boundaries presence as well as high lattice elastic microdistorsions. Cette étude présente une analyse de l'état mécanique et microstructurale dans un film mince de 100nm d'épaisseur d'YBCO déposé sur un substrat de MgO. En utilisant la diffraction des rayons X couplée à une approche tensorielle, nous avons déterminé les déformations, les contraintes, les paramètres libres de contraintes, les microdistorsions élastiques ainsi que la taille des domaines cohérents de diffraction. Les paramètres libres de contrainte sont supérieurs à ceux du massif. Une valeur élevée des contraintes est expliquée à partir des contraintes de cohérence, des contraintes thermiques et intrinsèques. L'analyse des profils des pics de diffraction suggère la présence de sous-joints et de distorsions élastiques élevées au niveau des mailles cristallographiques.

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

[Characterization of microstructure of ibuprofen-hydroxypropyl-beta-cyclodextrin and ibuprofen-beta-cyclodextrin by atomic force microscope].

PubMed

Wang, Li-juan; Zhu, Zhao-jing; Che, Ke-ke; Ju, Feng-ge

2008-09-01

The microstructures of ibuprofen-hydroxypropyl-bets-cyclodextrin (IBU-HP-beta-CyD) and ibuprofen-beta-cyclodextrin (IBU-beta-CyD) were observed by atomic force microscope (AFM). The high resolving capability of AFM has the tungsten filament probe with the spring constant of 0.06 N x m(-1). Samples were observed in a small scale scanning area of 10.5 nm x 10.5 nm and 800 x 800 pixels. The original scanning images were gained by tapping mode at room temperature. Their three-dimensional reconstruction of microstructure was performed by G3DR software. The outer diameters of HP-beta-CyD and beta-CyD are 1.53 nm. The benzene diameter of IBU is 0.62 nm, fitting to the inner diameters of HP-beta-CyD and beta-CyD. The benzene and hydrophobic chain of IBU enter into the hole of cyclodextrin at 1:1 ratio. The results were evidenced by IR, X-ray diffraction and the phase solubility.

Microstructure evolution of heat treated NiTi alloys

NASA Astrophysics Data System (ADS)

Losertová, M.; Štencek, M.; Matýsek, D.; Štefek, O.; Drápala, J.

2017-11-01

Superelastic behavior of off-stoichiometric NiTi alloys is significantly affected by microstructure changes due to heat treatment. Applying appropriate thermal treatments important effects on microstructural changes, transformation temperatures and thermomechanical properties of final NiTi products can be achieved. The experimental samples of NiTi alloy with 55.8 wt.% Ni were submitted to heat treatment and the microstructures before and after the treatment were observed. The thermal regimes consisted of annealing treatment at 600 °C for 1 hour followed by water quenching and of ageing at eight different temperatures (250, 270, 290, 300, 350, 400, 450 and 500 °C) for 30 minutes. Microstructure features studied by means of optical and scanning electron microscopies, EDX microanalyses, X-ray diffraction analyses and microhardness measurement, have shown that higher ageing temperatures led to microstructure changes and corresponding increase in microhardness.

Characterization of low thermal conductivity PAN-based carbon fibers

NASA Technical Reports Server (NTRS)

Katzman, Howard A.; Adams, P. M.; Le, T. D.; Hemminger, Carl S.

1992-01-01

The microstructure and surface chemistry of eight low thermal conductivity (LTC) PAN-based carbon fibers were determined and compared with PAN-based fibers heat treated to higher temperatures. Based on wide-angle x ray diffraction, the LTC PAN fibers all appear to have a similar turbostratic structure with large 002 d-spacings, small crystallite sizes, and moderate preferred orientation. Limited small-angle x ray scattering (SAXS) results indicate that, with the exception of LTC fibers made by BASF, the LTC fibers do not have well developed pores. Transmission electron microscopy shows that the texture of the two LTC PAN-based fibers studied (Amoco T350/23X and /25X) consists of multiple sets of parallel, wavy, bent layers that interweave with each other forming a complex three dimensional network oriented randomly around the fiber axis. X ray photoelectron spectroscopy (XPS) analysis finds correlations between heat treated temperatures and the surface composition chemistry of the carbon fiber samples.

Microstructure and corrosion resistance of sputter-deposited titanium-chromium alloy coatings

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

Landolt, D.; Robyr, C.; Mettraux, P.

1998-10-01

Titanium, chromium, and titanium-chromium alloy coatings were sputter-deposited to study their corrosion behaviors in relation to microstructure and composition. Silicon substrates were used to study the effect of alloying on intrinsic corrosion resistance of the coating materials, and brass substrates were used to study the effect of alloying on the penetrating porosity of the coatings. Corrosion behavior was characterized using linear sweep voltammetry. The crystal structure of the coatings was examined by x-ray diffraction (XRD) and the microstructure by scanning electron microscopy (SEM). Electrochemical impedance spectroscopy (EIS) was used to estimate the real surface area of the coatings. Results showedmore » alloying of titanium with chromium greatly influenced microstructure of the coatings. Alloying led to deposits of higher apparent density and, in some cases, to an x-ray amorphous structure. Alloy coatings showed significantly lower corrosion currents than the constituting metals. The effect was attributed to a smoother surface topography. When corrected of differences in real surface area, the intrinsic corrosion rate of the alloy coatings did not differ significantly from that of the constituting metals. Alloy coatings deposited on brass exhibited a lower porosity than titanium or chromium metal coatings produced under identical conditions.« less

Effect of sintering temperature on the electrolysis of TiO2

NASA Astrophysics Data System (ADS)

Li, Ze-quan; Ru, Li-yue; Bai, Cheng-guang; Zhang, Na; Wang, Hai-hua

2012-07-01

The effects of sintering temperature on the microstructure and the conductivity of TiO2 cathodes were studied by examining the phase composition, microstructure, and element contents of the sintered cathodes and the cathodic products using X-ray diffraction and scanning electronic microscopy-energy dispersive spectrometry. The oxygen vacancy, conductivity, average pore diameter, and specific surface area of the sintered cathodes were detected by X-ray photoelectron spectroscopy, four-point probe, and ASPA 2010. The results showed that TiO2 phase transformations occurred, and oxygen vacancies formed with the increase of sintering temperature. The cathodic conductivity improved, but the average pore diameter and the effective response area of the TiO2 cathode were reduced when the sintering temperature increased. These phenomena could weaken the contact between reaction ions and electrons and also had the same effect on the cathodes and the molten salt. Moreover, they were disadvantageous to ion migration, so a lower sintering temperature was favorable for the microstructure of electrolysis. Consequently, the cathodic conductivity may be improved, but the microstructure became compact with the increase of sintering temperature. The cathodic products at different temperatures indicated that the cathodic conductivity was more important for electrolysis.

In-situ Observation of Cross-Sectional Microstructural Changes and Stress Distributions in Fracturing TiN Thin Film during Nanoindentation.

PubMed

Zeilinger, Angelika; Todt, Juraj; Krywka, Christina; Müller, Martin; Ecker, Werner; Sartory, Bernhard; Meindlhumer, Michael; Stefenelli, Mario; Daniel, Rostislav; Mitterer, Christian; Keckes, Jozef

2016-03-07

Load-displacement curves measured during indentation experiments on thin films depend on non-homogeneous intrinsic film microstructure and residual stress gradients as well as on their changes during indenter penetration into the material. To date, microstructural changes and local stress concentrations resulting in plastic deformation and fracture were quantified exclusively using numerical models which suffer from poor knowledge of size dependent material properties and the unknown intrinsic gradients. Here, we report the first in-situ characterization of microstructural changes and multi-axial stress distributions in a wedge-indented 9 μm thick nanocrystalline TiN film volume performed using synchrotron cross-sectional X-ray nanodiffraction. During the indentation, needle-like TiN crystallites are tilted up to 15 degrees away from the indenter axis in the imprint area and strongly anisotropic diffraction peak broadening indicates strain variation within the X-ray nanoprobe caused by gradients of giant compressive stresses. The morphology of the multiaxial stress distributions with local concentrations up to -16.5 GPa correlate well with the observed fracture modes. The crack growth is influenced decisively by the film microstructure, especially by the micro- and nano-scopic interfaces. This novel experimental approach offers the capability to interpret indentation response and indenter imprint morphology of small graded nanostructured features.

Microstructure characteristics of Ni/WC composite cladding coatings

NASA Astrophysics Data System (ADS)

Yang, Gui-rong; Huang, Chao-peng; Song, Wen-ming; Li, Jian; Lu, Jin-jun; Ma, Ying; Hao, Yuan

2016-02-01

A multilayer tungsten carbide particle (WCp)-reinforced Ni-based alloy coating was fabricated on a steel substrate using vacuum cladding technology. The morphology, microstructure, and formation mechanism of the coating were studied and discussed in different zones. The microstructure morphology and phase composition were investigated by scanning electron microscopy, optical microscopy, X-ray diffraction, and energy-dispersive X-ray spectroscopy. In the results, the coating presents a dense and homogeneous microstructure with few pores and is free from cracks. The whole coating shows a multilayer structure, including composite, transition, fusion, and diffusion-affected layers. Metallurgical bonding was achieved between the coating and substrate because of the formation of the fusion and diffusion-affected layers. The Ni-based alloy is mainly composed of γ-Ni solid solution with finely dispersed Cr7C3/Cr23C6, CrB, and Ni+Ni3Si. WC particles in the composite layer distribute evenly in areas among initial Ni-based alloying particles, forming a special three-dimensional reticular microstructure. The macrohardness of the coating is HRC 55, which is remarkably improved compared to that of the substrate. The microhardness increases gradually from the substrate to the composite zone, whereas the microhardness remains almost unchanged in the transition and composite zones.

Microstructural Examination of Oxidized Fe_(14-x) Nb5_x Alloy Produced from Powders Prepared by Mechanical Alloying

NASA Astrophysics Data System (ADS)

Demirkıran, A. Şükran; Sen, Saduman; Ozdemir, Ozkan; Sen, Ugur

In the present study, ferrous niobium, ferrous boron and iron were used as starting powders. The mixture of the powders which were calculated to give the designed compositions was prepared by using planetary high energy ball mill. Mechanically alloyed powders were pressed and sintered at 1350°C for 120 min in Ar atmosphere. The cyclic oxidation experiments were carried out in an electrical furnace at 650, 750 and 850 °C in open atmosphere for 96 h. The specimens were periodically weighed for the determination of weight change. Before and after oxidation, the present phases of the samples were determined by X-ray diffraction analysis (XRD). The microstructural characterizations were realized using scanning electron microscopy (SEM) with EDS attachment.

Yttrium enrichment and improved magnetic properties in partially melted Y-Ba-Cu-O materials

NASA Technical Reports Server (NTRS)

Alterescu, Sidney; Hojaji, Hamid; Barkatt, Aaron; Michael, Karen A.; Hu, Shouxiang

1990-01-01

The yttrium-rich compositions in the Y-Ba-Cu-O system were mapped out in a systematic manner to quantify their magnetic properties and to correlate them with the microstructure and phase composition as determined by scanning electron microscopy and X-ray diffraction analysis. It is found that the microstructure of Y-Ba-Cu-O compositions is a sensitive function of both their composition and processing conditions. Measurements of magnetic susceptibility and maximum (low-field) and remanent magnetization for the system Y:Ba:Cu = x:2:3 show highest values for x = 2. The corresponding structures involve numerous small crystals of Y2BaCuO5 (211) embedded in highly ordered assemblages of continous YBa2Cu3O(7-y) (123) layers.

Deep X-ray lithography for the fabrication of microstructures at ELSA

NASA Astrophysics Data System (ADS)

Pantenburg, F. J.; Mohr, J.

2001-07-01

Two beamlines at the Electron Stretcher Accelerator (ELSA) of Bonn University are dedicated for the production of microstructures by deep X-ray lithography with synchrotron radiation. They are equipped with state-of-the-art X-ray scanners, maintained and used by Forschungszentrum Karlsruhe. Polymer microstructure heights between 30 and 3000 μm are manufactured regularly for research and industrial projects. This requires different characteristic energies. Therefore, ELSA operates routinely at 1.6, 2.3 and 2.7 GeV, for high-resolution X-ray mask fabrication, deep and ultra-deep X-ray lithography, respectively. The experimental setup, as well as the structure quality of deep and ultra deep X-ray lithographic microstructures are described.

Far-Field High-Energy Diffraction Microscopy: A Non-Destructive Tool for Characterizing the Microstructure and Micromechanical State of Polycrystalline Materials

DOE PAGES

Park, Jun-Sang; Zhang, Xuan; Kenesei, Peter; ...

2017-08-31

A suite of non-destructive, three-dimensional X-ray microscopy techniques have recently been developed and used to characterize the microstructures of polycrystalline materials. These techniques utilize high-energy synchrotron radiation and include near-field and far-field diffraction microscopy (NF- and FF-HEDM, respectively) and absorption tomography. Several compatible sample environments have also been developed, enabling a wide range of 3D studies of material evolution. In this article, the FF-HEDM technique is described in detail, including its implementation at the 1-ID beamline of the Advanced Photon Source. Examples of how the information obtained from FF-HEDM can be used to deepen our understanding of structure-property-processing relationships inmore » selected materials are presented.« less

The Influence of Pulsed Electroplating Frequency and Duty Cycle on Copper Film Microstructure and Stress State

PubMed Central

Marro, James B.; Darroudi, Taghi; Okoro, Chukwudi A.; Obeng, Yaw S.; Richardson, Kathleen C.

2017-01-01

In this work we studied the impact of pulse electroplating parameters on the cross-sectional and surface microstructures of blanket copper films using electron backscattering diffraction and x-ray diffraction. The films evaluated were highly (111) textured in the direction perpendicular to the film surface. The degree of preferential orientation was found to decrease with longer pulse on-times, due to strain energy driven growth of other grain orientations. Residual biaxial stresses were also measured in the films and higher pulse frequencies during deposition led to smaller biaxial stresses in the films. Film stress was also found to correlate with the amount of twinning in the copper film cross-sections. This has been attributed to the twins’ thermal stability and mechanical properties. PMID:28239200

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 leveraged modulation of X-ray pulses using MEMS-based X-ray optics

DOEpatents

Lopez, Daniel; Shenoy, Gopal; Wang, Jin; Walko, Donald A.; Jung, Il-Woong; Mukhopadhyay, Deepkishore

2016-08-09

A method and apparatus are provided for implementing Bragg-diffraction leveraged modulation of X-ray pulses using MicroElectroMechanical systems (MEMS) based diffractive optics. An oscillating crystalline MEMS device generates a controllable time-window for diffraction of the incident X-ray radiation. The Bragg-diffraction leveraged modulation of X-ray pulses includes isolating a particular pulse, spatially separating individual pulses, and spreading a single pulse from an X-ray pulse-train.

Effect of heat input on microstructure, wear and friction behavior of (wt.-%) 50FeCrC-20FeW-30FeB coating on AISI 1020 produced by using PTA welding.

PubMed

Özel, Cihan; Gürgenç, Turan

2018-01-01

In this study, AISI 1020 steel surface was coated in different heat inputs with (wt.-%) 50FeCrC-20FeW-30FeB powder mixture by using plasma transferred arc (PTA) welding method. The microstructure of the coated samples were investigated by using optical microscope (OM), scanning electron microscope (SEM), X-ray diffraction (XRD) and energy dispersive X-ray (EDS). The hardness was measured with micro hardness test device. The dry sliding wear and friction coefficient properties were determined using a block-on-disk type wear test device. Wear tests were performed at 19.62 N, 39.24 N, 58.86 N load and the sliding distance of 900 m. The results were shown that different microstructures formed due to the heat input change. The highest average micro hardness value was measured at 1217 HV on sample coated with low heat input. It was determined that the wear resistance decreased with increasing heat input.

Hierarchical structured tungsten oxide nanocrystals via hydrothermal route: microstructure, formation mechanism and humidity sensing

NASA Astrophysics Data System (ADS)

Pang, Hua-Feng; Li, Zhi-Jie; Xiang, Xia; Fu, Yong-Qing; Placido, Frank; Zu, Xiao-Tao

2013-09-01

Hierarchical structured tungsten oxide nanocrystals were synthesized via the hydrothermal route assisted by a capping agent of ammonium benzoate (AB). The products were characterized using scanning electron microscopy, X-ray diffraction, X-ray photoelectron spectroscopy, and transmission electron microscopy. The experimental results show that the crystal microstructures could be changed from flower-shape to star-shape by changing the mole ratio of ammonium benzoate to sodium tungstate (AB/ST). The crystal phases were changed from orthorhombic WO3ṡ0.33H2O to hexagonal WO3 with the increase in the concentration of AB. Based on the results from Fourier transform infrared spectroscopy and time-dependent growth analysis, a self-assembly growth mechanism has been proposed for the formation of flower, spherical, and star-netted microstructures at different mole ratios of the AB/ST. The star-netted WO3 nanocrystals were applied as a sensitive layer for humidity sensing performed using a Love-mode ZnO/36∘ Y-cut LiTaO3 surface acoustic wave device, and a stable and sensitive response to the change of relative humidity was obtained.

Effect of heat input on microstructure, wear and friction behavior of (wt.-%) 50FeCrC-20FeW-30FeB coating on AISI 1020 produced by using PTA welding

PubMed Central

Gürgenç, Turan

2018-01-01

In this study, AISI 1020 steel surface was coated in different heat inputs with (wt.-%) 50FeCrC-20FeW-30FeB powder mixture by using plasma transferred arc (PTA) welding method. The microstructure of the coated samples were investigated by using optical microscope (OM), scanning electron microscope (SEM), X-ray diffraction (XRD) and energy dispersive X-ray (EDS). The hardness was measured with micro hardness test device. The dry sliding wear and friction coefficient properties were determined using a block-on-disk type wear test device. Wear tests were performed at 19.62 N, 39.24 N, 58.86 N load and the sliding distance of 900 m. The results were shown that different microstructures formed due to the heat input change. The highest average micro hardness value was measured at 1217 HV on sample coated with low heat input. It was determined that the wear resistance decreased with increasing heat input. PMID:29324875

Linking initial microstructure and local response during quasistatic granular compaction

DOE PAGES

Hurley, R. C.; Lind, J.; Pagan, D. C.; ...

2017-07-24

In this study, we performed experiments combining three-dimensional x-ray diffraction and x-ray computed tomography to explore the relationship between microstructure and local force and strain during quasistatic granular compaction. We found that initial void space around a grain and contact coordination number before compaction can be used to predict regions vulnerable to above-average local force and strain at later stages of compaction. We also found correlations between void space around a grain and coordination number, and between grain stress and maximum interparticle force, at all stages of compaction. Finally, we observed grains that fracture to have an above-average initial localmore » void space and a below-average initial coordination number. In conclusion, our findings provide (1) a detailed description of microstructure evolution during quasistatic granular compaction, (2) an approach for identifying regions vulnerable to large values of strain and interparticle force, and (3) methods for identifying regions of a material with large interparticle forces and coordination numbers from measurements of grain stress and local porosity.« less

Correlation of Thermally Induced Pores with Microstructural Features Using High Energy X-rays

NASA Astrophysics Data System (ADS)

Menasche, David B.; Shade, Paul A.; Lind, Jonathan; Li, Shiu Fai; Bernier, Joel V.; Kenesei, Peter; Schuren, Jay C.; Suter, Robert M.

2016-11-01

Combined application of a near-field High Energy Diffraction Microscopy measurement of crystal lattice orientation fields and a tomographic measurement of pore distributions in a sintered nickel-based superalloy sample allows pore locations to be correlated with microstructural features. Measurements were carried out at the Advanced Photon Source beamline 1-ID using an X-ray energy of 65 keV for each of the measurement modes. The nickel superalloy sample was prepared in such a way as to generate significant thermally induced porosity. A three-dimensionally resolved orientation map is directly overlaid with the tomographically determined pore map through a careful registration procedure. The data are shown to reliably reproduce the expected correlations between specific microstructural features (triple lines and quadruple nodes) and pore positions. With the statistics afforded by the 3D data set, we conclude that within statistical limits, pore formation does not depend on the relative orientations of the grains. The experimental procedures and analysis tools illustrated are being applied to a variety of materials problems in which local heterogeneities can affect materials properties.

Comparative study of structural and magnetic properties of nano-crystalline Li 0.5Fe 2.5O 4 prepared by various methods

NASA Astrophysics Data System (ADS)

Verma, Vivek; Pandey, Vibhav; Singh, Sukhveer; Aloysius, R. P.; Annapoorni, S.; Kotanala, R. K.

2009-08-01

Lithium ferrite has been considered as one of the highly strategic magnetic material. Nano-crystalline Li 0.5Fe 2.5O 4 was prepared by four different techniques and characterized by X-ray diffraction, vibrating sample magnetometer (VSM), transmission electron microscope (TEM) and Fourier transform infrareds (FTIR). The effect of annealing temperature (700, 900 and 1050 °C) on microstructure has been correlated to the magnetic properties. From X-ray diffraction patterns, it is confirmed that the pure phase of lithium ferrite began to form at 900 °C annealing. The particle size of as-prepared lithium ferrite was observed around 40, 31, 22 and 93 nm prepared by flash combustion, sol-gel, citrate precursor and standard ceramic technique, respectively. Lithium ferrite prepared by citrate precursor method shows a maximum saturation magnetization 67.6 emu/g at 5 KOe.

Study of Initial Stages of Ball-Milling of Cu Powder Using X-ray Diffraction

NASA Astrophysics Data System (ADS)

Gayathri, N.; Mukherjee, Paramita

2018-04-01

The initial stage of size refinement of Cu powder is studied using detailed X-ray diffraction (XRD) analysis to understand the mechanism of formation of nanomaterials during the ball-milling process. The study was restricted to samples obtained for milling time up to 240 min to understand the deformation mechanism at the early stages of ball milling. Various model based approaches for the analysis of the XRD were used to study the evolution of the microstructural parameters such as domain size and microstrain along the different crystallographic planes. It was seen that the domain size saturates at a low value along the (311) plane whereas the size along the (220) and (200) plane is still higher. The r.m.s microstrain showed a non-monotonic change along the different crystallographic directions up to the milling time of 240 min.

Properties of micro-arc oxidation coatings on aluminum alloy at different negative peak current densities

NASA Astrophysics Data System (ADS)

Gu, Xin; Jiang, Bailing; Li, Hongtao; Liu, Cancan; Shao, Lianlian

2018-05-01

Micro-arc oxidation coatings were fabricated on 6061 aluminum alloy using whereby bipolar pulse mode in the case of different negative peak current densities. The phase composition, microstructures and wear properties were studied using x-ray diffraction, scanning electron microscopy and ball-on-disk wear tester, respectively. As results indicate, by virtue of negative peak current density, the oxygen can be expelled by produced hydrogen on anode in the case of negative pulse width and via the opened discharge channel. The results of x-ray diffraction, surface and cross-sectional morphology indicated that the coating was structured compactly taking on less small-diameter micro-pores and defects with negative peak current density of 75 A dm‑2. Additionally, as the results of wear tracks and weight loss bespeak, by virtue of appropriate negative peak current density, coatings resisted the abrasive wear and showed excellent wear resistance.

Microstructural changes in CdSe-coated ZnO nanowires evaluated by in situ annealing in transmission electron microscopy and x-ray diffraction

NASA Astrophysics Data System (ADS)

Majidi, Hasti; Winkler, Christopher R.; Taheri, Mitra L.; Baxter, Jason B.

2012-07-01

We report on the crystallite growth and phase change of electrodeposited CdSe coatings on ZnO nanowires during annealing. Both in situ transmission electron microscopy (TEM) and x-ray diffraction (XRD) reveal that the nanocrystal size increases from ˜3 to ˜10 nm upon annealing at 350 °C for 1 h and then to more than 30 nm during another 1 h at 400 °C, exhibiting two distinct growth regimes. Nanocrystal growth occurs together with a structural change from zinc blende to wurtzite. The structural transition begins at 350 °C, which results in the formation of stacking faults. Increased crystallite size, comparable to the coating thickness, can improve charge separation in extremely thin absorber solar cells. We demonstrate a nearly two-fold improvement in power conversion efficiency upon annealing.

Structural and magnetic properties of nanocrystalline NiFe2O4 thin film prepared by spray pyrolysis technique

NASA Astrophysics Data System (ADS)

Chavan, Apparao R.; Chilwar, R. R.; Shisode, M. V.; Hivrekar, Mahesh M.; Mande, V. K.; Jadhav, K. M.

2018-05-01

The nanocrystalline NiFe2O4 thin film has been prepared using a spray pyrolysis technique on glass substrate. The prepared thin film was characterized by using X-ray diffraction (XRD), Fourier transform Infrared spectroscopy (FTIR), and Field Emission-Scanning Electron Microscopy (FE-SEM) characterization techniques for the structural and microstructural analysis. The magnetic property was measured using vibrating sample magnetometer (VSM) at room temperature. X-ray diffraction studies show the formation of single phase spinel structure of the thin film. The octahedral and tetrahedral vibration in the sample was studied by Fourier transform infrared (FT-IR) spectra. Magnetic hysteresis loop was recorded for thin film at room temperature. At 15 kOe, saturation magnetization (Ms) was found to increase while coercivity (Hc) decreases with thickness of the NiFe2O4 thin film.

Fabrication, characterization and fracture study of a machinable hydroxyapatite ceramic.

PubMed

Shareef, M Y; Messer, P F; van Noort, R

1993-01-01

In this study the preparation of a machinable hydroxyapatite from mixtures of a fine, submicrometer powder and either a coarse powder composed of porous aggregates up to 50 microns or a medium powder composed of dense particles of 3 microns median size is described. These were characterized using X-ray diffraction, transmission and scanning electron microscopy and infra-red spectroscopy. Test-pieces were formed by powder pressing and slip casting mixtures of various combinations of the fine, medium and coarse powders. The fired test-pieces were subjected to measurements of firing shrinkage, porosity, bulk density, tensile strength and fracture toughness. The microstructure and composition were examined using scanning electron microscopy and X-ray diffraction. For both processing methods, a uniform interconnected microporous structure was produced of a high-purity hydroxyapatite. The maximum tensile strength and fracture toughness that could be attained while retaining machinability were 37 MPa and 0.8 MPa m1/2 respectively.

The Microstructure and Physical Properties of Incinerated Paper-Cullet-Clay Ceramics

NASA Astrophysics Data System (ADS)

Sahar, M. R.; Hamzah, K.; Rohani, M. S.; Samah, K. A.; Razi, M. M.

A series of ceramic based on (x) incinerated recycle paper - (80-x) cullet - 20 Kaolin clay (where 10×45 wt%) has successfully been made by slip casting technique followed by sintering at 1000 °C. The actual composition of ceramic is analyzed using Energy Dispersive of X-Ray (EDAX) while the phase existence is determined using X-Ray Diffraction (XRD) technique. Their microstructural morphology is observed under Scanning Electron Microscope (SEM) and the physical properties are measured in term of their thermal shrinkage and hardness. It is found that the ceramic contain mostly of Silica and the phase is dominated by the existence of Quartz (SiO2), Wollastonite (CaSiO3) and Anorthite (Ca(Al2SiO8)). The SEM micrograph shows that the morphology is dominated by the existence of granular structure, and then become smoother as the cullet level is further increased. It is also found out that the thermal shrinkage is in the range 18% - 6.5% while the hardness is in the range of 152MPa- 1.463 GPa depending on composition.

Plutonium-uranium mixed oxide characterization by coupling micro-X-ray diffraction and absorption investigations

NASA Astrophysics Data System (ADS)

Degueldre, C.; Martin, M.; Kuri, G.; Grolimund, D.; Borca, C.

2011-09-01

Plutonium-uranium mixed oxide (MOX) fuels are currently used in nuclear reactors. The potential differences of metal redox state and microstructural developments of the matrix before and after irradiation are commonly analysed by electron probe microanalysis. In this work the structure and next-neighbor atomic environments of Pu and U oxide features within unirradiated homogeneous MOX and irradiated (60 MW d kg -1) MOX samples was analysed by micro-X-ray fluorescence (μ-XRF), micro-X-ray diffraction (μ-XRD) and micro-X-ray absorption fine structure (μ-XAFS) spectroscopy. The grain properties, chemical bonding, valences and stoichiometry of Pu and U are determined from the experimental data gained for the unirradiated as well as for irradiated fuel material examined in the center of the fuel as well as in its peripheral zone (rim). The formation of sub-grains is observed as well as their development from the center to the rim (polygonization). In the irradiated sample Pu remains tetravalent (>95%) and no (<5%) Pu(V) or Pu(VI) can be detected while the fuel could undergo slight oxidation in the rim zone. Any slight potential plutonium oxidation is buffered by the uranium dioxide matrix while locally fuel cladding interaction could also affect the redox of the fuel.

Study of the specific features of single-crystal boron microstructure

NASA Astrophysics Data System (ADS)

Blagov, A. E.; Vasil'ev, A. L.; Dmitriev, V. P.; Ivanova, A. G.; Kulikov, A. G.; Marchenkov, N. V.; Popov, P. A.; Presnyakov, M. Yu.; Prosekov, P. A.; Pisarevskii, Yu. V.; Targonskii, A. V.; Chernaya, T. S.; Chernyshov, D. Yu.

2017-09-01

A complex study of the structure of β-boron single crystal grown by the floating-zone method, with sizes significantly exceeding the analogs known in the literature, has been performed. The study includes X-ray diffraction analysis and X-ray diffractometry (measurement of pole figures and rocking curves), performed on both laboratory and synchrotron sources; atomic-resolution scanning transmission electron microscopy with spherical aberration correction; and energy-dispersive microanalysis. X-ray diffraction analysis using synchrotron radiation has been used to refine the β-boron structure and find impurity Si atoms. The relative variations in the unit-cell parameters a and c for the crystal bulk are found to be δ a/ a ≈ 0.4 and δ c/ c ≈ 0.1%. X-ray diffractometry has revealed that the single-crystal growth axis coincides with the [2\\bar 2013] crystallographic axis and makes an angle of 21.12° with the [0001] threefold axis. Electron microscopy data have confirmed that the sample under study is a β-boron crystal, which may contain 0.3-0.4 at % Si as an impurity. Planar defects (stacking faults and dislocations) are found. The results of additional measurements of the temperature dependence of the thermal conductivity of the crystal in the range of 50-300 K are indicative of its high structural quality.

Non-destructive mapping of grain orientations in 3D by laboratory X-ray microscopy

PubMed Central

McDonald, S. A.; Reischig, P.; Holzner, C.; Lauridsen, E. M.; Withers, P. J.; Merkle, A. P.; Feser, M.

2015-01-01

The ability to characterise crystallographic microstructure, non-destructively and in three-dimensions, is a powerful tool for understanding many aspects related to damage and deformation mechanisms in polycrystalline materials. To this end, the technique of X-ray diffraction contrast tomography (DCT) using monochromatic synchrotron and polychromatic laboratory X-ray sources has been shown to be capable of mapping crystal grains and their orientations non-destructively in 3D. Here we describe a novel laboratory-based X-ray DCT modality (LabDCT), enabling the wider accessibility of the DCT technique for routine use and in-depth studies of, for example, temporal changes in crystallographic grain structure non-destructively over time through ‘4D’ in situ time-lapse studies. The capability of the technique is demonstrated by studying a titanium alloy (Ti-β21S) sample. In the current implementation the smallest grains that can be reliably detected are around 40 μm. The individual grain locations and orientations are reconstructed using the LabDCT method and the results are validated against independent measurements from phase contrast tomography and electron backscatter diffraction respectively. Application of the technique promises to provide important insights related to the roles of recrystallization and grain growth on materials properties as well as supporting 3D polycrystalline modelling of materials performance. PMID:26494523

Non-destructive mapping of grain orientations in 3D by laboratory X-ray microscopy

NASA Astrophysics Data System (ADS)

McDonald, S. A.; Reischig, P.; Holzner, C.; Lauridsen, E. M.; Withers, P. J.; Merkle, A. P.; Feser, M.

2015-10-01

The ability to characterise crystallographic microstructure, non-destructively and in three-dimensions, is a powerful tool for understanding many aspects related to damage and deformation mechanisms in polycrystalline materials. To this end, the technique of X-ray diffraction contrast tomography (DCT) using monochromatic synchrotron and polychromatic laboratory X-ray sources has been shown to be capable of mapping crystal grains and their orientations non-destructively in 3D. Here we describe a novel laboratory-based X-ray DCT modality (LabDCT), enabling the wider accessibility of the DCT technique for routine use and in-depth studies of, for example, temporal changes in crystallographic grain structure non-destructively over time through ‘4D’ in situ time-lapse studies. The capability of the technique is demonstrated by studying a titanium alloy (Ti-β21S) sample. In the current implementation the smallest grains that can be reliably detected are around 40 μm. The individual grain locations and orientations are reconstructed using the LabDCT method and the results are validated against independent measurements from phase contrast tomography and electron backscatter diffraction respectively. Application of the technique promises to provide important insights related to the roles of recrystallization and grain growth on materials properties as well as supporting 3D polycrystalline modelling of materials performance.

Non-destructive mapping of grain orientations in 3D by laboratory X-ray microscopy.

PubMed

McDonald, S A; Reischig, P; Holzner, C; Lauridsen, E M; Withers, P J; Merkle, A P; Feser, M

2015-10-23

The ability to characterise crystallographic microstructure, non-destructively and in three-dimensions, is a powerful tool for understanding many aspects related to damage and deformation mechanisms in polycrystalline materials. To this end, the technique of X-ray diffraction contrast tomography (DCT) using monochromatic synchrotron and polychromatic laboratory X-ray sources has been shown to be capable of mapping crystal grains and their orientations non-destructively in 3D. Here we describe a novel laboratory-based X-ray DCT modality (LabDCT), enabling the wider accessibility of the DCT technique for routine use and in-depth studies of, for example, temporal changes in crystallographic grain structure non-destructively over time through '4D' in situ time-lapse studies. The capability of the technique is demonstrated by studying a titanium alloy (Ti-β21S) sample. In the current implementation the smallest grains that can be reliably detected are around 40 μm. The individual grain locations and orientations are reconstructed using the LabDCT method and the results are validated against independent measurements from phase contrast tomography and electron backscatter diffraction respectively. Application of the technique promises to provide important insights related to the roles of recrystallization and grain growth on materials properties as well as supporting 3D polycrystalline modelling of materials performance.

Synthesis and characterization of lanthanum doped zinc oxide nanoparticles

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

Kumar, Vinod; Sonia,; Suman,

La doped ZnO (Zn{sub 1-x}La{sub x}O, x = 0, 3, 6 and 9) were prepared via chemical co-precipitation method using Zinc Acetate, Lanthanum Acetate and Sodium Hydroxide at 50°C. Hydrate nanoparticles were annealed in air at 300°C for 3 hours. The synthesized samples have been characterized by powder X-ray diffraction and UV–Visible spectrophotometer. The XRD measurement revealsthat the prepared nanoparticles have different microstructure without changing a hexagonal wurtzite structure. The result shows the change in nanoparticles size with the increment of lanthanum concentration for lower concentration for x = 0 to 6 and decreases at x = 9.

Supplementary Microstructural Features Induced During Laser Surface Melting of Thermally Sprayed Inconel 625 Coatings

NASA Astrophysics Data System (ADS)

Ahmed, Nauman; Voisey, K. T.; McCartney, D. G.

2014-02-01

Laser surface melting of thermally sprayed coatings has the potential to enhance their corrosion properties by incorporating favorable microstructural changes. Besides homogenizing the as-sprayed structure, laser melting may induce certain microstructural modifications (i.e., supplementary features) in addition to those that directly improve the corrosion performance. Such features, being a direct result of the laser treatment process, are described in this paper which is part of a broader study in which high velocity oxy-fuel sprayed Inconel 625 coatings on mild-steel substrates were treated with a diode laser and the modified microstructure characterized using optical and scanning electron microscopy and x-ray diffraction. The laser treated coating features several different zones, including a region with a microstructure in which there is a continuous columnar dendritic structure through a network of retained oxide stringers.

Observation of martensitic transformation in Ni50Mn41Cu4Sn5 Heusler alloy prepared by mechanical alloying

NASA Astrophysics Data System (ADS)

Saini, Dinesh; Singh, Satyavir; Banerjee, M. K.; Sachdev, K.

2017-05-01

Mechanical alloying route has been employed for preparation of a single phase Ni50Mn41Cu4Sn5 (atomic %) Heusler alloy. Use of high energy planetary ball mill enables successful preparation of the same as authenticated by detailed X-ray diffraction (XRD) study. Microstructural study is carried out by optical and scanning electron microscopic techniques. XRD results reveal that increasing milling time leads to reduction in crystallite size and concurrent increase in lattice strain. Microstructural results indicate formation of self-assembled martensite twins.

Study of Carbide Evolution During Thermo-Mechanical Processing of AISI D2 Tool Steel

NASA Astrophysics Data System (ADS)

Bombac, D.; Fazarinc, M.; Podder, A. Saha; Kugler, G.

2013-03-01

The microstructure of a cold-worked tool steel (AISI D2) with various thermo-mechanical treatments was examined in the current study to identify the effects of these treatments on phases. X-ray diffraction was used to identify phases. Microstructural changes such as spheroidization and coarsening of carbides were studied. Thermodynamic calculations were used to verify the results of the differential thermal analysis. It was found that soaking temperature and time have a large influence on dissolution, precipitation, spheroidization, and coalescence of carbides present in the steel. This consequently influences the hot workability and final properties.

Microstructural characterization of dental zinc phosphate cements using combined small angle neutron scattering and microfocus X-ray computed tomography.

PubMed

Viani, Alberto; Sotiriadis, Konstantinos; Kumpová, Ivana; Mancini, Lucia; Appavou, Marie-Sousai

2017-04-01

To characterize the microstructure of two zinc phosphate cement formulations in order to investigate the role of liquid/solid ratio and composition of powder component, on the developed porosity and, consequently, on compressive strength. X-ray powder diffraction with the Rietveld method was used to study the phase composition of zinc oxide powder and cements. Powder component and cement microstructure were investigated with scanning electron microscopy. Small angle neutron scattering (SANS) and microfocus X-ray computed tomography (XmCT) were together employed to characterize porosity and microstructure of dental cements. Compressive strength tests were performed to evaluate their mechanical performance. The beneficial effects obtained by the addition of Al, Mg and B to modulate powder reactivity were mitigated by the crystallization of a Zn aluminate phase not involved in the cement setting reaction. Both cements showed spherical pores with a bimodal distribution at the micro/nano-scale. Pores, containing a low density gel-like phase, developed through segregation of liquid during setting. Increasing liquid/solid ratio from 0.378 to 0.571, increased both SANS and XmCT-derived specific surface area (by 56% and 22%, respectively), porosity (XmCT-derived porosity increased from 3.8% to 5.2%), the relative fraction of large pores ≥50μm, decreased compressive strength from 50±3MPa to 39±3MPa, and favored microstructural and compositional inhomogeneities. Explain aspects of powder design affecting the setting reaction and, in turn, cement performance, to help in optimizing cement formulation. The mechanism behind development of porosity and specific surface area explains mechanical performance, and processes such as erosion and fluoride release/uptake. Copyright © 2017 The Authors. Published by Elsevier Ltd.. All rights reserved.

An x-ray diffraction study of microstructural deformation induced by cyclic loading of selected steels

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

Fourspring, P.M.; Pangborn, R.N.

1997-12-31

X-ray double crystal diffractometry (XRDCD) was used to assess cyclic microstructural deformation in a face centered cubic (fcc) steel (AISI304) and a body centered cubic (bcc) steel (SA508 class 2). The objectives of the investigation were to determine if XRDCD could be used effectively to monitor cyclic microstructural deformation in polycrystalline Fe alloys and to study the distribution of the microstructural deformation induced by cyclic loading in these alloys. The approach used in the investigation was to induce fatigue damage in a material and to characterize the resulting microstructural deformation at discrete fractions of the fatigue life of the material.more » Also, characterization of microstructural deformation was carried out to identify differences in the accumulation of damage from the surface to the bulk, focusing on the following three regions: near surface (0--10 {micro}m), subsurface (10--300 {micro}m), and bulk. Characterization of the subsurface region was performed only on the AISI304 material because of the limited availability of the SA508 material. The results from the XRDCD data indicate a measurable change induced by fatigue from the initial state to subsequent states of both the AISI304 and the SA508 materials. Therefore, the XRDCD technique was shown to be sensitive to the microstructural deformation caused by fatigue in steels; thus, the technique can be used to monitor fatigue damage in steels.« less

Effect of Bainitic Microstructure on Ballistic Performance of Armour Steel Weld Metal Using Developed High Ni-Coated Electrode

NASA Astrophysics Data System (ADS)

Pramanick, A. K.; Das, H.; Reddy, G. M.; Ghosh, M.; Nandy, S.; Pal, T. K.

2018-05-01

Welding of armour steel has gained significant importance during the past few years as recent civilian and military requirements demand weld metal properties matching with base metal having good ballistic performance along with high strength and toughness at - 40 °C as per specification. The challenge of armour steel welding therefore lies in controlling the weld metal composition which is strongly dependent on welding electrode/consumables, resulting in desired weld microstructure consisting of lower bainite along with retained austenite. The performance of butt-welded armour steel joints produced by the developed electrodes was evaluated using tensile testing, ballistic testing, impact toughness at room temperature and subzero temperature. Microstructures of weld metals are exclusively characterized by x-ray diffraction technique, scanning electron microscope and transmission electron microscopy with selected area diffraction pattern. Experimental results show that weld metal with relatively lower carbon, higher manganese and lower nickel content was attributed to lower bainite with film type of retained austenite may be considered as a most covetable microstructure for armour steel weld metal.

Effect of Bainitic Microstructure on Ballistic Performance of Armour Steel Weld Metal Using Developed High Ni-Coated Electrode

NASA Astrophysics Data System (ADS)

Pramanick, A. K.; Das, H.; Reddy, G. M.; Ghosh, M.; Nandy, S.; Pal, T. K.

2018-04-01

Welding of armour steel has gained significant importance during the past few years as recent civilian and military requirements demand weld metal properties matching with base metal having good ballistic performance along with high strength and toughness at - 40 °C as per specification. The challenge of armour steel welding therefore lies in controlling the weld metal composition which is strongly dependent on welding electrode/consumables, resulting in desired weld microstructure consisting of lower bainite along with retained austenite. The performance of butt-welded armour steel joints produced by the developed electrodes was evaluated using tensile testing, ballistic testing, impact toughness at room temperature and subzero temperature. Microstructures of weld metals are exclusively characterized by x-ray diffraction technique, scanning electron microscope and transmission electron microscopy with selected area diffraction pattern. Experimental results show that weld metal with relatively lower carbon, higher manganese and lower nickel content was attributed to lower bainite with film type of retained austenite may be considered as a most covetable microstructure for armour steel weld metal.

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

In situ X-ray diffraction measurement of shock-wave-driven twinning and lattice dynamics

NASA Astrophysics Data System (ADS)

Wehrenberg, C. E.; McGonegle, D.; Bolme, C.; Higginbotham, A.; Lazicki, A.; Lee, H. J.; Nagler, B.; Park, H.-S.; Remington, B. A.; Rudd, R. E.; Sliwa, M.; Suggit, M.; Swift, D.; Tavella, F.; Zepeda-Ruiz, L.; Wark, J. S.

2017-10-01

Pressure-driven shock waves in solid materials can cause extreme damage and deformation. Understanding this deformation and the associated defects that are created in the material is crucial in the study of a wide range of phenomena, including planetary formation and asteroid impact sites, the formation of interstellar dust clouds, ballistic penetrators, spacecraft shielding and ductility in high-performance ceramics. At the lattice level, the basic mechanisms of plastic deformation are twinning (whereby crystallites with a mirror-image lattice form) and slip (whereby lattice dislocations are generated and move), but determining which of these mechanisms is active during deformation is challenging. Experiments that characterized lattice defects have typically examined the microstructure of samples after deformation, and so are complicated by post-shock annealing and reverberations. In addition, measurements have been limited to relatively modest pressures (less than 100 gigapascals). In situ X-ray diffraction experiments can provide insights into the dynamic behaviour of materials, but have only recently been applied to plasticity during shock compression and have yet to provide detailed insight into competing deformation mechanisms. Here we present X-ray diffraction experiments with femtosecond resolution that capture in situ, lattice-level information on the microstructural processes that drive shock-wave-driven deformation. To demonstrate this method we shock-compress the body-centred-cubic material tantalum—an important material for high-energy-density physics owing to its high shock impedance and high X-ray opacity. Tantalum is also a material for which previous shock compression simulations and experiments have provided conflicting information about the dominant deformation mechanism. Our experiments reveal twinning and related lattice rotation occurring on the timescale of tens of picoseconds. In addition, despite the common association between twinning and strong shocks, we find a transition from twinning to dislocation-slip-dominated plasticity at high pressure (more than 150 gigapascals), a regime that recovery experiments cannot accurately access. The techniques demonstrated here will be useful for studying shock waves and other high-strain-rate phenomena, as well as a broad range of processes induced by plasticity.

In situ X-ray diffraction measurement of shock-wave-driven twinning and lattice dynamics

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

Wehrenberg, C. E.; McGonegle, D.; Bolme, C.

We report that pressure-driven shock waves in solid materials can cause extreme damage and deformation. Understanding this deformation and the associated defects that are created in the material is crucial in the study of a wide range of phenomena, including planetary formation and asteroid impact sites, the formation of interstellar dust clouds, ballistic penetrators, spacecraft shielding and ductility in high-performance ceramics. At the lattice level, the basic mechanisms of plastic deformation are twinning (whereby crystallites with a mirror-image lattice form) and slip (whereby lattice dislocations are generated and move), but determining which of these mechanisms is active during deformation ismore » challenging. Experiments that characterized lattice defects have typically examined the microstructure of samples after deformation, and so are complicated by post-shock annealing and reverberations. In addition, measurements have been limited to relatively modest pressures (less than 100 gigapascals). In situ X-ray diffraction experiments can provide insights into the dynamic behaviour of materials, but have only recently been applied to plasticity during shock compression and have yet to provide detailed insight into competing deformation mechanisms. Here we present X-ray diffraction experiments with femtosecond resolution that capture in situ, lattice-level information on the microstructural processes that drive shock-wave-driven deformation. To demonstrate this method we shock-compress the body-centred-cubic material tantalum—an important material for high-energy-density physics owing to its high shock impedance and high X-ray opacity. Tantalum is also a material for which previous shock compression simulations and experiments have provided conflicting information about the dominant deformation mechanism. Our experiments reveal twinning and related lattice rotation occurring on the timescale of tens of picoseconds. In addition, despite the common association between twinning and strong shocks, we find a transition from twinning to dislocation-slip-dominated plasticity at high pressure (more than 150 gigapascals), a regime that recovery experiments cannot accurately access. Lastly, the techniques demonstrated here will be useful for studying shock waves and other high-strain-rate phenomena, as well as a broad range of processes induced by plasticity.« less

In situ X-ray diffraction measurement of shock-wave-driven twinning and lattice dynamics

DOE PAGES

Wehrenberg, C. E.; McGonegle, D.; Bolme, C.; ...

2017-10-25

We report that pressure-driven shock waves in solid materials can cause extreme damage and deformation. Understanding this deformation and the associated defects that are created in the material is crucial in the study of a wide range of phenomena, including planetary formation and asteroid impact sites, the formation of interstellar dust clouds, ballistic penetrators, spacecraft shielding and ductility in high-performance ceramics. At the lattice level, the basic mechanisms of plastic deformation are twinning (whereby crystallites with a mirror-image lattice form) and slip (whereby lattice dislocations are generated and move), but determining which of these mechanisms is active during deformation ismore » challenging. Experiments that characterized lattice defects have typically examined the microstructure of samples after deformation, and so are complicated by post-shock annealing and reverberations. In addition, measurements have been limited to relatively modest pressures (less than 100 gigapascals). In situ X-ray diffraction experiments can provide insights into the dynamic behaviour of materials, but have only recently been applied to plasticity during shock compression and have yet to provide detailed insight into competing deformation mechanisms. Here we present X-ray diffraction experiments with femtosecond resolution that capture in situ, lattice-level information on the microstructural processes that drive shock-wave-driven deformation. To demonstrate this method we shock-compress the body-centred-cubic material tantalum—an important material for high-energy-density physics owing to its high shock impedance and high X-ray opacity. Tantalum is also a material for which previous shock compression simulations and experiments have provided conflicting information about the dominant deformation mechanism. Our experiments reveal twinning and related lattice rotation occurring on the timescale of tens of picoseconds. In addition, despite the common association between twinning and strong shocks, we find a transition from twinning to dislocation-slip-dominated plasticity at high pressure (more than 150 gigapascals), a regime that recovery experiments cannot accurately access. Lastly, the techniques demonstrated here will be useful for studying shock waves and other high-strain-rate phenomena, as well as a broad range of processes induced by plasticity.« less

[Study on high strength mica-based machinable glass-ceramic].

PubMed

Li, Hong; Ran, Junguo; Gou, Li; Wang, Fanghu

2004-02-01

The phase constitution, microstructure and properties of a new type of machinable glass-ceramics containing fluorophlogopite-type (FPT) Ca-mica for used in restorative dentistry were investigated. According to the results of X-ray diffraction (XRD) and energy-dispersive spectrometry(EDS), its main crystalline phases were FPT Ca-mica and t-ZrO2, together with few KxCa(1-x)/2Mg2Si4O10F2, m-ZrO2. The flexible strength was 235 MPa, which was nearly two times larger than that of the present mica-based dental materials, and the highest fracture toughness was 2.17 MPa.m1/2. The microstructure had a great effect on properties, the glass-ceramics contained a large volume, and the fine crystals showed higher strength. The material possessed typical microstructure of machinable glass-ceramics and displayed excellent machinability during drilling test and CAD/CAM.

Effect of Cooling Rates on γ → α Transformation and Metastable States in Fe-Cu Alloys with Addition of Ni

NASA Astrophysics Data System (ADS)

Crozet, C.; Verdier, M.; Lay, S.; Antoni-Zdziobek, A.

2018-07-01

α/γ phase transformations occurring in Fe-10Cu-xNi alloys (0 ≤ x ≤ 15 in mass%) were studied using X-ray diffraction, scanning electron microscopy, electron back scattered diffraction, transmission electron microscopy and chemical analysis, combining X-ray microanalysis with energy dispersive spectrometry in the scanning electron microscope and electron microprobe analysis with wavelength dispersive spectrometry. The influence of cooling rate on the microstructure was investigated using ice-brine quenching and 2 °C/min slow cooling rate performed with dilatometry. Ni addition induces metastable transformations on cooling: massive and bainitic ferrite are formed depending on the alloy composition and cooling rate. Moreover, most of the Cu phase precipitates on cooling giving rise to a fine distribution of Cu particles in the ferrite grains. For both cooling conditions, the hardness increases with increasing Ni content and a higher hardness is obtained in the quenched alloy for each composition. The change in hardness is correlated to the effect of Ni solid solution, transformation structure and size of Cu particles.

Microstructural Characteristic of the Al-Fe-Cu Alloy During High-Speed Repetitive Continuous Extrusion Forming

NASA Astrophysics Data System (ADS)

Hu, Jiamin; Teng, Jie; Ji, Xiankun; Kong, Xiangxin; Jiang, Fulin; Zhang, Hui

2016-11-01

High-speed repetitive continuous extrusion forming process (R-Conform process) was performed on the Al-Fe-Cu alloy. The microstructural evolution and mechanical properties were studied by x-ray diffraction, electron backscatter diffraction, transmission electron microscopy and tensile testing. The results show that a significant improvement of tensile ductility concurs with a considerable loss of tensile strength before four passes, after that the process on mechanical properties variation tends to be steady, indicating an accelerated mechanical softening occurs when comparing to low-speed R-Conform process. Microstructure characterization indicates that the accumulated strain promotes the transformation of low angle boundaries to high angle boundaries, thus leading to the acceleration of continuous dynamic recrystallization process, and the precipitates are broken, spheroidized and homogeneously distribute in Al matrix as increasing R-Conform passes. Massive microshear bands are observed after initial passes of R-Conform process, which may promote continuous dynamic recrystallization and further grain refinement during high-speed R-Conform process.

Effect of Different Thermomechanical Processes on the Microstructure, Texture, and Mechanical Properties of API 5L X70 Steel

NASA Astrophysics Data System (ADS)

Masoumi, Mohammad; Echeverri, Edwan Anderson Ariza; Silva, Cleiton Carvalho; Béreš, Miloslav; de Abreu, Hamilton Ferreira Gomes

2018-03-01

A commercial API 5L X70 steel plate was subjected to different thermomechanical processes to propose a novel thermomechanical rolling path to achieve improved mechanical properties. Scanning electron microscopy, electron backscatter diffraction, and x-ray texture analysis were employed for microstructural characterization. The results showed that strain-free recrystallized {001} ferrite grains that developed at higher rolling temperature could not meet the American Petroleum Institute (API) requirements. Also, refined and work-hardened grains that have formed in the intercritical region with high stored energy do not provide suitable tensile properties. However, fine martensite-austenite constituents dispersed in ferrite matrix with grains having predominantly {111} and {110} orientations parallel to the normal direction that developed under isothermal rolling at 850 °C provided an outstanding combination of tensile strength and ductility.

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.

Measuring twinning and slip in shock-compressed Ta from in-situ x-ray diffraction

NASA Astrophysics Data System (ADS)

Wehrenberg, Christopher; McGonegle, David; Sliwa, Marcin; Suggit, Matt; Wark, Justin; Lee, Hae Ja; Nagler, Bob; Tavella, Franz; Remington, Bruce; Rudd, Rob; Lazicki, Amy; Park, Hye-Sook; Swift, Damian; Zepeda-Ruiz, Louis; Higginbotham, Andrew; Bolme, Cindy

2017-06-01

A fundamental understanding of high-pressure and high-strain-rate deformation rests on grasping the underlying microstructural processes, such as twinning and dislocation generation and transport (slip), yet simulations and ex-post-facto recovery experiments provide conflicting answers to these basic issues. Here, we report direct, in-situ observation of twinning and slip in shock compressed Ta using in-situ x-ray diffraction. A series of shock experiments were performed on the Matter in Extreme Conditions end station at LCLS. Direct laser ablation was used to drive a shock, ranging in pressure from 10-300 GPa, into a Ta sample with an initial (110) fiber texture. The subsequent changes in texture were observed in-situ by examining the azimuthal distribution of the diffraction intensity and found to match twinning and lattice rotation. Measurements of the twin fraction and lattice rotation were used to calculate the equivalent plastic strain from twinning and slip. This work was performed under the auspices of the U.S. Department of Energy by Lawrence Livermore National Laboratory under Contract No. DE-AC52-07NA27344.

Microstructural investigation of nickel silicide thin films and the silicide-silicon interface using transmission electron microscopy.

PubMed

Bhaskaran, M; Sriram, S; Mitchell, D R G; Short, K T; Holland, A S; Mitchell, A

2009-01-01

This article discusses the results of transmission electron microscopy (TEM)-based investigation of nickel silicide (NiSi) thin films grown on silicon. Nickel silicide is currently used as the CMOS technology standard for local interconnects and in electrical contacts. Films were characterized with a range of TEM-based techniques along with glancing angle X-ray diffraction. The nickel silicide thin films were formed by vacuum annealing thin films of nickel (50 nm) deposited on (100) silicon. The cross-sectional samples indicated a final silicide thickness of about 110 nm. This investigation studied and reports on three aspects of the thermally formed thin films: the uniformity in composition of the film using jump ratio maps; the nature of the interface using high resolution imaging; and the crystalline orientation of the thin films using selected-area electron diffraction (SAED). The analysis highlighted uniform composition in the thin films, which was also substantiated by spectroscopy techniques; an interface exhibiting the desired abrupt transition from silicide to silicon; and desired and preferential crystalline orientation corresponding to stoichiometric NiSi, supported by glancing angle X-ray diffraction results.

Nanoscale contact resistance of V2O5 xerogel films developed by nanostructured powder

NASA Astrophysics Data System (ADS)

Bera, Biswajit; Sekhar Das, Pradip; Bhattacharya, Manjima; Ghosh, Swapankumar; Mukhopadhyay, Anoop Kumar; Dey, Arjun

2016-03-01

Here we report the synthesis of V2O5 nanostructures by a fast, simple, cost-effective, low-temperature chemical process; followed by the deposition of V2O5 xerogel thin films on a glass substrate by a sol-gel route. Phase analysis, phase transition, microstructural and electronic characterization studies are carried out by x-ray diffraction, texture coefficient analysis, field emission scanning electron microscopy, transmission electron microscopy (TEM), related selected area electron diffraction pattern (SAED) analysis, Fourier transform infrared spectroscopy, thermogravimetry and differential thermal analysis, differential scanning calorimetry, and x-ray photoelectron spectroscopy techniques. Confirmatory TEM and SAED data analysis prove further that in this polycrystalline powder there is a unique localized existence of purely single crystalline V2O5 powder with a preferred orientation in the (0 1 0) direction. The most interesting result obtained in the present work is that the xerogel thin films exhibit an inherent capability to enhance the intrinsic resistance against contact induced deformations as more external load is applied during the nanoindentation experiments. In addition, both the nanohardness and Young’s modulus of the films are found to be insensitive to load variations (e.g. 1 to 7 mN). These results are explained in terms of microstructural parameters, e.g. porosity and structural configuration.

The effects of ageing time on the microstructure and properties of mesoporous silica-hydroxyapatite nanocomposite

NASA Astrophysics Data System (ADS)

Yousefpour, Mardali; Taherian, Zahra

2013-02-01

In this study, a mesoporous silica-hydroxyapatite nanocomposite (MCM-41/HA) was synthesized via sol-gel technique as a drug delivery system. The synthesis of MCM-41/hydroxyapatite nanocomposite was carried out at room temperature. The effect of various ageing time on the nanocomposite properties was studied during synthesis process. 0, 24, 36, and 48 h aging times were chosen. Textural properties and microstructure of the nanocomposites were characterized by X-ray diffraction (XRD), Transmission Electron Microscopy (TEM), Energy Dispersive X-ray Spectroscopy (EDS), Electron Diffraction pattern (ED), and N2 adsorption-desorption. Results showed that ageing process led to HA crystals nucleation and growth on the surface of mesoporous silica. At 48 h of aging time, the surface area and total pore volume increased from 36.2 to 334 m2/g and 0.14-0.7 cm3/g, respectively. In contrast, the average pore diameter considerably decreased from 20.1 nm for (MCM-41/HA)24 to 8.39 nm for (MCM-41/HA)48. Furthermore, it was observed more homogeneous pore distribution with increasing the ageing time. In conclusion, the ageing time play an important role on textural properties of MCM-41/HA nanocomposite which could have a major effect on drug delivery properties such as molecular loading and release kinetics.

Behavior of Quartz and Carbon Black Pellets at Elevated Temperatures

NASA Astrophysics Data System (ADS)

Li, Fei; Tangstad, Merete

This paper studies the quartz and carbon black pellets at elevated temperature with varying temperature and gas atmosphere. High-purity quartz and commercial ultra-pure carbon black was mixed (carbon content vet. 15%), and then pelletized into particles of l-3mm in diameter. The stoichiometric analysis of the pellet during heating is studied in thermogravimetric analysis (TGA) furnace at different temperature in CO and Ar atmosphere. The microstructure, phase changes and element content of sample before/after heating is characterized by X-ray diffraction, scanning electron microscope, X-ray fluorescence and LECO analyzer. The reaction process can be divided into two stages. Higher temperature and argon atmosphere are the positive parameters for SiC formation.

Preparation and characterisation of titania/hydroxyapatite composite coatings obtained by sol-gel process.

PubMed

Milella, E; Cosentino, F; Licciulli, A; Massaro, C

2001-06-01

In the present work a titania network encapsulating a hydroxyapatite particulate phase is proposed as a bioceramic composite coating. The coating on a titanium substrate was produced starting from a sol containing a mixture of titania colloidal particles and hydroxyapatite submicron particles using the dip-coating technique. The microstructure, the morphology and the surface chemical composition of the coating were characterised using X-ray diffraction (XRD), scanning electron microscopy (SEM) and X-ray photoelectron spectroscopy (XPS), respectively. Adhesion tests were also performed. These analyses showed that the obtained coating was chemically clean, homogeneous, rough, porous, with a low thickness and well-defined phase composition as well as a good adhesion to the substrate.

Study the Synthesis, Characterization and Immersion of Dense and Porous Bovine Hydroxyapatite Structures in Hank's Balanced Salt Solution

NASA Astrophysics Data System (ADS)

Eslami, N.; Mahmoodian, R.; Hamdi, M.; Khatir, Nadia Mahmoudi; Herliansyah, M. K.; Rafieerad, Ali Reza

2017-04-01

The bone-bonding potential of biomaterials is evaluated in vitro through examining the surface apatite formation in Hank's media to enhance biocompatibility, which is also applicable to facilitate in vivo osseointegration of implantable devices. Hence, bovine hydroxyapatite (BHA) bioceramic structures have been used in various biomedical applications such as orthopedic implants. In this article, the microstructure, in vitro bioactivity, and nanomechanical properties of the synthesized dense and porous BHA are investigated via scanning electron microscopy, x-ray diffraction, energy-dispersive x-ray spectroscopy, Fourier transform infrared spectroscopy, and nanoindentation analysis. From the obtained results, porous BHA mostly possesses adequate requirements for substitution as implants in the human body.

Microstructural Anisotropy of Magnetocaloric Gadolinium Cylinders: Effect on the Mechanical Properties of the Material

PubMed Central

Petrovič, Darja Steiner; Šturm, Roman; Naglič, Iztok; Markoli, Boštjan; Pepelnjak, Tomaž

2016-01-01

The development of advanced materials and technologies based on magnetocaloric Gd and its compounds requires an understanding of the dependency of mechanical properties on their underlying microstructure. Therefore, the aim of the study was to characterize microstructural inhomogeneities in the gadolinium that can be used in magnetocaloric refrigeration systems. Microstructures of magnetocaloric gadolinium cylinders were investigated by light microscopy and FE-SEM (Field Emission Scanning Electron Microscopy), EDS (Energy-dispersive X-ray Spectroscopy), and BSE (Back-scattered Electrons) in both the extrusion and the extrusion-transversal directions. XRD (X-ray Diffraction) analyses were performed to reveal the presence of calcium- and fluorine-based compounds. Metallographic characterization showed an oxidized and inhomogeneous microstructure of the cross-sections. The edges and the outer parts of the cylinders were oxidized more intensively on the surfaces directly exposed to the processing tools. Moreover, a significant morphological anisotropy of the non-metallic inclusions was observed. CaF inclusions act as active nucleation sites for internal oxidation. The non-metallic, Ca- and F-containing inclusions can be classified as complex calciumoxyfluorides. The solubility of Er and Yb in the CaF was negligible compared to the Gd matrix and/or the oxide phase. Lower mechanical properties of the material are a consequence of the lower structural integrity due to selective oxidation of surfaces and interfaces. PMID:28773502

In-situ Observation of Cross-Sectional Microstructural Changes and Stress Distributions in Fracturing TiN Thin Film during Nanoindentation

PubMed Central

Zeilinger, Angelika; Todt, Juraj; Krywka, Christina; Müller, Martin; Ecker, Werner; Sartory, Bernhard; Meindlhumer, Michael; Stefenelli, Mario; Daniel, Rostislav; Mitterer, Christian; Keckes, Jozef

2016-01-01

Load-displacement curves measured during indentation experiments on thin films depend on non-homogeneous intrinsic film microstructure and residual stress gradients as well as on their changes during indenter penetration into the material. To date, microstructural changes and local stress concentrations resulting in plastic deformation and fracture were quantified exclusively using numerical models which suffer from poor knowledge of size dependent material properties and the unknown intrinsic gradients. Here, we report the first in-situ characterization of microstructural changes and multi-axial stress distributions in a wedge-indented 9 μm thick nanocrystalline TiN film volume performed using synchrotron cross-sectional X-ray nanodiffraction. During the indentation, needle-like TiN crystallites are tilted up to 15 degrees away from the indenter axis in the imprint area and strongly anisotropic diffraction peak broadening indicates strain variation within the X-ray nanoprobe caused by gradients of giant compressive stresses. The morphology of the multiaxial stress distributions with local concentrations up to −16.5 GPa correlate well with the observed fracture modes. The crack growth is influenced decisively by the film microstructure, especially by the micro- and nano-scopic interfaces. This novel experimental approach offers the capability to interpret indentation response and indenter imprint morphology of small graded nanostructured features. PMID:26947558

Evolution of microstructure of Haynes 230 and Inconel 617 under mechanical testing at high temperatures

NASA Astrophysics Data System (ADS)

Hrutkay, Kyle

Haynes 230 and Inconel 617 are austenitic nickel based superalloys, which are candidate structural materials for next generation high temperature nuclear reactors. High temperature deformation behavior of Haynes 230 and Inconel 617 have been investigated at the microstructural level in order to gain a better understanding of mechanical properties. Tensile tests were performed at strain rates ranging from 10-3-10-5 s -1 at room temperature, 600 °C, 800 °C and 950 °C. Subsequent microstructural analysis, including Scanning Electron Microscopy, Transmission Electron Microscopy, Energy-Dispersive X-ray Spectroscopy, and X-Ray Diffraction were used to relate the microstructural evolution at high temperatures to that of room temperature samples. Grain sizes and precipitate morphologies were used to determine high temperature behavior and fracture mechanics. Serrated flow was observed at intermediate and high temperatures as a result of discontinuous slip and dynamic recrystallization. The amplitude of serration increased with a decrease in the strain rate and increase in the temperature. Dynamic strain ageing was responsible for serrations at intermediate temperatures by means of a locking and unlocking phenomenon between dislocations and solute atoms. Dynamic recrystallization nucleated by grain and twin bulging resulting in a refinement of grain size. Existing models found in the literature were discussed to explain both of these phenomena.

Microstructural Architecture, Microstructures, and Mechanical Properties for a Nickel-Base Superalloy Fabricated by Electron Beam Melting

NASA Astrophysics Data System (ADS)

Murr, L. E.; Martinez, E.; Gaytan, S. M.; Ramirez, D. A.; Machado, B. I.; Shindo, P. W.; Martinez, J. L.; Medina, F.; Wooten, J.; Ciscel, D.; Ackelid, U.; Wicker, R. B.

2011-11-01

Microstructures and a microstructural, columnar architecture as well as mechanical behavior of as-fabricated and processed INCONEL alloy 625 components produced by additive manufacturing using electron beam melting (EBM) of prealloyed precursor powder are examined in this study. As-fabricated and hot-isostatically pressed ("hipped") [at 1393 K (1120 °C)] cylinders examined by optical metallography (OM), scanning electron microscopy (SEM), transmission electron microscopy (TEM), energy-dispersive (X-ray) spectrometry (EDS), and X-ray diffraction (XRD) exhibited an initial EBM-developed γ″ (bct) Ni3Nb precipitate platelet columnar architecture within columnar [200] textured γ (fcc) Ni-Cr grains aligned in the cylinder axis, parallel to the EBM build direction. Upon annealing at 1393 K (1120 °C) (hot-isostatic press (HIP)), these precipitate columns dissolve and the columnar, γ, grains recrystallized forming generally equiaxed grains (with coherent {111} annealing twins), containing NbCr2 laves precipitates. Microindentation hardnesses decreased from 2.7 to 2.2 GPa following hot-isostatic pressing ("hipping"), and the corresponding engineering (0.2 pct) offset yield stress decreased from 0.41 to 0.33 GPa, while the UTS increased from 0.75 to 0.77 GPa. However, the corresponding elongation increased from 44 to 69 pct for the hipped components.

Fabrication, phase, microstructure and electrical properties of BNT-doped (Sr,La)TiO3 ceramics

NASA Astrophysics Data System (ADS)

Eaksuwanchai, Preeyakarn; Promsawat, Methee; Jiansirisomboon, Sukanda; Watcharapasorn, Anucha

2014-08-01

This research studied the effects of Bi0.5Na0.5TiO3 (BNT) doping on the phase, density, microstructure and electrical properties of (Sr,La)TiO3 (SLTO) ceramics. Separately calcined SLTO and BNT powders were mixed together to form (1-x)SLTO-xBNT (where x = 0, 0.01, 0.03, 0.05 and 0.07 mol fraction) compounds that were pressed into pellets and then sintered at 1500 °C for 3 h under ambient atmosphere. The relative bulk densities of all the ceramics were greater than 95% their theoretical values which were confirmed by their nearly zero-porosity microstructure. X-ray diffraction patterns indicated complete solid solutions with a cubic structure and a slight lattice contraction when BNT was added. The electrical conductivity was found to decrease with BNT addition, suggesting a reduced number of mobile charges. The dielectric constant also showed limited polarization due to defect dipoles formed by aliovalent ionic substitution of BNT. Further optimization in terms of composition and defect chemistry could lead to a compound suitable for thermoelectric applications.

3D/4D analyses of damage and fracture behaviours in structural materials via synchrotron X-ray tomography.

PubMed

Toda, Hiroyuki

2014-11-01

X-ray microtomography has been utilized for the in-situ observation of various structural metals under external loading. Recent advances in X-ray microtomography provide remarkable tools to image the interior of materials. In-situ X-ray microtomography provides a unique possibility to access the 3D character of internal microstructure and its time evolution behaviours non-destructively, thereby enabling advanced techniques for measuring local strain distribution. Local strain mapping is readily enabled by processing such high-resolution tomographic images either by the particle tracking technique or the digital image correlation technique [1]. Procedures for tracking microstructural features which have been developed by the authors [2], have been applied to analyse localised deformation and damage evolution in a material [3]. Typically several tens of thousands of microstructural features, such as particles and pores, are tracked in a tomographic specimen (0.2 - 0.3 mm(3) in volume). When a sufficient number of microstructural features is dispersed in 3D space, the Delaunay tessellation algorithm is used to obtain local strain distribution. With these techniques, 3D strain fields can be measured with reasonable accuracy. Even local crack driving forces, such as local variations in the stress intensity factor, crack tip opening displacement and J integral along a crack front line, can be measured from discrete crack tip displacement fields [4]. In the present presentation, complicated crack initiation and growth behaviour and the extensive formation of micro cracks ahead of a crack tip are introduced as examples.A novel experimental method has recently been developed by amalgamating a pencil beam X-Ray diffraction (XRD) technique with the microstructural tracking technique [5]. The technique provides information about individual grain orientations and 1-micron-level grain morphologies in 3D together with high-density local strain mapping. The application of this technique to the deformation behavior of a polycrystalline aluminium alloy will be demonstrated in the presentation [6].The synchrotron-based microtomography has been mainly utilized to light materials due to their good X-ray transmission. In the present talk, the application of the synchrotron-based microtomography to steels will be also introduced. Degradation of contrast and spatial resolution due to forward scattering could be avoided by selecting appropriate experimental conditions in order to obtain superior spatial resolution close to the physical limit even in ferrous materials [7]. © The Author 2014. Published by Oxford University Press on behalf of The Japanese Society of Microscopy. All rights reserved. For permissions, please e-mail: journals.permissions@oup.com.

Improved electrochemical properties of a coin cell using LiMn 1.5Ni 0.5O 4 as cathode in the 5 V range

NASA Astrophysics Data System (ADS)

Singhal, Rahul; Das, Suprem R.; Oviedo, Osbert; Tomar, Maharaj S.; Katiyar, Ram S.

Phase pure LiMn 1.5Ni 0.5O 4 powders were synthesized by a chemical synthesis route and were subsequently characterized as cathode materials in a Li-ion coin cell comprising a Li anode and lithium hexafluorophosphate (LiPF 6), dissolved in dimethyl carbonate (DMC) + ethylene carbonate (EC) [1:1, v/v ratio] as electrolyte. The spinel structure and phase purity of the powders were characterized using X-ray diffraction and micro-Raman spectroscopy. The presence of both oxidation and reduction peaks in the cyclic voltammogram revealed Li + extraction and insertion from the spinel structure. The charge-discharge characteristics of the coin cell were performed in the 3.0-4.8 V range. An initial discharge capacity of ∼140 mAh g -1 was obtained with 94% initial discharge capacity retention after 50 repeated cycles. The microstructures and compositions of the cathode before and after electrochemistry were investigated using scanning electron microscopy and energy-dispersive analysis by X-ray analysis, respectively. Using X-ray diffraction, Raman spectroscopy and electrochemical analysis, we correlated the structural stability and the electrochemical performance of this cathode.

Dye sensitized solar cell applications of CdTiO3-TiO2 composite thin films deposited from single molecular complex

NASA Astrophysics Data System (ADS)

Ehsan, Muhammad Ali; Khaledi, Hamid; Pandikumar, Alagarsamy; Huang, Nay Ming; Arifin, Zainudin; Mazhar, Muhammad

2015-10-01

A heterobimetallic complex [Cd2Ti4(μ-O)6(TFA)8(THF)6]·1.5THF (1) (TFA=trifluoroacetato, THF=tetrahydrofuran) comprising of Cd:Ti (1:2) ratio was synthesized by a chemical reaction of cadmium (II) acetate with titanium (IV) isopropoxide and triflouroacetic acid in THF. The stoichiometry of (1) was recognized by single crystal X-ray diffraction, spectroscopic and elemental analyses. Thermal studies revealed that (1) neatly decomposes at 450 °C to furnish 1:1 ratio of cadmium titanate:titania composite oxides material. The thin films of CdTiO3-TiO2 composite oxides were deposited at 550 °C on fluorine doped tin oxide coated conducting glass substrate in air ambient. The micro-structure, crystallinity, phase identification and chemical composition of microspherical architectured CdTiO3-TiO2 composite thin film have been determined by scanning electron microscopy, X-ray diffraction, Raman spectroscopy and energy dispersive X-ray analysis. The scope of composite thin film having band gap of 3.1 eV was explored as photoanode for dye-sensitized solar cell application.

Microstructural analysis in the depth direction of a heteroepitaxial AlN thick film grown on a trench-patterned template by nanobeam X-ray diffraction

NASA Astrophysics Data System (ADS)

Shida, K.; Takeuchi, S.; Tohei, T.; Miyake, H.; Hiramatsu, K.; Sumitani, K.; Imai, Y.; Kimura, S.; Sakai, A.

2018-04-01

This work quantitatively assessed the three-dimensional distribution of crystal lattice distortions in an epitaxial AlN thick film grown on a trench-patterned template, using nanobeam X-ray diffraction. Position-dependent ω-2θ-φ mapping clearly demonstrated local tilting, spacing and twisting of lattice planes as well as fluctuations in these phenomena on a sub-micrometer scale comparable to the pitch of the trench-and-terrace patterning. Analysis of the crystal lattice distortion in the depth direction was performed using a newly developed method in which the X-ray nanobeam diffracted from the sample surface to specific depths can be selectively detected by employing a Pt wire profiler. This technique generated depth-resolved ω-2θ-φ maps confirming that fluctuations in lattice plane tilting and spacing greatly depend on the dislocation distribution and the history of the AlN epitaxial growth on the trench-patterned structure. It was also found that both fluctuations were reduced on approaching the AlN surface and, in particular, were sharply reduced at specific depths in the terrace regions. These sharp reductions are attributed to the formation of sacrificial zones with degraded crystal quality around the trenches and possibly lead to raising the crystal quality near the surface of the AlN film.

Multiferroic properties in NdFeO3-PbTiO3 solid solutions

NASA Astrophysics Data System (ADS)

Kumar, Sunil; Pal, Jaswinder; Kaur, Shubhpreet; Agrawal, P.; Singh, Mandeep; Singh, Anupinder

2018-05-01

The x(NdFeO3) - 1-x(PbTiO3) where x = 0.2 solid solution was prepared using solid state reaction route. The X-ray diffraction (XRD) data reveals the single phase formation. The microstructure shows grain growth with lesser porosity. The energy dispersive analysis confirms the presence of elements in stochiometric proportion. The polarization vs. Electric field loop estabilished a ferroelectric type behavior but lossy in nature. This lossy nature may be due to the presence of large leakage current in solid solution. The Magnetization vs. Magnetic field plot exhibits a unsaturated hysteriss loop indicates that the sample is not purely ferromagnetic.

Micro X-ray diffraction analysis of thin films using grazing-exit conditions.

PubMed

Noma, T; Iida, A

1998-05-01

An X-ray diffraction technique using a hard X-ray microbeam for thin-film analysis has been developed. To optimize the spatial resolution and the surface sensitivity, the X-ray microbeam strikes the sample surface at a large glancing angle while the diffracted X-ray signal is detected with a small (grazing) exit angle. Kirkpatrick-Baez optics developed at the Photon Factory were used, in combination with a multilayer monochromator, for focusing X-rays. The focused beam size was about 10 x 10 micro m. X-ray diffraction patterns of Pd, Pt and their layered structure were measured. Using a small exit angle, the signal-to-background ratio was improved due to a shallow escape depth. Under the grazing-exit condition, the refraction effect of diffracted X-rays was observed, indicating the possibility of surface sensitivity.

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

Garcia-Mateo, Carlos, E-mail: cgm@cenim.csic.es

Since the major strengthening mechanisms in nanocrystalline bainitic steels arise from the exceptionally small size of the bainitc ferrite plate, accurate determination of this parameter is fundamental for quantitative relating the microstructure to the mechanical properties. In this work, the thickness of the bainitic ferrite subunits obtained by different bainitic heat treatments was determined in two steels, with carbon contents of 0.3 and 0.7 wt.%, from SEM and TEM micrographs. As these measurements were made on 2D images taken from random sections, the method includes some stereological correction factors to obtain accurate information. Finally, the determined thicknesses of bainitic ferritemore » plates were compared with the crystallite size calculated from the analysis of X-ray diffraction peak broadening. Although in some case the values obtained for crystallite size and plate thickness can be similar, this study confirms that indeed they are two different parameters. - Highlights: •Bainitic microstructure in a nanostructured and sub-micron steel •Bainitic ferrite plate thickness measured by SEM and TEM •Crystallite size determined by X-ray analysis.« less

Influence of microstructure on hardness of plasma sprayed Al2O3-TiO2-MgO coatings with interface diffusion by heat treatment

NASA Astrophysics Data System (ADS)

Chen, Kunlun; Song, Peng; Li, Chao; Lu, Jiansheng

2017-12-01

The effect of heat treatment on the microstructure and mechanical properties of Al2O3-TiO2 coatings doped with 5 wt% MgO was investigated in this paper. The composite coatings were prepared by atmospheric plasma spraying (APS) and heat treated at 1000 °C for 24 h in Ar. The coatings were analyzed using scanning electron microscopy with electron probe x-ray microanalysis and x-ray diffraction. The hardness was determined using a Vickers hardness test on the as-sprayed coatings and after heat treatment. The results showed that the interface diffusion between the Al-rich and Ti-rich layers resulted in mutual pinning within the coating during the heat treatment. The newly formed MgAl2O4 phase promoted cracking-healing behavior within the coating. We conclude that increase of the hardness of the coatings was mainly caused by the mutual pinning interface and crack healing.

Advanced Microstructural Study of Suspension Plasma Sprayed Hydroxyapatite Coatings

NASA Astrophysics Data System (ADS)

Podlesak, Harry; Pawlowski, Lech; D'Haese, Romain; Laureyns, Jacky; Lampke, Thomas; Bellayer, Severine

2010-03-01

Fine, home-synthesized, hydroxyapatite powder was formulated with water and alcohol to obtain a suspension used to plasma spray coatings onto a titanium substrate. The deposition process was optimized using statistical design of 2 n experiments with two variables: spray distance and electric power input to plasma. X-ray diffraction (XRD) was used to determine quantitatively the phase composition of obtained deposits. Raman microscopy and electron probe microanalysis (EPMA) enabled localization of the phases in different positions of the coating cross sections. Transmission electron microscopic (TEM) study associated with energy-dispersive x-ray spectroscopy (EDS) enabled visualization and analysis of a two-zone microstructure. One zone contained crystals of hydroxyapatite, tetracalcium phosphate, and a phase rich in calcium oxide. This zone included lamellas, usually observed in thermally sprayed coatings. The other zone contained fine hydroxyapatite grains that correspond to nanometric and submicrometric solids from the suspension that were agglomerated and sintered in the cold regions of plasma jet and on the substrate.

THE PHYSICAL AND CHEMICAL MICROSTRUCTURE OF THE ACHATINA FULICA EPIPHRAGM.

PubMed

Struthers, M.; Rosair, G.; Buckman, J.; Viney, C.

2002-05-01

Microstructural characterization of Achatina fulica Bowdich, 1822 epiphragms and mucus secretions was performed to address two questions: what are the structure and composition of the reinforcing inorganic phase in the epiphragms, and what enables a durable epiphragm to form quickly in comparison to other biomineralized materials? Characterization was performed by a combination of light microscopy (relying on a variety of contrast modes), wet chemical tests, environmental scanning electron microscopy (including the use of energy dispersive X-ray analysis to obtain compositional data), and X-ray diffraction. The morphology of the inorganic phase promotes mechanical interlocking and presents a large surface for binding to the organic matrix. Strong binding occurs between the organic and inorganic phases. The inorganic phase adopts the calcite structure; its composition is Ca(0.912) Mg(0.088) CO(3). Epiphragms can form quickly because pre-grown crystals of the inorganic reinforcing phase are co-deposited with the mucus matrix. Unlike other biomineralized material, the crystals are not solution-grown in situ on an organic template in the final product.

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

Yadav, Praveen Kumar, E-mail: praveenyadav@rrcat.gov.in; Nayak, Maheswar; Rai, Sanjay Kumar

The authors report the effect of argon ion to molybdenum atom ratio (r) on the microstructure of low energy (70 eV) argon ion assisted electron beam evaporated Mo thin films. Surface roughness, morphology, and crystallinity of Mo films are found to strongly depend on “r.” Increase of “r” from 0 to 100 induces gradual loss in crystallinity, reduction in surface roughness and systematic increase in density of the film. For “r” ∼ 100, average atomic density of the film approaches the bulk value (97%) with lowest surface roughness. Further, increasing “r” up to 170 reduces the atomic density, increases roughness, and increase inmore » crystallinity induced by low energy Ar ion beam. The observed surface roughness and grain size determined by x-ray reflectivity and glancing incidence x-ray diffraction correlate well with atomic force microscopy measurements. This study demonstrates that for r = 100 one gets lowest roughness Mo film with highest density and nearly amorphous microstructure. The growth model is discussed by structural zone model.« less

Effect of aluminum contents on sputter deposited CrAlN thin films

NASA Astrophysics Data System (ADS)

Vyas, A.; Zhou, Z. F.; Shen, Y. G.

2018-02-01

Pure CrN and CrAlN films with varied Al concentrations were prepared onto Si(100) substrates by an unbalanced reactive dc-magnetron sputtering system. The crystal structure, chemical states, and microstructure of the films were characterized by X-ray diffraction, X-ray photoelectron microscopy, transmission electron microscopy whereas mechanical properties were determined by nano-indentation measurements. XRD results showed a prominent (200) reflection in both CrN and CrAlN films. Results demonstrate that CrAlN films formed a solid solution and doping of Al atoms replace the Cr atoms affecting the lattice parameter and crystallization of the films. All Al doped films were of B1 NaCl-type structure, demonstrating that CrAlN films primarily crystallized in cubic structure. Microstructural investigation by TEM for a CrAlN film containing Al content of 24.1 at.%, revealed that there exists an amorphous/nanocrystalline domains (grains of about ∼ 11 nm) and hardness increases 22% when compared with pure CrN film.

Thermal effects of laser marking on microstructure and corrosion properties of stainless steel.

PubMed

Švantner, M; Kučera, M; Smazalová, E; Houdková, Š; Čerstvý, R

2016-12-01

Laser marking is an advanced technique used for modification of surface optical properties. This paper presents research on the influence of laser marking on the corrosion properties of stainless steel. Processes during the laser beam-surface interaction cause structure and color changes and can also be responsible for reduction of corrosion resistance of the surface. Corrosion tests, roughness, microscopic, energy dispersive x-ray, grazing incidence x-ray diffraction, and ferrite content analyses were carried out. It was found that increasing heat input is the most crucial parameter regarding the degradation of corrosion resistance of stainless steel. Other relevant parameters include the pulse length and pulse frequency. The authors found a correlation between laser processing parameters, grazing incidence x-ray measurement, ferrite content, and corrosion resistance of the affected surface. Possibilities and limitations of laser marking of stainless steel in the context of the reduction of its corrosion resistance are discussed.

Applications of synchrotron x-ray diffraction topography to fractography

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

Bilello, J.C.

1983-01-01

Fractographs have been taken using a variety of probes each of which produces different types of information. Methods which have been used to examine fracture surfaces include: (a) optical microscopy, particularly interference contrast methods, (b) scanning electron microscopy (SEM), (c) SEM with electron channelling, (d) SEM with selected-area electron channelling, (e) Berg-Barrett (B-B) topography, and now (f) synchrotron x-radiation fractography (SXRF). This review concentrated on the role that x-ray methods can play in such studies. In particular, the ability to nondestructively assess the subsurface microstructure associated with the fracture to depths of the order of 5 to 10 ..mu..m becomesmore » an important attribute for observations of a large class of semi-brittle metals, semiconductors and ceramics.« less

Stability of Catalyzed Magnesium Hydride Nanocrystalline During Hydrogen Cycling. Part II: Microstructure Evolution

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

Zhou, Chengshang; Fang, Zhigang Zak; Bowman, Robert C.

2015-10-01

In Part I, the cyclic stabilities of the kinetics of catalyzed MgH2 systems including MgH2–TiH2, MgH2–TiMn2, and MgH2–VTiCr were investigated, showing stable kinetics at 300 °C but deteriorations of the hydrogenation kinetics at temperatures below 150 °C. The present Part II describes the characterization of uncycled and cycled catalyzed MgH2 by X-ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM), and X-ray photoelectron spectroscopy (XPS) analysis. XRD analysis shows the crystallite sizes of the Mg and MgH2 significantly increased after the cycling. The mean crystallite sizes of the catalysts (TiH2 and VTiCr) increased moderately after the cycling. SEMmore » and TEM imaging were used to compare the microstructures of uncycled (as-milled) and cycled materials, revealing a drastic change of the microstructure after 100 cycles. In particular, results from energy-dispersive spectroscopy (EDS) mapping show that a change of distribution of the catalyst particles in the Mg and MgH2 phase occurred during the cycling.« less

Microstructural analyses of two high noble gold-platinum alloys before and after conditioning in a cell culture medium

NASA Astrophysics Data System (ADS)

Rudolf, R.; Anzel, I.; Gusel, L.; Stamenkovi, D.; Todorovi, A.; Colic, M.

2010-12-01

Microstructures of two high noble experimental Au-Pt alloys were compared before and after conditioning for biocompatibility, in order to identify phases and microelements responsible for the alloys' corrosive behaviour. Microstructural characterization was carried-out by optical and scanning electron microscopy, in addition to energy dispersive X-ray analysis. X-ray diffraction was applied to determine the phases' composition and their contribution in the alloys. Additionally, simultaneous thermal analysis was used to identify the temperatures of phase transformations. An overall assessment before conditioning showed that Au-Pt I is a two-phase alloy containing a dominant Au-rich α1 phase and a minor Pt-rich α2 phase, while the Au-Pt II alloy contains in addition three minor phases: AuZn3, Pt3Zn and Au1.4Zn0.52. The highest content of Zn (up to 6.76 wt.%) was detected in the Pt3Zn phase. After RPMI cell culture medium conditioning, the Pt3Zn and AuZn3 phases disappeared, suggesting that they are predominantly responsible for Zn loss and the lower corrosive stability of the Au-Pt II alloy.

Structure and Infrared Emissivity Properties of the MAO Coatings Formed on TC4 Alloys in K2ZrF6-Based Solution

PubMed Central

Li, Ying; Hu, Dan; Xi, Zhengping

2018-01-01

Micro-arc oxidation (MAO) ceramic coatings were formed on TC4 alloy surface in silicate and metaphosphate electrolytes based with K2ZrF6 for various concentrations. X-ray diffraction (XRD), Scanning electron microscopy (SEM), X-ray photoelectron spectroscopy (XPS) were used to characterize the phase composition, microstructure and chemical compositions of the coatings. The infrared emissivity of the coatings was measured at 50 °C in a wavelength range of 8–20 µm. The microstructural observations all revealed the typical porousstructures. Moreover, adecline in roughness and thickness of the prepared coatings can be observed when the concentration of K2ZrF6 increases. Combined with the results of XRD and XPS, it was found that all the oxides existed as the amorphous form in the coatings except the TiO2 phase. The coatings exhibited the highest infrared emissivity value (about 0.89) when the concentration of K2ZrF6 was 6 g/L, which was possibly attributed to the defect microstructure and the optimal role of ZrO2. PMID:29414841

Growth of carbon nanotubes in arc plasma treated graphite disc: microstructural characterization and electrical conductivity study

NASA Astrophysics Data System (ADS)

Nayak, B. B.; Sahu, R. K.; Dash, T.; Pradhan, S.

2018-03-01

Circular graphite discs were treated in arc plasma by varying arcing time. Analysis of the plasma treated discs by field emission scanning electron microscope revealed globular grain morphologies on the surfaces, but when the same were observed at higher magnification and higher resolution under transmission electron microscope, growth of multiwall carbon nanotubes of around 2 nm diameter was clearly seen. In situ growth of carbon nanotube bundles/bunches consisting of around 0.7 nm tube diameter was marked in the case of 6 min treated disc surface. Both the untreated and the plasma treated graphite discs were characterized by X-ray diffraction, energy dispersive spectra of X-ray, X-ray photoelectron spectroscopy, transmission electron microscopy, micro Raman spectroscopy and BET surface area measurement. From Raman spectra, BET surface area and microstructure observed in transmission electron microscope, growth of several layers of graphene was identified. Four-point probe measurements for electrical resistivity/conductivity of the graphite discs treated under different plasma conditions showed significant increase in conductivity values over that of untreated graphite conductivity value and the best result, i.e., around eightfold increase in conductivity, was observed in the case of 6 min plasma treated sample exhibiting carbon nanotube bundles/bunches grown on disc surface. By comparing the microstructures of the untreated and plasma treated graphite discs, the electrical conductivity increase in graphite disc is attributed to carbon nanotubes (including bundles/bunches) growth on disc surface by plasma treatment.

Microstructure of Haynes® 282® Superalloy after Vacuum Induction Melting and Investment Casting of Thin-Walled Components.

PubMed

Matysiak, Hubert; Zagorska, Malgorzata; Andersson, Joel; Balkowiec, Alicja; Cygan, Rafal; Rasinski, Marcin; Pisarek, Marcin; Andrzejczuk, Mariusz; Kubiak, Krzysztof; Kurzydlowski, Krzysztof J

2013-11-01

The aim of this work was to characterize the microstructure of the as-cast Haynes ® 282 ® alloy. Observations and analyses were carried out using techniques such as X-ray diffraction (XRD), light microscopy (LM), scanning electron microscopy (SEM), transmission electron microscopy (TEM), X-ray spectroscopy (EDS), wave length dispersive X-ray spectroscopy (WDS), auger electron spectroscopy (AES) and electron energy-loss spectrometry (EELS). The phases identified in the as-cast alloy include: γ (gamma matrix), γ' (matrix strengthening phase), (TiMoCr)C (primary carbide), TiN (primary nitride), σ (sigma-TCP phase), (TiMo)₂SC (carbosulphide) and a lamellar constituent consisting of molybdenum and chromium rich secondary carbide phase together with γ phase. Within the dendrites the γ' appears mostly in the form of spherical, nanometric precipitates (74 nm), while coarser (113 nm) cubic γ' precipitates are present in the interdendritic areas. Volume fraction content of the γ' precipitates in the dendrites and interdendritic areas are 9.6% and 8.5%, respectively. Primary nitrides metallic nitrides (MN), are homogeneously dispersed in the as-cast microstructure, while primary carbides metallic carbides (MC), preferentially precipitate in interdendritic areas. Such preference is also observed in the case of globular σ phase. Lamellar constituents characterized as secondary carbides/γ phases were together with (TiMo)₂SC phase always observed adjacent to σ phase precipitates. Crystallographic relations were established in-between the MC, σ, secondary carbides and γ/γ' matrix.

Novel multiform morphologies of hydroxyapatite: Synthesis and growth mechanism

NASA Astrophysics Data System (ADS)

Mary, I. Reeta; Sonia, S.; Viji, S.; Mangalaraj, D.; Viswanathan, C.; Ponpandian, N.

2016-01-01

Morphological evolution of materials becomes a prodigious challenge due to their key role in defining their functional properties and desired applications. Herein, we report the synthesis of hydroxyapatite (HAp) microstructures with multiform morphologies, such as spheres, cubes, hexagonal rods and nested bundles constructed from their respective nanoscale building blocks via a simple cost effective hydro/solvothermal method. A possible formation mechanism of diverse morphologies of HAp has been presented. Structural analysis based on X-ray diffraction (XRD) and Fourier transform infrared (FTIR) spectroscopy confirms the purity of the HAp microstructures. The multiform morphologies of HAp were corroborated by using Field emission scanning electron microscope (FESEM).

Zirconium diselenite microstructures, formation and mechanism

NASA Astrophysics Data System (ADS)

Naik, Chandan C.; Salker, A. V.

2018-04-01

In this work, a series of microstructures of zirconium diselenite (Zr(SeO3)2) has been prepared via a simple precipitation method at room temperature without adding any organic surfactants. Phase purity of the sample has been checked by X-ray Diffraction. From the SEM, FESEM, and TEM images spheroid nanoparticles to the starfish-like structure of zirconium diselenite are detected. The morphological evolution processes were investigated carefully following time-dependent experiments and a growth mechanism has been proposed. Two different crystal growth processes, the oriented attachment process accompanying the Ostwald ripening process were held responsible for the formation of a structure resembling starfish having four arms.

The microstructure and magnetic properties of Cu/CuO/Ni core/multi-shell nanowire arrays

NASA Astrophysics Data System (ADS)

Yang, Feng; Shi, Jie; Zhang, Xiaofeng; Hao, Shijie; Liu, Yinong; Feng, Chun; Cui, Lishan

2018-04-01

Multifunctional metal/oxide/metal core/multi-shell nanowire arrays were prepared mostly by physical or chemical vapor deposition. In our study, the Cu/CuO/Ni core/multi-shell nanowire arrays were prepared by AAO template-electrodeposition and oxidation processes. The Cu/Ni core/shell nanowire arrays were prepared by AAO template-electrodeposition method. The microstructure and chemical compositions of the core/multi-shell nanowires and core/shell nanowires have been characterized using transmission electron microscopy with HADDF-STEM and X-ray diffraction. Magnetization measurements revealed that the Cu/CuO/Ni and Cu/Ni nanowire arrays have high coercivity and remanence ratio.

Understanding corrosion behavior of Mg-Zn-Ca alloys from subcutaneous mouse model: effect of Zn element concentration and plasma electrolytic oxidation.

PubMed

Jang, Yongseok; Tan, Zongqing; Jurey, Chris; Xu, Zhigang; Dong, Zhongyun; Collins, Boyce; Yun, Yeoheung; Sankar, Jagannathan

2015-03-01

Mg-Zn-Ca alloys are considered as suitable biodegradable metallic implants because of their biocompatibility and proper physical properties. In this study, we investigated the effect of Zn concentration of Mg-xZn-0.3Ca (x=1, 3 and 5wt.%) alloys and surface modification by plasma electrolytic oxidation (PEO) on corrosion behavior in in vivo environment in terms of microstructure, corrosion rate, types of corrosion, and corrosion product formation. Microstructure analysis of alloys and morphological characterization of corrosion products were conducted using x-ray computed tomography (micro-CT) and scanning electron microscopy (SEM). Elemental composition and crystal structure of corrosion products were determined using x-ray diffraction (XRD) and electron dispersive x-ray spectroscopy (EDX). The results show that 1) as-cast Mg-xZn-0.3Ca alloys are composed of Mg matrix and a secondary phase of Ca2Mg6Zn3 formed along grain boundaries, 2) the corrosion rate of Mg-xZn-0.3Ca alloys increases with increasing concentration of Zn in the alloy, 3) corrosion rates of alloys treated by PEO sample are decreased in in vivo environment, and 4) the corrosion products of these alloys after in vivo tests are identified as brucite (Mg(OH)2), hydroxyapatite (Ca10(PO4)6(OH)2), and magnesite (MgCO3·3H2O). Copyright © 2014 Elsevier B.V. All rights reserved.

Microstructures of GaN1-xPx layers grown on (0001) GaN substrates by gas source molecular beam epitaxy

NASA Astrophysics Data System (ADS)

Seong, Tae-Yeon; Bae, In-Tae; Choi, Chel-Jong; Noh, D. Y.; Zhao, Y.; Tu, C. W.

1999-03-01

Transmission electron microscope (TEM), transmission electron diffraction (TED), and synchrotron x-ray diffraction (XRD) studies have been performed to investigate microstructural behavior of gas source molecular beam epitaxial GaN1-xPx layers grown on (0001) GaN/sapphire at temperatures (Tg) in the range 500-760 °C. TEM, TED, and XRD results indicate that the samples grown at Tg⩽600 °C undergo phase separation resulting in a mixture of GaN-rich and GaP-rich GaNP with zinc-blende structure. However, the samples grown at Tg⩾730 °C are found to be binary zinc-blende GaN(P) single crystalline materials. As for the 500 °C layer, the two phases are randomly oriented and distributed, whereas the 600 °C layer consists of phases that are elongated and inclined by 60°-70° clockwise from the [0001]α-GaN direction. The samples grown at Tg⩾730 °C are found to consist of two types of microdomains, namely, GaN(P)I and GaN(P)II; the former having twin relation to the latter.

X-ray imaging and controlled solidification of Al-Cu alloys toward microstructures by design

DOE PAGES

Clarke, Amy J.; Tourret, Damien; Imhoff, Seth D.; ...

2015-01-30

X-ray imaging, which permits the microscopic visualization of metal alloy solidification dynamics, can be coupled with controlled solidification to create microstructures by design. In this study, this x-ray image shows a process-derived composite microstructure being made from a eutectic Al-17.1 at.%Cu alloy by successive solidification and remelting steps.

Structure of Al-Fe alloys prepared by different methods after severe plastic deformation under pressure

NASA Astrophysics Data System (ADS)

Dobromyslov, A. V.; Taluts, N. I.

2017-06-01

Al-Fe alloys prepared by casting, rapid quenching from the melt, and mechanical alloying from elemental powders have been studied using X-ray diffraction analysis, optical metallography, transmission electron microscopy, and microhardness measurements in the initial state and after severe plastic deformation by high-pressure torsion using Bridgman anvils. The relationship between the phase composition, microstructure, and the microhardness of the investigated alloys has been established.

Comparison of Microstructures and Mechanical Properties for Solid and Mesh Cobalt-Base Alloy Prototypes Fabricated by Electron Beam Melting

NASA Astrophysics Data System (ADS)

Gaytan, S. M.; Murr, L. E.; Martinez, E.; Martinez, J. L.; Machado, B. I.; Ramirez, D. A.; Medina, F.; Collins, S.; Wicker, R. B.

2010-12-01

The microstructures and mechanical behavior of simple, as-fabricated, solid geometries (with a density of 8.4 g/cm3), as-fabricated and fabricated and annealed femoral (knee) prototypes, and reticulated mesh components (with a density of 1.5 g/cm3) all produced by additive manufacturing (AM) using electron beam melting (EBM) of Co-26Cr-6Mo-0.2C powder are examined and compared in this study. Microstructures and microstructural issues are examined by optical metallography (OM), scanning electron microscopy (SEM), transmission electron microscopy (TEM), energy-dispersive X-ray spectrometry (EDS), and X-ray diffraction (XRD), while mechanical properties included selective specimen tensile testing and Vickers microindentation hardness (HV) and Rockwell C-scale hardness (HRC) measurements. Orthogonal (X-Y) melt scanning of the electron beam during AM produced unique, orthogonal and related Cr23C6 carbide (precipitate) arrays (a controlled microstructural architecture) with dimensions of 2 μm in the build plane perpendicular to the build direction, while connected carbide columns were formed in the vertical plane, parallel to the build direction, with microindentation hardnesses ranging from 4.4 to 5.9 GPa, corresponding to a yield stress and ultimate tensile strength (UTS) of 0.51 and 1.45 GPa with elongations ranging from 1.9 to 5.3 pct. Annealing produced an equiaxed fcc grain structure with some grain boundary carbides, frequent annealing twins, and often a high density of intrinsic {111} stacking faults within the grains. The reticulated mesh strut microstructure consisted of dense carbide arrays producing an average microindentation hardness of 6.2 GPa or roughly 25 pct higher than the fully dense components.

High T(sub c) superconductor/ferroelectric heterostructures

NASA Astrophysics Data System (ADS)

Ryder, Daniel F., Jr.

1994-12-01

Thin films of the ferroelectric perovskite, Ba(x) Sr(1-x) TiO3 (BST), were deposited on superconducting (100)YBa2Cu3O(x)(YBCO)/ (100)Yttria-stabilized zirconia(YSZ) substrates and (100)Si by ion-beam sputtering. Microstructural and compositional features of the ceramic bilayer were assessed by a combination of x-ray diffraction (XRD) and scanning electron microscopy. The films were smooth and featureless, and energy dispersive x-ray spectroscopy (EDX) data indicated that film composition closely matched target composition. XRD analysis showed that films deposited on YBCO substrates were highly c-axis textured, while the films deposited on (100)Si did not exhibit any preferred growth morphology. The superconducting properties of the YBCO substrate layer were maintained throughout the processing stages and, as such, it was demonstrated that ion beam sputtering is a viable method for the deposition of Ferroelectric/YBCO heterostructures.

The Influence of Sintering Temperature on the Microstructure and Thermoelectric Properties of n-Type Bi2Te3- x Se x Nanomaterials

NASA Astrophysics Data System (ADS)

Du, Y.; Cai, K. F.; Li, H.; An, B. J.

2011-05-01

Pure Bi2Te3 and Bi2Se3 nanopowders were hydrothermally synthesized, and n-type Bi2Te3- x Se x bulk samples were prepared by hot pressing a mixture of Bi2Te3 and Bi2Se3 nanopowders at 623 K, 648 K or 673 K and 80 MPa in vacuum. The phase composition of the powders and bulk samples were characterized by x-ray diffraction. The morphology of the powders was examined by transmission electron microscopy. The microstructure and composition of the bulk samples were characterized by field-emission scanning electron microscopy and energy-dispersive x-ray spectroscopy, respectively. The density of the samples increased with sintering temperature. The samples were somewhat oxidized, and the amount of oxide (Bi2TeO5) present increased with sintering temperature. The samples consisted of sheet-like grains with a thickness less than 100 nm. Seebeck coefficient, electrical conductivity, and thermal conductivity of the samples were measured from room temperature up to 573 K. Throughout the temperature range investigated, the sample sintered at 623 K had a higher power factor than the samples sintered at 648 K or 673 K.

Microstructural, Optical and Dielectric Properties of Al-Incorporated SnO2 Nanoparticles

NASA Astrophysics Data System (ADS)

Ahmed, Ateeq; Tripathi, P.; Naseem Siddique, M.; Ali, Tinku

2017-08-01

In this work, Pure SnO2 and Al doped SnO2 nanoparticles with the composition Sn1-xAlxO2 (x = 0, and 0.05) have been successfully prepared using sol-gel technique. The effect of Al dopant on microstructural, optical and dielectric properties has been investigated by X-ray diffraction (XRD), Scanning electron microscopy (SEM), Ultraviolet (UV-Visible) absorption spectroscopy andImpedance spectroscopy (LCR meter)respectively. The XRD patterns indicated tetragonal rutile structure with single phase without any detectable impurity for all samples and incorporation of Al ions into the SnO2 lattice. Crystalline size decreased with aluminum content. The results of SEM confirm nanoparticles size decreases with Al dopant. UV-Visible results showed that optical band also decreases when Al is doped into pure SnO2 lattice. Frequency dependent dielectric properties of pure and doped SnO2 nanoparticles have been also studied.

X-ray diffraction from shock-loaded polycrystals.

PubMed

Swift, Damian C

2008-01-01

X-ray diffraction was demonstrated from shock-compressed polycrystalline metals on nanosecond time scales. Laser ablation was used to induce shock waves in polycrystalline foils of Be, 25-125 microm thick. A second laser pulse was used to generate a plasma x-ray source by irradiation of a Ti foil. The x-ray source was collimated to produce a beam of controllable diameter, which was directed at the Be sample. X-rays were diffracted from the sample, and detected using films and x-ray streak cameras. The diffraction angle was observed to change with shock pressure. The diffraction angles were consistent with the uniaxial (elastic) and isotropic (plastic) compressions expected for the loading conditions used. Polycrystalline diffraction will be used to measure the response of the crystal lattice to high shock pressures and through phase changes.

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.

Synthesis, Characterization and Antibacterial Activity of BiVO4 Microstructure

NASA Astrophysics Data System (ADS)

Ekthammathat, Nuengruethai; Phuruangrat, Anukorn; Thongtem, Somchai; Thongtem, Titipun

2018-05-01

Hyperbranched BiVO4 microstructure were successfully synthesized by a hydrothermal method. Upon characterization the products by X-ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM), Fourier transform infrared (FTIR) spectroscopy, Raman spectroscopy, selected area electron diffraction (SAED) and photoluminescence (PL) spectroscopy, pure monoclinic hyperbranched BiVO4 with dominant vibration peak at 810 cm-1 and strong photoemission peak at 360 nm was synthesized in the solution with pH 1. In the solution with pH 2, tetragonal BiVO4 phase was also detected. In this research, antibacterial activity against S. aureus and E. coli was investigated by counting the colony forming unit (CFU). At 37°C within 24 h, the monoclinic BiVO4 phase can play the role in inhibiting S. aureus growth (350 CFU/mL remaining bacteria) better than that against E. coli (a large number of remaining bacteria).

Characterization of the α phase nucleation in a two-phase metastable β titanium alloy

NASA Astrophysics Data System (ADS)

Lenain, A.; Clément, N.; Jacques, P. J.; Véron, M.

2005-12-01

Beta titanium alloys are increasingly the best choice for automotive and aerospace applications due to their high performance-to-density ratio. Among these alloys, the TIMETAL Ti-LCB is already used in the automotive industry because it presents excellent mechanical properties and a lower cost compared with other Ti alloys. The current study deals with the characterization of the nucleation and growth of the α phase in several thermomechanical processes, because the distribution and size of the α phase strongly influence the mechanical properties of the resulting microstructures. Several heat treatments were conducted after either cold rolling or annealing. The resulting microstructures were characterized by scanning electron microscopy, transmission electron microscopy, x-ray diffraction, or electron backscatter diffraction. It was observed that the morphology and the volume fraction of the α phase are strongly dependent on the holding temperature, on the heating or cooling rate, and on the β grain size.

Single-pulse x-ray diffraction using polycapillary optics for in situ dynamic diffraction

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

Maddox, B. R., E-mail: maddox3@llnl.gov; Akin, M. C., E-mail: akin1@llnl.gov; Teruya, A.

2016-08-15

Diagnostic use of single-pulse x-ray diffraction (XRD) at pulsed power facilities can be challenging due to factors such as the high flux and brightness requirements for diffraction and the geometric constraints of experimental platforms. By necessity, the x-ray source is usually positioned very close, within a few inches of the sample. On dynamic compression platforms, this puts the x-ray source in the debris field. We coupled x-ray polycapillary optics to a single-shot needle-and-washer x-ray diode source using a laser-based alignment scheme to obtain high-quality x-ray diffraction using a single 16 ns x-ray pulse with the source >1 m from themore » sample. The system was tested on a Mo sample in reflection geometry using 17 keV x-rays from a Mo anode. We also identified an anode conditioning effect that increased the x-ray intensity by 180%. Quantitative measurements of the x-ray focal spot produced by the polycapillary yielded a total x-ray flux on the sample of 3.3 ± 0.5 × 10{sup 7} molybdenum Kα photons.« less

Catalytic Graphitization of Coal-Based Carbon Materials with Light Rare Earth Elements.

PubMed

Wang, Rongyan; Lu, Guimin; Qiao, Wenming; Yu, Jianguo

2016-08-30

The catalytic graphitization mechanism of coal-based carbon materials with light rare earth elements was investigated using X-ray diffraction, scanning electron microscopy, energy-dispersive X-ray spectroscopy, selected-area electron diffraction, and high-resolution transmission electron microscopy. The interface between light rare earth elements and carbon materials was carefully observed, and two routes of rare earth elements catalyzing the carbon materials were found: dissolution-precipitation and carbide formation-decomposition. These two simultaneous processes certainly accelerate the catalytic graphitization of carbon materials, and light rare earth elements exert significant influence on the microstructure and thermal conductivity of graphite. Moreover, by virtue of praseodymium (Pr), it was found that a highly crystallographic orientation of graphite was induced and formed, which was reasonably attributed to the similar arrangements of the planes perpendicular to (001) in both graphite and Pr crystals. The interface between Pr and carbon was found to be an important factor for the orientation of graphite structure.

Template-free solution approach to synthesize CdS dendrites with SCN based ionic liquid

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

Li, Kangfeng; Li, Jiajia; Cheng, Xianyi

2011-07-15

Highlights: {yields} Template-free solution approach to synthesize CdS hierarchical dendrites. {yields} The 1-butyl-3-methlyimidazole thiocyanate ([BMIM][SCN]) plays doubly functional roles in the progress. {yields} The CdS hierarchical dendrites exhibit a more intense emission at 710 nm belongs to infrared band. -- Abstract: Cadmium sulfide dendrites were synthesized by a facile hydrothermal treatment from CdCl{sub 2} and ionic liquid 1-butyl-3-methlyimidazole thiocyanate acted both as sulfur source and surfactant. The product was characterized by means of X-ray powder diffraction and scanning electron microscopy. X-ray powder diffraction studies indicated that the product was well-crystallized hexagonal phase of CdS, and the scanning electron microscopy imagesmore » showed that the obtained powders consisted of a wealth of well-defined CdS dendritic microstructures with a pronounced trunk and highly ordered branches. The UV-Vis and photoluminescence spectroscopy measurements were taken as well. The possible formation mechanism of CdS dendrites was simply proposed in the end.« less

Development of Cu Reinforced SiC Particulate Composites

NASA Astrophysics Data System (ADS)

Singh, Harshpreet; Kumar, Lailesh; Nasimul Alam, Syed

2015-02-01

This paper presents the results of Cu-SiCp composites developed by powder metallurgy route and an attempt has been made to make a comparison between the composites developed by using unmilled Cu powder and milled Cu powder. SiC particles as reinforcement was blended with unmilled and as-milled Cu powderwith reinforcement contents of 10, 20, 30, 40 vol. % by powder metallurgy route. The mechanical properties of pure Cu and the composites developed were studied after sintering at 900°C for 1 h. Density of the sintered composites were found out based on the Archimedes' principle. X-ray diffraction of all the composites was done in order to determine the various phases in the composites. Scanning electron microscopy (SEM) and EDS (electron diffraction x-ray spectroscopy) was carried out for the microstructural analysis of the composites. Vickers microhardness tester was used to find out the hardness of the samples. Wear properties of the developed composites were also studied.

Kinetics of methane hydrate decomposition studied via in situ low temperature X-ray powder diffraction.

PubMed

Everett, S Michelle; Rawn, Claudia J; Keffer, David J; Mull, Derek L; Payzant, E Andrew; Phelps, Tommy J

2013-05-02

Gas hydrate is known to have a slowed decomposition rate at ambient pressure and temperatures below the melting point of ice. As hydrate exothermically decomposes, gas is released and water of the clathrate cages transforms into ice. Based on results from the decomposition of three nominally similar methane hydrate samples, the kinetics of two regions, 180-200 and 230-260 K, within the overall decomposition range 140-260 K, were studied by in situ low temperature X-ray powder diffraction. The kinetic rate constants, k(a), and the reaction mechanisms, n, for ice formation from methane hydrate were determined by the Avrami model within each region, and activation energies, E(a), were determined by the Arrhenius plot. E(a) determined from the data for 180-200 K was 42 kJ/mol and for 230-260 K was 22 kJ/mol. The higher E(a) in the colder temperature range was attributed to a difference in the microstructure of ice between the two regions.

Kinetics of Methane Hydrate Decomposition Studied via in Situ Low Temperature X-ray Powder Diffraction

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

Everett, Susan M; Rawn, Claudia J; Keffer, David J.

Gas hydrates are known to have a slowed decomposition rate at ambient pressure and temperatures below the melting point of ice termed self-preservation or anomalous preservation. As hydrate exothermically decomposes, gas is released and water of the clathrate cages transforms into ice. Two regions of slowed decomposition for methane hydrate, 180 200 K and 230 260 K, were observed, and the kinetics were studied by in situ low temperature x-ray powder diffraction. The kinetic constants for ice formation from methane hydrate were determined by the Avrami model within each region and activation energies, Ea, were determined by the Arrhenius plot.more » Ea determined from the data for 180 200 K was 42 kJ/mol and for 230 260 K was 22 kJ/mol. The higher Ea in the colder temperature range was attributed to a difference in the microstructure of ice between the two regions.« less

Effect of cobalt on microstructure and properties of AlCr1.5CuFeNi2Cox high-entropy alloys

NASA Astrophysics Data System (ADS)

Kukshal, Vikas; Patnaik, Amar; Bhat, I. K.

2018-04-01

The present paper investigates the effect of Co addition on the alloying behaviour, microstructure and the resulting properties of cast AlCr1.5CuFeNi2Cox high-entropy alloys intended to be used for high temperature applications. The elements Al, Cr, Cu, Fe, Ni and Co (Purity > 99) weighing approximately 800 g was melted in a high temperature vacuum induction furnace. The microstructure, phase transformation, density, microhardness and compressive strength of the samples were analysed using x-ray diffraction (XRD), scanning electron microscopes (SEM), Vickers microhardness tester and universal Testing machine. The crystalline structure of the alloys exhibits simple FCC and BCC phases. The microstructures investigation of the alloys shows the segregation of copper in the interdendritic region resulting in Cu-rich FCC phase. The addition of Co further enhances the formation of FCC phase resulting in the decrease in micro hardness value of the alloys, which varies from 471 HV to 364 HV with increase in the cobalt content from x = 0 to x = 1 (molar ratio). The similar decreasing trend is also observed for the compressive strength of the alloys.

Self catalytic growth of indium oxide (In2O3) nanowires by resistive thermal evaporation.

PubMed

Kumar, R Rakesh; Rao, K Narasimha; Rajanna, K; Phani, A R

2014-07-01

Self catalytic growth of Indium Oxide (In2O3) nanowires (NWs) have been grown by resistive thermal evaporation of Indium (In) in the presence of oxygen without use of any additional metal catalyst. Nanowires growth took place at low substrate temperature of 370-420 degrees C at an applied current of 180-200 A to the evaporation boat. Morphology, microstructures, and compositional studies of the grown nanowires were performed by employing field emission scanning electron microscopy (FESEM), X-Ray diffraction (XRD), transmission electron microscopy (TEM), energy dispersive X-ray spectroscopy (EDS) and X-ray photoelectron spectroscopy (XPS) respectively. Nanowires were uniformly grown over the entire Si substrate and each of the nanowire is capped with a catalyst particle at their end. X-ray diffraction study reveals the crystalline nature of the grown nanowires. Transmission electron microscopy study on the nanowires further confirmed the single crystalline nature of the nanowires. Energy dispersive X-ray analysis on the nanowires and capped nanoparticle confirmed that Indium act as catalyst for In2O3 nanowires growth. A self catalytic Vapor-Liquid-Solid (VLS) growth mechanism was responsible for the growth of In2O3 nanowires. Effect of oxygen partial pressure variation and variation of applied currents to the evaporation boat on the nanowires growth was systematically studied. These studies concluded that at oxygen partial pressure in the range of 4 x 10(-4), 6 x 10(-4) mbar at applied currents to the evaporation boat of 180-200 A were the best conditions for good nanowires growth. Finally, we observed another mode of VLS growth along with the standard VLS growth mode for In2O3 nanowires similar to the growth mechanism reported for GaAs nanowires.

Inorganic polymers from laterite using activation with phosphoric acid and alkaline sodium silicate solution: Mechanical and microstructural properties

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

Lassinantti Gualtieri, Magdalena, E-mail: magdalena.gualtieri@unimore.it; Romagnoli, Marcello; Pollastri, Simone

2015-01-15

Geopolymers from laterite, an iron-rich soil available in developing countries, have great potential as building materials. In this work, laterite from Togo (Africa) was used to prepare geopolymers using both phosphoric acid and alkaline sodium silicate solution. Microstructural properties were investigated by scanning electron microscopy, X-ray powder diffraction and mercury porosimetry, whereas thermal properties were evaluated by thermal analyses. The local environment of iron was studied by X-ray Absorption Spectroscopy (XANES region). The mechanical properties were determined. Modulus of Rupture and Young's modulus fell in the ranges 3.3–4.5 MPa and 12–33 GPa, respectively, rendering the materials good candidates for constructionmore » purposes. Heating above 900 °C results in weight-gain, presumably due to iron redox reactions. X-ray Absorption Spectroscopy data evidence changes in the chemical and structural environments of iron following thermal treatment of geopolymers. These changes indicate interaction between the geopolymer structure and iron during heating, possibly leading to redox properties. -- Highlights: •Geopolymerization of laterite is promising for fabrication of building materials. •Both phosphoric acid and alkaline sodium silicate solution can be used for activation. •Thermally activated redox properties of the inorganic polymers were observed.« less

Investigation of fatigue crack initiation from a non-metallic inclusion via high energy x-ray diffraction microscopy

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

Naragani, Diwakar; Sangid, Michael D.; Shade, Paul A.

Crack initiation at inclusions is a dominant, unavoidable and life-limiting failure mechanism of important structural materials. Fatigue progresses in a complex manner to find the ‘weakest link’ in the microstructure, leading to crack nucleation. In this study, fully 3-D characterization methods using high-energy synchrotron x-rays are combined with in-situ mechanical testing to study the crack initiation mechanism in a Ni-based superalloy specimen. The specimen was produced via powder metallurgy and seeded with a non-metallic inclusion. Two x-ray techniques were employed: absorption contrast computed micro-tomography (μ-CT) to determine the morphology of the inclusion and its location in the gauge section ofmore » the specimen; and far-field high-energy diffraction microscopy (FF-HEDM) to resolve the centroids, average orientations, and lattice strains of the individual grains comprising the microstructure surrounding the inclusion. Sequential μ-CT and FF-HEDM scans were carried out at both peak and zero applied stress following schedules of cyclic deformation. The µ-CT data showed the onset and location of crack initiation, and the FF-HEDM data provided temporal and spatial evolution of the intergranular strains. Strain partitioning and the associated stress heterogeneities that develop are shown to stabilize within a few loading cycles. Elasto-viscoplastic fast Fourier transform simulations were utilized to supplement interpretation of the experimental stress distributions and compared with the experimental stress distributions. In conclusion, appropriate conditions for crack nucleation in the form of stress gradients were demonstrated and created by virtue of the inclusion, specifically the residual stress state and local bonding state at the inclusion-matrix interface.« less

Investigation of fatigue crack initiation from a non-metallic inclusion via high energy x-ray diffraction microscopy

DOE PAGES

Naragani, Diwakar; Sangid, Michael D.; Shade, Paul A.; ...

2017-07-14

Crack initiation at inclusions is a dominant, unavoidable and life-limiting failure mechanism of important structural materials. Fatigue progresses in a complex manner to find the ‘weakest link’ in the microstructure, leading to crack nucleation. In this study, fully 3-D characterization methods using high-energy synchrotron x-rays are combined with in-situ mechanical testing to study the crack initiation mechanism in a Ni-based superalloy specimen. The specimen was produced via powder metallurgy and seeded with a non-metallic inclusion. Two x-ray techniques were employed: absorption contrast computed micro-tomography (μ-CT) to determine the morphology of the inclusion and its location in the gauge section ofmore » the specimen; and far-field high-energy diffraction microscopy (FF-HEDM) to resolve the centroids, average orientations, and lattice strains of the individual grains comprising the microstructure surrounding the inclusion. Sequential μ-CT and FF-HEDM scans were carried out at both peak and zero applied stress following schedules of cyclic deformation. The µ-CT data showed the onset and location of crack initiation, and the FF-HEDM data provided temporal and spatial evolution of the intergranular strains. Strain partitioning and the associated stress heterogeneities that develop are shown to stabilize within a few loading cycles. Elasto-viscoplastic fast Fourier transform simulations were utilized to supplement interpretation of the experimental stress distributions and compared with the experimental stress distributions. In conclusion, appropriate conditions for crack nucleation in the form of stress gradients were demonstrated and created by virtue of the inclusion, specifically the residual stress state and local bonding state at the inclusion-matrix interface.« less

Graphene nanoplate-MnO2 composites for supercapacitors: a controllable oxidation approach.

PubMed

Huang, Huajie; Wang, Xin

2011-08-01

Graphene nanoplate-MnO(2) composites have been synthesized by oxidising part of the carbon atoms in the framework of graphene nanoplates at ambient temperature. The composites were characterized by means of X-ray diffraction (XRD), Raman spectroscopy, scanning electron microscopy (SEM), transmission electron microscopy (TEM), X-ray photoelectron spectroscopy (XPS) and cyclic voltammetry (CV). It was found that the oxidation extent of the carbon atoms in the graphene framework in these composites was dependent on the reaction time, which also influenced their microstructure, morphology and electrochemical properties. Compared with MnO(2) nanolamellas, the nanocomposite prepared with a reaction time of 3 h reveals better electrochemical properties as a supercapacitor electrode material. This journal is © The Royal Society of Chemistry 2011

Preparation and electrical properties of electrospun tin-doped indium oxide nanowires

NASA Astrophysics Data System (ADS)

Lin, Dandan; Wu, Hui; Zhang, Rui; Pan, Wei

2007-11-01

Well-aligned tin-doped indium (ITO) nanowires have been prepared using the electrospinning process. The Sn doping mechanism and microstructure have been characterized by x-ray diffraction (XRD) and x-ray photoelectron spectroscopy (XPS). Devices for I-V measurement and field-effect transistors (FETs) were assembled using ITO nanowires with top contact configurations. The effect of Sn doping on the electrical conductivity was significant in that it enhanced the conductance by over 107 times, up to ~1 S cm-1 for ITO nanowires with an Sn content of 17.5 at.%. The nanowire FETs were operated in the depletion mode with an electron mobility of up to 0.45 cm2 V-1 s-1 and an on/off ratio of 103.

Characterizing the Nano and Micro Structure of Concrete toImprove its Durability

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

Monteiro, P.J.M.; Kirchheim, A.P.; Chae, S.

2009-01-13

New and advanced methodologies have been developed to characterize the nano and microstructure of cement paste and concrete exposed to aggressive environments. High resolution full-field soft X-ray imaging in the water window is providing new insight on the nano scale of the cement hydration process, which leads to a nano-optimization of cement-based systems. Hard X-ray microtomography images of ice inside cement paste and cracking caused by the alkali?silica reaction (ASR) enables three-dimensional structural identification. The potential of neutron diffraction to determine reactive aggregates by measuring their residual strains and preferred orientation is studied. Results of experiments using these tools aremore » shown on this paper.« less

Characterizing the nano and micro structure of concrete to improve its durability

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

Monteiro, P.J.M.; Kirchheim, A.P.; Chae, S.

2008-10-22

New and advanced methodologies have been developed to characterize the nano and microstructure of cement paste and concrete exposed to aggressive environments. High resolution full-field soft X-ray imaging in the water window is providing new insight on the nano scale of the cement hydration process, which leads to a nano-optimization of cement-based systems. Hard X-ray microtomography images on ice inside cement paste and cracking caused by the alkali-silica reaction (ASR) enables three-dimensional structural identification. The potential of neutron diffraction to determine reactive aggregates by measuring their residual strains and preferred orientation is studied. Results of experiments using these tools willmore » be shown on this paper.« less

X-Ray Diffraction Apparatus

NASA Technical Reports Server (NTRS)

Blake, David F. (Inventor); Bryson, Charles (Inventor); Freund, Friedmann (Inventor)

1996-01-01

An x-ray diffraction apparatus for use in analyzing the x-ray diffraction pattern of a sample is introduced. The apparatus includes a beam source for generating a collimated x-ray beam having one or more discrete x-ray energies, a holder for holding the sample to be analyzed in the path of the beam, and a charge-coupled device having an array of pixels for detecting, in one or more selected photon energy ranges, x-ray diffraction photons produced by irradiating such a sample with said beam. The CCD is coupled to an output unit which receives input information relating to the energies of photons striking each pixel in the CCD, and constructs the diffraction pattern of photons within a selected energy range striking the CCD.

The Microstructure and Properties of Super Martensitic Stainless Steel Microalloyed with Tungsten and Copper

NASA Astrophysics Data System (ADS)

Ye, Dong; Li, Jun; Liu, Yu-Rong; Yong, Qi-Long; Su, Jie; Cao, Jian-Chun; Tao, Jing-Mei; Zhao, Kun-Yu

2011-06-01

The microstructure and properties of super martensitic stainless steel (SMSS) microalloyed with tungsten and copper were studied by means of optical microscopy, dilatometer, X-ray diffraction, and tensile tests. The results showed that the microstructure of SMSS, after quenching and tempering, was a typical biphase structure with tempered martensite and reversed austenite dispersedly distributed in the martensite matrix. W and Cu were added into the SMSS to reduce the transformation temperature (Ms) and improve the strength and hardness of the matrix by grain refining and solid solution strengthening. Thermocalc calculations confirmed that M23C6 compound and Laves phase were precipitated during tempering in the investigated steel. Compared with the traditional SMSS, the steel microalloyed with W and Cu performed better mechanical properties.

Effect of sodium monofluorophosphate treatment on microstructure and frost salt scaling durability of slag cement paste

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

Copuroglu, O.; Fraaij, A.L.A.; Bijen, J.M.J.M.

2006-08-15

Sodium-monofluorophosphate (Na-MFP) is currently in use as a surface applied corrosion inhibitor in the concrete industry. Its basic mechanism is to protect the passive layer of the reinforcement steel against disruption due to carbonation. Carbonation is known as the most detrimental environmental effect on blast furnace slag cement (BFSC) concrete with respect to frost salt scaling. In this paper the effect of Na-MFP on the microstructure and frost salt scaling resistance of carbonated BFSC paste is presented. The results of electron microscopy, mercury intrusion porosimetry (MIP) and X-ray diffraction (XRD) are discussed. It is found that the treatment modifies themore » microstructure and improves the resistance of carbonated BFSC paste against frost salt attack.« less

Effect of 0.2 and 0.5% Ti on the microstructure and mechanical properties of 13Cr supermartensitic stainless steel

NASA Astrophysics Data System (ADS)

Lian, Yong; Huang, Jinfeng; Zhang, Jin; Zhang, Cheng; Gao, Wen; Zhao, Chao

2015-11-01

The effect that a 0, 0.2, and 0.5 wt.% titanium content has on the microstructure and mechanical properties of 13Cr supermartensitic stainless steel was investigated using an optical microscope, transmission electron microscope, and X-ray diffraction. The resultant microstructures of the three steels were tempered martensite with a reversed austenite dispersed throughout the matrix. Additionally, the formation of Cr-rich carbides was suppressed by stable Ti(C, N), which improved the strength without severely decreasing in the Ti-microalloyed steel toughness. Nano-precipitation of Ni3Ti was found for the 0.5 wt.% Ti steel during tempering, which significantly increased the strength, but decreased the toughness. The reversed austenite volume fraction also significantly influenced the mechanical properties.

An x-ray diffraction study of microstructural deformation induced by cyclic loading of selected steels

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

Fourspring, P.M.; Pangborn, R.N.

1996-06-01

X-ray double crystal diffractometry (XRDCD) was used to assess cyclic microstructural deformation in a face centered cubic (fcc) steel (AISI304) and a body centered cubic (bcc) steel (SA508 class 2). The first objective of the investigation was to determine if XRDCD could be used to effectively monitor cyclic microstructural deformation in polycrystalline Fe alloys. A second objective was to study the microstructural deformation induced by cyclic loading of polycrystalline Fe alloys. The approach used in the investigation was to induce fatigue damage in a material and to characterize the resulting microstructural deformation at discrete fractions of the fatigue life ofmore » the material. Also, characterization of microstructural deformation was carried out to identify differences in the accumulation of damage from the surface to the bulk, focusing on the following three regions: near surface (0--10 {micro}m), subsurface (10--300 {micro}m), and bulk. Characterization of the subsurface region was performed only on the AISI304 material because of the limited availability of the SA508 material. The results from the XRDCD data indicate a measurable change induced by fatigue from the initial state to subsequent states of both the AISI304 and the SA508 materials. Therefore, the XRDCD technique was shown to be sensitive to the microstructural deformation caused by fatigue in steels; thus, the technique can be used to monitor fatigue damage in steels. In addition, for the AISI304 material, the level of cyclic microstructural deformation in the bulk material was found to be greater than the level in the near surface material. In contrast, previous investigations have shown that the deformation is greater in the near surface than the bulk for Al alloys and bcc Fe alloys.« less

Real-time X-ray Diffraction: Applications to Materials Characterization

NASA Technical Reports Server (NTRS)

Rosemeier, R. G.

1984-01-01

With the high speed growth of materials it becomes necessary to develop measuring systems which also have the capabilities of characterizing these materials at high speeds. One of the conventional techniques of characterizing materials was X-ray diffraction. Film, which is the oldest method of recording the X-ray diffraction phenomenon, is not quite adequate in most circumstances to record fast changing events. Even though conventional proportional counters and scintillation counters can provide the speed necessary to record these changing events, they lack the ability to provide image information which may be important in some types of experiment or production arrangements. A selected number of novel applications of using X-ray diffraction to characterize materials in real-time are discussed. Also, device characteristics of some X-ray intensifiers useful in instantaneous X-ray diffraction applications briefly presented. Real-time X-ray diffraction experiments with the incorporation of image X-ray intensification add a new dimension in the characterization of materials. The uses of real-time image intensification in laboratory and production arrangements are quite unlimited and their application depends more upon the ingenuity of the scientist or engineer.

Radiation damage free ghost diffraction with atomic resolution

DOE PAGES

Li, Zheng; Medvedev, Nikita; Chapman, Henry N.; ...

2017-12-21

The x-ray free electron lasers can enable diffractive structural determination of protein nanocrystals and single molecules that are too small and radiation-sensitive for conventional x-ray diffraction. However the electronic form factor may be modified during the ultrashort x-ray pulse due to photoionization and electron cascade caused by the intense x-ray pulse. For general x-ray imaging techniques, the minimization of the effects of radiation damage is of major concern to ensure reliable reconstruction of molecular structure. Here in this paper, we show that radiation damage free diffraction can be achieved with atomic spatial resolution by using x-ray parametric down-conversion and ghostmore » diffraction with entangled photons of x-ray and optical frequencies. We show that the formation of the diffraction patterns satisfies a condition analogous to the Bragg equation, with a resolution that can be as fine as the crystal lattice length scale of several Ångstrom. Since the samples are illuminated by low energy optical photons, they can be free of radiation damage.« less

Radiation damage free ghost diffraction with atomic resolution

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

Li, Zheng; Medvedev, Nikita; Chapman, Henry N.

The x-ray free electron lasers can enable diffractive structural determination of protein nanocrystals and single molecules that are too small and radiation-sensitive for conventional x-ray diffraction. However the electronic form factor may be modified during the ultrashort x-ray pulse due to photoionization and electron cascade caused by the intense x-ray pulse. For general x-ray imaging techniques, the minimization of the effects of radiation damage is of major concern to ensure reliable reconstruction of molecular structure. Here in this paper, we show that radiation damage free diffraction can be achieved with atomic spatial resolution by using x-ray parametric down-conversion and ghostmore » diffraction with entangled photons of x-ray and optical frequencies. We show that the formation of the diffraction patterns satisfies a condition analogous to the Bragg equation, with a resolution that can be as fine as the crystal lattice length scale of several Ångstrom. Since the samples are illuminated by low energy optical photons, they can be free of radiation damage.« less

Synchrotron Radiation X-ray Diffraction Techniques Applied to Insect Flight Muscle.

PubMed

Iwamoto, Hiroyuki

2018-06-13

X-ray fiber diffraction is a powerful tool used for investigating the molecular structure of muscle and its dynamics during contraction. This technique has been successfully applied not only to skeletal and cardiac muscles of vertebrates but also to insect flight muscle. Generally, insect flight muscle has a highly ordered structure and is often capable of high-frequency oscillations. The X-ray diffraction studies on muscle have been accelerated by the advent of 3rd-generation synchrotron radiation facilities, which can generate brilliant and highly oriented X-ray beams. This review focuses on some of the novel experiments done on insect flight muscle by using synchrotron radiation X-rays. These include diffraction recordings from single myofibrils within a flight muscle fiber by using X-ray microbeams and high-speed diffraction recordings from the flight muscle during the wing-beat of live insects. These experiments have provided information about the molecular structure and dynamic function of flight muscle in unprecedented detail. Future directions of X-ray diffraction studies on muscle are also discussed.

Effects of Nb Modification and Cooling Rate on the Microstructure in an Ultrahigh Carbon Steel

NASA Astrophysics Data System (ADS)

Hecht, Matthew D.; Webler, Bryan A.; Picard, Yoosuf N.

2018-04-01

In this study, two different melting methods were used to investigate effects of Nb modification on microstructure in ultrahigh carbon steel (UHCS). Nb-free and Nb-modified UHCS samples were produced by melting and resolidifying an industrially produced base UHCS with and without addition of Nb powder. Microstructure was characterized using scanning electron microscopy, X-ray diffraction, and electron dispersive spectroscopy. Equilibrium computations of phase fractions and compositions were utilized to help describe microstructural changes caused by the Nb additions. Nb combined with C to form NbC structures before and during austenite solidification, reducing the effective amount of carbon available for the other phases. Cementite network spacing in the Nb-free samples was controlled by the cooling rate during solidification (faster cooling led to a more refined network). Network spacing in the Nb-modified UHCS could be enlarged by NbC structures that formed cooperatively with austenite.

The influence of sintering temperature on microstructure and mechanical properties of Ni-Al intermetallics fabricated by SPS

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

Thömmes, A., E-mail: thoemmes.alexander@gmail.com; Shevtsova, L. I., E-mail: edeliya2010@mail.ru; Laptev, I. S., E-mail: ilya-laptev-nstu@mail.ru

2015-10-27

In the present study PN85Yu15 was used as elemental powder to produce a sintered compound with Ni3Al as main phase. The Spark Plasma Sintering (SPS) technique is used to compact the powders. The powder was sintered in a temperature range between 1000°C and 1150°C to observe the influence of the sintering temperature on the microstructure and the mechanical properties. The microstructure was observed with optical microscope (OM), the phase composition was characterized by X-ray diffraction (XRD) technique. Density and microhardness were observed and compared the values with the results of other researchers. The compressive-, density- and microhardness tests show asmore » clear result that with increasing the sintering temperature nearly all properties become better and also the microstructure studies show that porous places become less.« less

Sintering and microstructure of silicon carbide ceramic with Y3Al5O12 added by sol-gel method*

PubMed Central

Guo, Xing-zhong; Yang, Hui

2005-01-01

Silicon carbide (SiC) ceramic with YAG (Y3Al5O12) additive added by sol-gel method was liquid-phase sintered at different sintering temperatures, and the sintering mechanism and microstructural characteristics of resulting silicon carbide ceramics were analyzed by X-ray diffraction (XRD), scanning electron microscopy (SEM) and elemental distribution of surface (EDS). YAG (yttrium aluminum garnet) phase formed before the sintering and its uniform distribution in the SiC/YAG composite powder decreased the sintering temperature and improved the densification of SiC ceramic. The suitable sintering temperature was 1860 °C with the specimen sintered at this temperature having superior sintering and mechanical properties, smaller crystal size and fewer microstructure defects. Three characteristics of improved toughness of SiC ceramic with YAG added by sol-gel method were microstructural densification, main-crack deflection and crystal ‘bridging’. PMID:15682507

Effect of Quenching Process on the Microstructure and Hardness of High-Carbon Martensitic Stainless Steel

NASA Astrophysics Data System (ADS)

Zhu, Qin-tian; Li, Jing; Shi, Cheng-bin; Yu, Wen-tao

2015-11-01

The microstructure and hardness of high-carbon martensitic stainless steel (HMSS) were investigated using thermal expansion analyzer, Thermo-calc, scanning electron microscope, x-ray diffraction, and Ultra-high temperature confocal microscope. The results indicate that the experimental steel should be austenitized in the temperature range of 1025-1075 °C, which can give a maximum hardness of 62 HRc with the microstructure consisting of martensite, retained austenite, and some undissolved carbides. With increasing austenitizing temperature, the amount of retained austenite increases, while the volume fraction of carbides increases first and then decreases. The starting temperature and finish temperature of martensite formation decrease with increasing cooling rates. Air-quenched samples can obtain less retained austenite, more compact microstructure, and higher hardness, compared with that of oil-quenched samples. For HMSS, the martensitic transformation takes place at some isolated areas with a slow nucleation rate.

Effects of Nb Modification and Cooling Rate on the Microstructure in an Ultrahigh Carbon Steel

NASA Astrophysics Data System (ADS)

Hecht, Matthew D.; Webler, Bryan A.; Picard, Yoosuf N.

2018-06-01

In this study, two different melting methods were used to investigate effects of Nb modification on microstructure in ultrahigh carbon steel (UHCS). Nb-free and Nb-modified UHCS samples were produced by melting and resolidifying an industrially produced base UHCS with and without addition of Nb powder. Microstructure was characterized using scanning electron microscopy, X-ray diffraction, and electron dispersive spectroscopy. Equilibrium computations of phase fractions and compositions were utilized to help describe microstructural changes caused by the Nb additions. Nb combined with C to form NbC structures before and during austenite solidification, reducing the effective amount of carbon available for the other phases. Cementite network spacing in the Nb-free samples was controlled by the cooling rate during solidification (faster cooling led to a more refined network). Network spacing in the Nb-modified UHCS could be enlarged by NbC structures that formed cooperatively with austenite.

Electromagnetic nondestructive evaluation of tempering process in AISI D2 tool steel

NASA Astrophysics Data System (ADS)

Kahrobaee, Saeed; Kashefi, Mehrdad

2015-05-01

The present paper investigates the potential of using eddy current technique as a reliable nondestructive tool to detect microstructural changes during the different stages of tempering treatment in AISI D2 tool steel. Five stages occur in tempering of the steel: precipitation of ɛ carbides, formation of cementite, retained austenite decomposition, secondary hardening effect and spheroidization of carbides. These stages were characterized by destructive methods, including dilatometry, differential scanning calorimetry, X-ray diffraction, scanning electron microscopic observations, and hardness measurements. The microstructural changes alter the electrical resistivity/magnetic saturation, which, in turn, influence the eddy current signals. Two EC parameters, induced voltage sensed by pickup coil and impedance point detected by excitation coil, were evaluated as a function of tempering temperature to characterize the microstructural features, nondestructively. The study revealed that a good correlation exists between the EC parameters and the microstructural changes.

Microstructure-related properties of magnesium fluoride films at 193nm by oblique-angle deposition.

PubMed

Guo, Chun; Kong, Mingdong; Lin, Dawei; Liu, Cunding; Li, Bincheng

2013-01-14

Magnesium fluoride (MgF2) films deposited by resistive heating evaporation with oblique-angle deposition have been investigated in details. The optical and micro-structural properties of single-layer MgF2 films were characterized by UV-VIS and FTIR spectrophotometers, scanning electron microscope (SEM), atomic force microscope (AFM), and x-ray diffraction (XRD), respectively. The dependences of the optical and micro-structural parameters of the thin films on the deposition angle were analyzed. It was found that the MgF2 film in a columnar microstructure was negatively inhomogeneous of refractive index and polycrystalline. As the deposition angle increased, the optical loss, extinction coefficient, root-mean-square (rms) roughness, dislocation density and columnar angle of the MgF2 films increased, while the refractive index, packing density and grain size decreased. Furthermore, IR absorption of the MgF2 films depended on the columnar structured growth.

Microstructural modification of pure Mg for improving mechanical and biocorrosion properties.

PubMed

Ahmadkhaniha, D; Järvenpää, A; Jaskari, M; Sohi, M Heydarzadeh; Zarei-Hanzaki, A; Fedel, M; Deflorian, F; Karjalainen, L P

2016-08-01

In this study, the effect of microstructural modification on mechanical properties and biocorrosion resistance of pure Mg was investigated for tailoring a load-bearing orthopedic biodegradable implant material. This was performed utilizing the friction stir processing (FSP) in 1-3 passes to refine the grain size. Microstructure was examined in an optical microscope and scanning electron microscope with an electron backscatter diffraction unit. X-ray diffraction method was used to identify the texture. Mechanical properties were measured by microhardness and tensile testing. Electrochemical impedance spectroscopy was applied to evaluate corrosion behavior. The results indicate that even applying a single pass of FSP refined the grain size significantly. Increasing the number of FSP passes further refined the structure, increased the mechanical strength and intensified the dominating basal texture. The best combination of mechanical properties and corrosion resistance were achieved after three FSP passes. In this case, the yield strength was about six times higher than that of the as-cast Mg and the corrosion resistance was also improved compared to that in the as-cast condition. Copyright © 2016 Elsevier Ltd. All rights reserved.

Influence of Applied Voltage and Film-Formation Time on Microstructure and Corrosion Resistance of Coatings Formed on Mg-Zn-Zr-Ca Bio-magnesium Alloy

NASA Astrophysics Data System (ADS)

Yandong, Yu; Shuzhen, Kuang; Jie, Li

2015-09-01

The influence of applied voltage and film-formation time on the microstructure and corrosion resistance of coatings formed on a Mg-Zn-Zr-Ca novel bio-magnesium alloy has been investigated by micro-arc oxidation (MAO) treatment. Phase composition and microstructure of as-coated samples were analyzed by the x-ray diffraction, energy dispersive x-ray spectroscopy and scanning electron microscopy. And the porosity and average of micro-pore aperture of the surface on ceramic coatings were analyzed by general image software. Corrosion microstructure of as-coated samples was caught by a microscope digital camera. The long-term corrosion resistance of as-coated samples was tested in simulated body fluid for 30 days. The results showed that the milky white smooth ceramic coating formed on the Mg-Zn-Zr-Ca novel bio-magnesium alloy was a compound of MgO, Mg2SiO4 and MgSiO3, and its corrosion resistance was significantly improved compared with that of the magnesium substrate. In addition, when the MAO applied voltage were 450 V and 500 V and film-formation time were 9 min and 11 min, the surface micro-morphology and the corrosion resistance of as-coated samples were relatively improved. The results provided a theoretical foundation for the application of the Mg-Zn-Zr-Ca novel bio-magnesium alloy in biomedicine.

Combining experiment and optical simulation in coherent X-ray nanobeam characterization of Si/SiGe semiconductor heterostructures

DOE PAGES

Tilka, J. A.; Park, J.; Ahn, Y.; ...

2016-07-06

Here, the highly coherent and tightly focused x-ray beams produced by hard x-ray light sources enable the nanoscale characterization of the structure of electronic materials but are accompanied by significant challenges in the interpretation of diffraction and scattering patterns. X-ray nanobeams exhibit optical coherence combined with a large angular divergence introduced by the x-ray focusing optics. The scattering of nanofocused x-ray beams from intricate semiconductor heterostructures produces a complex distribution of scattered intensity. We report here an extension of coherent xray optical simulations of convergent x-ray beam diffraction patterns to arbitrary x-ray incident angles to allow the nanobeam diffraction patternsmore » of complex heterostructures to be simulated faithfully. These methods are used to extract the misorientation of lattice planes and the strain of individual layers from synchrotron x-ray nanobeam diffraction patterns of Si/SiGe heterostructures relevant to applications in quantum electronic devices. The systematic interpretation of nanobeam diffraction patterns from semiconductor heterostructures presents a new opportunity in characterizing and ultimately designing electronic materials.« less

Characterization of morphology and hydration products of high-volume fly ash paste by monochromatic scanning x-ray micro-diffraction (μ-SXRD)

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

Bae, Sungchul; Meral, Cagla; Department of Civil Engineering, Middle East Technical University, 06800 Ankara

2014-05-01

The present study focuses on identification and micro-structural characterization of the hydration products formed in high-volume fly ash (HVFA)/portland cement (PC) systems using monochromatic scanning x-ray micro-diffraction (μ-SXRD) and SEM-EDS. Pastes with up to 80% fly ash replacement were studied. Phase maps for HVFA samples using μ-SXRD patterns prove that μ-SXRD is an effective method to identify and visualize the distribution of phases in the matrix. μ-SXRD and SEM-EDS analysis shows that the C-S-H formed in HVFA system containing 50% or more of fly ash has a similar structure as C-S-H(I) with comparatively lower Ca/Si ratio than the one producedmore » in PC system. Moreover, coexistence of C-S-H(I) and strätlingite is observed in the system containing 80% of fly ash, confirming that the amount of alumina and silicate phases provided by the fly ash is a major factor for the formation of C-S-H(I) and strätlingite in HVFA system. - Highlights: • High-volume fly ash (HVFA) paste was studied by scanning x-ray micro-diffraction. • Coexistence of C-S-H(I) and strätlingite in the HVFA system is clearly shown. • The distribution of minor phases in the HVFA system is shown. • Differences between inner and outer products of fly ash are observed by SEM-EDS.« less

Effect of process parameters on microstructure and mechanical properties of friction stir welded joints: A review

NASA Astrophysics Data System (ADS)

Wanare, S. P.; Kalyankar, V. D.

2018-04-01

Friction stir welding is emerging as a promising technique for joining of lighter metal alloys due to its several advantages over conventional fusion welding processes such as low thermal distortion, good mechanical properties, fine weld joint microstructure, etc. This review article mainly focuses on analysis of microstructure and mechanical properties of friction stir welded joints. Various microstructure characterization techniques used by previous researchers such as optical microscopes, x-ray diffraction, electron probe microscope, transmission electron microscope, scanning electron microscopes with electron back scattered diffraction, electron dispersive microscopy, etc. are thoroughly overviewed and their results are discussed. The effects of friction stir welding process parameters such as tool rotational speed, welding speed, tool plunge depth, axial force, tool shoulder diameter to tool pin diameter ratio, tool geometry etc. on microstructure and mechanical properties of welded joints are studied and critical observations are noted down. The microstructure examination carried out by previous researchers on various zones of welded joints such as weld zone, heat affected zone and base metal are studied and critical remarks have been presented. Mechanical performances of friction stir welded joints based on tensile test, micro-hardness test, etc. are discussed. This article includes exhaustive literature review of standard research articles which may become ready information for subsequent researchers to establish their line of action.

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

Fabrication and testing of a newly designed slit system for depth-resolved X-ray diffraction measurements

DOE PAGES

Sinsheimer, John; Bouet, Nathalie; Ghose, Sanjit; ...

2016-10-06

A new system of slits called `spiderweb slits' have been developed for depth-resolved powder or polycrystalline X-ray diffraction measurements. The slits act on diffracted X-rays to select a particular gauge volume of sample, while absorbing diffracted X-rays from outside of this volume. Although the slit geometry is to some extent similar to that of previously developed conical slits or spiral slits, this new design has advantages over the previous ones in use for complex heterogeneous materials and in situ and operando diffraction measurements. For example, the slits can measure a majority of any diffraction cone for any polycrystalline material, overmore » a continuous range of diffraction angles, and work for X-ray energies of tens to hundreds of kiloelectronvolts. In addition, the design is generated and optimized using ray-tracing simulations, and fabricated through laser micromachining. The first prototype was successfully tested at the X17A beamline at the National Synchrotron Light Source, and shows similar performance to simulations, demonstrating gauge volume selection for standard powders, for all diffraction peaks over angles of 2–10°. A similar, but improved, design will be implemented at the X-ray Powder Diffraction beamline at the National Synchrotron Light Source II.« less

Structural, vibrational and luminescence properties of the (1−x)CaWO{sub 4}−xCdWO{sub 4} system

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

Taoufyq, A.; Laboratoire Matériaux et Environnement LME, Faculté des Sciences, Université Ibn Zohr, BP 8106, Cité Dakhla, Agadir, Maroc; CEA/DEN, Département d’Études des Réacteurs, Laboratoire Dosimétrie Capteurs Instrumentation, CEA Cadarache, 13108, Saint-Paul-lez-Durance

2014-11-15

In the present work, we investigate the structural, microstructural, vibrational and luminescence properties of the system (1−x)CaWO{sub 4}−xCdWO{sub 4} with x ranging between 0 and 1. Polycrystalline samples were elaborated using a coprecipitation technique followed by thermal treatment at 1000 °C. The samples were then characterized using X-ray diffraction, scanning electron microscopy, Raman spectroscopy and luminescence analyses. X-ray diffraction profile analyses using Rietveld method showed that two kinds of solid solutions Ca{sub 1−x}Cd{sub x}WO{sub 4} having scheelite and wolframite structures, with respectively tetragonal and monoclinic crystal cells, were observed, with a biphasic system for compositions x=0.6 and 0.7. The scanningmore » electron microscopy experiments showed a complex evolution of morphologies and crystallite sizes as x increased. The vibration modes of Raman spectra were characteristic of composition-dependent disordered solid solutions with decreasing wavenumbers as x increased. Luminescence experiments were performed under UV-laser light irradiation. The energies of emission bands increased linearly with cadmium composition x. The integrated intensity of luminescence reached a maximum value for the substituted wolframite phase with composition x=0.8. - Graphical abstract: Luminescence on UV excitation (364.5 nm) of (1−x)CaWO{sub 4−x}CdWO{sub 4} system, elaborated from coprecipitation technique at 1000 °C, with 0« less

Dynamical scattering in coherent hard x-ray nanobeam Bragg diffraction

NASA Astrophysics Data System (ADS)

Pateras, A.; Park, J.; Ahn, Y.; Tilka, J. A.; Holt, M. V.; Kim, H.; Mawst, L. J.; Evans, P. G.

2018-06-01

Unique intensity features arising from dynamical diffraction arise in coherent x-ray nanobeam diffraction patterns of crystals having thicknesses larger than the x-ray extinction depth or exhibiting combinations of nanoscale and mesoscale features. We demonstrate that dynamical scattering effects can be accurately predicted using an optical model combined with the Darwin theory of dynamical x-ray diffraction. The model includes the highly divergent coherent x-ray nanobeams produced by Fresnel zone plate focusing optics and accounts for primary extinction, multiple scattering, and absorption. The simulation accurately reproduces the dynamical scattering features of experimental diffraction patterns acquired from a GaAs/AlGaAs epitaxial heterostructure on a GaAs (001) substrate.

Coherent x-ray diffraction imaging with nanofocused illumination.

PubMed

Schroer, C G; Boye, P; Feldkamp, J M; Patommel, J; Schropp, A; Schwab, A; Stephan, S; Burghammer, M; Schöder, S; Riekel, C

2008-08-29

Coherent x-ray diffraction imaging is an x-ray microscopy technique with the potential of reaching spatial resolutions well beyond the diffraction limits of x-ray microscopes based on optics. However, the available coherent dose at modern x-ray sources is limited, setting practical bounds on the spatial resolution of the technique. By focusing the available coherent flux onto the sample, the spatial resolution can be improved for radiation-hard specimens. A small gold particle (size <100 nm) was illuminated with a hard x-ray nanobeam (E=15.25 keV, beam dimensions approximately 100 x 100 nm2) and is reconstructed from its coherent diffraction pattern. A resolution of about 5 nm is achieved in 600 s exposure time.

DynAMITe: a prototype large area CMOS APS for breast cancer diagnosis using x-ray diffraction measurements

NASA Astrophysics Data System (ADS)

Konstantinidis, A.; Anaxagoras, T.; Esposito, M.; Allinson, N.; Speller, R.

2012-03-01

X-ray diffraction studies are used to identify specific materials. Several laboratory-based x-ray diffraction studies were made for breast cancer diagnosis. Ideally a large area, low noise, linear and wide dynamic range digital x-ray detector is required to perform x-ray diffraction measurements. Recently, digital detectors based on Complementary Metal-Oxide- Semiconductor (CMOS) Active Pixel Sensor (APS) technology have been used in x-ray diffraction studies. Two APS detectors, namely Vanilla and Large Area Sensor (LAS), were developed by the Multidimensional Integrated Intelligent Imaging (MI-3) consortium to cover a range of scientific applications including x-ray diffraction. The MI-3 Plus consortium developed a novel large area APS, named as Dynamically Adjustable Medical Imaging Technology (DynAMITe), to combine the key characteristics of Vanilla and LAS with a number of extra features. The active area (12.8 × 13.1 cm2) of DynaMITe offers the ability of angle dispersive x-ray diffraction (ADXRD). The current study demonstrates the feasibility of using DynaMITe for breast cancer diagnosis by identifying six breast-equivalent plastics. Further work will be done to optimize the system in order to perform ADXRD for identification of suspicious areas of breast tissue following a conventional mammogram taken with the same sensor.

Structural studies on carbon materials for advanced space technology. Part 1: Structure and oxidation behavior of some carbon/carbon composite materials

NASA Technical Reports Server (NTRS)

Fischbach, D. B.; Uptegrove, D. R.; Srinivasagopalan, S.

1974-01-01

The microstructure and some microstructural effects of oxidation have been investigated for laminar carbon fiber cloth/cloth binder matrix composite materials. It was found that cloth wave is important in determining the macrostructure of the composites X-ray diffraction analysis showed that the composites were more graphitic than the constituent fiber phases, indicating a graphitic binder matrix phase. Various tests which were conducted to investigate specific properties of the material are described. It was learned that under the moderate temperature and oxidant flow conditions studied, C-700, 730 materials exhibit superior oxidation resistance primarily because of the inhibiting influence of the graphitized binder matrix.

Resolution enhancement in coherent x-ray diffraction imaging by overcoming instrumental noise.

PubMed

Kim, Chan; Kim, Yoonhee; Song, Changyong; Kim, Sang Soo; Kim, Sunam; Kang, Hyon Chol; Hwu, Yeukuang; Tsuei, Ku-Ding; Liang, Keng San; Noh, Do Young

2014-11-17

We report that reference objects, strong scatterers neighboring weak phase objects, enhance the phase retrieval and spatial resolution in coherent x-ray diffraction imaging (CDI). A CDI experiment with Au nano-particles exhibited that the reference objects amplified the signal-to-noise ratio in the diffraction intensity at large diffraction angles, which significantly enhanced the image resolution. The interference between the diffracted x-ray from reference objects and a specimen also improved the retrieval of the phase of the diffraction signal. The enhancement was applied to image NiO nano-particles and a mitochondrion and confirmed in a simulation with a bacteria phantom. We expect that the proposed method will be of great help in imaging weakly scattering soft matters using coherent x-ray sources including x-ray free electron lasers.

Low Conductive Thermal Barrier Coatings Produced by Ion Beam Assisted EB-PVD with Controlled Porosity, Microstructure Refinement and Alloying Additions for High Temperature Applications

NASA Technical Reports Server (NTRS)

Wolfe, Douglas E.; Singh, Jogender

2005-01-01

Various advanced Hafnia-based thermal barrier coatings (TBC) were applied on nickel-based superalloy coupons by electron beam physical vapor deposition. In addition, microstructural modifications to the coating material were made in an effort to reduce the thermal conductivity of the coating materials. Various processing parameters and coating system modifications were made in order to deposit the alloyed TBC with the desired microstructure and thus coating performance, some of which include applying coatings at substrate temperatures of 1150 C on both PtAl and CoNiCrAlY bond coated samples, as well as using 8YSZ as a bond layer. In addition, various characterization techniques including thermal cyclic tests, scanning electron microscopy, x-ray diffraction, thermal conductivity, and reflectivity measurements were performed. Although the coating microstructure was never fully optimized due to funding being cut short, significant reductions in thermal conductivity were accomplished through both chemistry changes (composition) and microstructural modifications.

Fabrication and testing of a newly designed slit system for depth-resolved X-ray diffraction measurements

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

Sinsheimer, John; Bouet, Nathalie; Ghose, Sanjit

2016-10-06

A new system of slits called `spiderweb slits' have been developed for depth-resolved powder or polycrystalline X-ray diffraction measurements. The slits act on diffracted X-rays to select a particular gauge volume of sample, while absorbing diffracted X-rays from outside of this volume. Although the slit geometry is to some extent similar to that of previously developed conical slits or spiral slits, this new design has advantages over the previous ones in use for complex heterogeneous materials andin situandoperandodiffraction measurements. For example, the slits can measure a majority of any diffraction cone for any polycrystalline material, over a continuous range ofmore » diffraction angles, and work for X-ray energies of tens to hundreds of kiloelectronvolts. The design is generated and optimized using ray-tracing simulations, and fabricated through laser micromachining. The first prototype was successfully tested at the X17A beamline at the National Synchrotron Light Source, and shows similar performance to simulations, demonstrating gauge volume selection for standard powders, for all diffraction peaks over angles of 2–10°. A similar, but improved, design will be implemented at the X-ray Powder Diffraction beamline at the National Synchrotron Light Source II.« less

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

Xiao, Ya; Cultural Relics and Archaeology Institute of Hunan, Changsha 410083; Fu, Xuan

Urgent restoration of the Wugang Ming dynasty city wall brings about the need for a study of the formulation and properties of mortars. In the present paper, mortar samples from the Wugang Ming dynasty city wall were characterized in a combination of sheet polarized light optical microscopy, scanning electron microscopy with X-ray energy dispersive spectrometer, thermogravimetric/differential scanning calorimetry, X-ray powder diffraction, Fourier transform infrared spectroscopy, and inductively coupled plasma emission spectroscopy. Results show that mortars are mainly built up from inorganic calcium carbonate based organic–inorganic hybrid material with a small amount of sticky rice, which plays a crucial role inmore » forming dense and compact microstructure of mortars and effectively hindering penetration of water and air into mortars. Analysis of decayed products shows that the detrimental soluble salts originates from ambient environment. - Highlights: • Mortars used in the Wugang city wall are a calcium carbonate-sticky rice hybrid bonding material. • Carbonation processing is extremely slow due to dense and compact microstructure of mortars. • Decying of mortars results from the appearance of soluble salt from ambient environment.« less

Environmental performance, mechanical and microstructure analysis of concrete containing oil-based drilling cuttings pyrolysis residues of shale gas.

PubMed

Wang, Chao-Qiang; Lin, Xiao-Yan; He, Ming; Wang, Dan; Zhang, Si-Lan

2017-09-15

The overall objective of this research project is to investigate the feasibility of incorporating oil-based drilling cuttings pyrolysis residues (ODPR) and fly ash serve as replacements for fine aggregates and cementitious materials in concrete. Mechanical and physical properties, detailed environmental performances, and microstructure analysis were carried out. Meanwhile, the early hydration process and hydrated products of ODPR concrete were analyzed with X-ray diffraction (XRD), Fourier transform infrared (FT-IR), scanning electron microscopy (SEM) and energy-dispersive X-ray spectroscopy (EDX). The results indicated that ODPR could not be categorize into hazardous wastes. ODPR had specific pozzolanic characteristic and the use of ODPR had certain influence on slump and compressive strength of concrete. The best workability and optimal compressive strength were achieved with the help of 35% ODPR. Environmental performance tests came to conclusion that ODPR as recycled aggregates and admixture for the preparation of concrete, from the technique perspective, were the substance of mere environmental contamination. Copyright © 2017 Elsevier B.V. All rights reserved.

Carbon foam/hydroxyapatite coating for carbon/carbon composites: Microstructure and biocompatibility

NASA Astrophysics Data System (ADS)

Zhang, Leilei; Li, Hejun; Li, Kezhi; Zhang, Shouyang; Lu, Jinhua; Li, Wei; Cao, Sheng; Wang, Bin

2013-12-01

To improve the surface biocompatibility of carbon/carbon composites, a carbon foam/hydroxyapatite coating was applied using a combination method of slurry procedure and ultrasound-assisted electrochemical deposition procedure. The morphology, microstructure and chemical composition of the coating were investigated by scanning electron microscopy, energy dispersive X-ray spectroscopy, Fourier transform infrared spectroscopy, Raman spectroscopy and X-ray diffraction. The biocompatibility of the carbon foam/hydroxyapatite coating was investigated by osteoblast-like MG63 cell culture tests. The results showed that the carbon foam could provide a large number of pores on the surface of carbon/carbon composites. The hydroxyapatite crystals could infiltrate into the pores and form the carbon foam/hydroxyapatite coating. The coating covered the carbon/carbon composites fully and uniformly with slice morphology. The cell response tests showed that the MG63 cells on carbon foam/hydroxyapatite coating had a better cell adhesion and cell proliferation than those on uncoated carbon/carbon composites. The carbon foam/hydroxyapatite coatings were cytocompatible and were beneficial to improve the biocompatibility. The approach presented here may be exploited for fabrication of carbon/carbon composite implant surfaces.

Microstructural Change and Mechanical Properties with Isochronal Aging in Al-Ni-Gd Metallic Glasses

NASA Astrophysics Data System (ADS)

Kato, Hideomi; Hirosawa, Shoichi; Matsuda, Kenji; Shiflet, Gary J.

The changes of precipitation microstructures and mechanical properties during isochronal aging have been studied for melt-spun metallic glasses of Al-Ni-Gd ternary system. The fabricated Al90Ni3Gd7, Al87Ni7Gd6 and Al85Ni7Gd8 ribbons were isochronally aged up to 400°C and then examined by X-ray diffraction (XRD), transmission electron microscopy (TEM) and energy dispersive X-ray spectrometry (EDX). It was found that two different intermetallic compounds of Al23Ni6Gd4 and Al19Ni5Gd3 as well as primary crystallized α-Al are formed by the isochronal aging in good agreement with the fact that three exothermic peaks are detected in the differential scanning calorimetry (DSC) curves. The highest nanoindentation hardness and Young's modulus were obtained for the isochronally-aged Al85Ni7Gd8, suggesting that not only the increase in Ni and Gd contents but also the isochronal aging is quite effective in strengthening the melt-spun Al-Ni-Gd alloys.

Co removal and phase transformations during high power diode laser irradiation of cemented carbide

NASA Astrophysics Data System (ADS)

Barletta, M.; Rubino, G.; Gisario, A.

2011-02-01

The use of a continuous wave-high power diode laser for removing surface Co-binder from Co-cemented tungsten carbide (WC-Co (5.8 wt%.)) hardmetal slabs was investigated. Combined scanning electron microscopy, energy dispersive X-ray spectroscopy and X-ray diffraction analyses were performed in order to study the phase transformations and micro-structural modifications of the WC-Co substrates occurring during and after laser irradiation. The micro-structure of the WC-Co progressively transforms as energy density increased, exhibiting stronger removal of Co and WC grain growth. At very high energy density, local melting of the WC grains with the formation of big agglomerates of interlaced grains is observed, and the crystalline structure of the irradiated substrate shows the presence of a brittle ternary eutectic phase of W, Co and C (often referred to as the η-phase). The latter can be detrimental to the mechanical properties of WC-Co. Therefore, the proper adjustment of the laser processing parameters plays a crucial role in surface treatments of WC-Co substrates prior to post-processing like diamond deposition.

Microstructures and Properties of Laser Cladding Al-TiC-CeO2 Composite Coatings

PubMed Central

Kong, Dejun; Song, Renguo

2018-01-01

Al-TiC-CeO2 composite coatings have been prepared by using a laser cladding technique, and the microstructure and properties of the resulting composite coatings have been investigated using scanning electron microscopy (SEM), a 3D microscope system, X-ray diffraction (XRD), micro-hardness testing, X-ray stress measurements, friction and wear testing, and an electrochemical workstation. The results showed that an Al-Fe phase appears in the coatings under different applied laser powers and shows good metallurgical bonding with the matrix. The dilution rate of the coating first decreases and then increases with increasing laser power. The coating was transformed from massive and short rod-like structures into a fine granular structure, and the effect of fine grain strengthening is significant. The microhardness of the coatings first decreases and then increases with increasing laser power, and the maximum microhardness can reach 964.3 HV0.2. In addition, the residual stress of the coating surface was tensile stress, and crack size increases with increasing stress. When the laser power was 1.6 kW, the coating showed high corrosion resistance. PMID:29373555

Microstructures and Properties of Laser Cladding Al-TiC-CeO₂ Composite Coatings.

PubMed

He, Xing; Kong, Dejun; Song, Renguo

2018-01-26

Al-TiC-CeO₂ composite coatings have been prepared by using a laser cladding technique, and the microstructure and properties of the resulting composite coatings have been investigated using scanning electron microscopy (SEM), a 3D microscope system, X-ray diffraction (XRD), micro-hardness testing, X-ray stress measurements, friction and wear testing, and an electrochemical workstation. The results showed that an Al-Fe phase appears in the coatings under different applied laser powers and shows good metallurgical bonding with the matrix. The dilution rate of the coating first decreases and then increases with increasing laser power. The coating was transformed from massive and short rod-like structures into a fine granular structure, and the effect of fine grain strengthening is significant. The microhardness of the coatings first decreases and then increases with increasing laser power, and the maximum microhardness can reach 964.3 HV 0.2 . In addition, the residual stress of the coating surface was tensile stress, and crack size increases with increasing stress. When the laser power was 1.6 kW, the coating showed high corrosion resistance.

Mesoscale Science with High Energy X-ray Diffraction Microscopy at the Advanced Photon Source

NASA Astrophysics Data System (ADS)

Suter, Robert

2014-03-01

Spatially resolved diffraction of monochromatic high energy (> 50 keV) x-rays is used to map microstructural quantities inside of bulk polycrystalline materials. The non-destructive nature of High Energy Diffraction Microscopy (HEDM) measurements allows tracking of responses as samples undergo thermo-mechanical or other treatments. Volumes of the order of a cubic millimeter are probed with micron scale spatial resolution. Data sets allow direct comparisons to computational models of responses that frequently involve long-ranged, multi-grain interactions; such direct comparisons have only become possible with the development of HEDM and other high energy x-ray methods. Near-field measurements map the crystallographic orientation field within and between grains using a computational reconstruction method that simulates the experimental geometry and matches orientations in micron sized volume elements to experimental data containing projected grain images in large numbers of Bragg peaks. Far-field measurements yield elastic strain tensors through indexing schemes that sort observed diffraction peaks into sets associated with individual crystals and detect small radial motions in large numbers of such peaks. Combined measurements, facilitated by a new end station hutch at Advanced Photon Source beamline 1-ID, are mutually beneficial and result in accelerated data reduction. Further, absorption tomography yields density contrast that locates secondary phases, void clusters, and cracks, and tracks sample shape during deformation. A collaboration led by the Air Force Research Laboratory and including the Advanced Photon Source, Lawrence Livermore National Laboratory, Carnegie Mellon University, Petra-III, and Cornell University and CHESS is developing software and hardware for combined measurements. Examples of these capabilities include tracking of grain boundary migrations during thermal annealing, tensile deformation of zirconium, and combined measurements of nickel superalloys and a titanium alloy under tensile forces. Work supported by NSF grant DMR-1105173

Thermal x-ray diffraction and near-field phase contrast imaging

NASA Astrophysics Data System (ADS)

Li, Zheng; Classen, Anton; Peng, Tao; Medvedev, Nikita; Wang, Fenglin; Chapman, Henry N.; Shih, Yanhua

2017-10-01

Using higher-order coherence of thermal light sources, the resolution power of standard x-ray imaging techniques can be enhanced. In this work, we applied the higher-order measurement to far-field x-ray diffraction and near-field phase contrast imaging (PCI), in order to achieve superresolution in x-ray diffraction and obtain enhanced intensity contrast in PCI. The cost of implementing such schemes is minimal compared to the methods that achieve similar effects by using entangled x-ray photon pairs.

Thermal x-ray diffraction and near-field phase contrast imaging

DOE PAGES

Li, Zheng; Classen, Anton; Peng, Tao; ...

2017-12-27

Using higher-order coherence of thermal light sources, the resolution power of standard x-ray imaging techniques can be enhanced. Here in this work, we applied the higher-order measurement to far-field x-ray diffraction and near-field phase contrast imaging (PCI), in order to achieve superresolution in x-ray diffraction and obtain enhanced intensity contrast in PCI. The cost of implementing such schemes is minimal compared to the methods that achieve similar effects by using entangled x-ray photon pairs.

Grain Refinement by Authigenic Inoculation Inherited from the Medium-Range Order Structure of Ni-Cr-W Superalloy

NASA Astrophysics Data System (ADS)

Gao, Zhongtang; Hu, Rui; Guo, Wei; Zhang, Chuanwei

2018-04-01

The combination of liquidus casting and thermal control solidification furnace was applied to obtain a fine-grained ingot. A rapid quenching method and x-ray diffraction measurement were used to investigate the effect of authigenic inoculation on grain refinement. The structure factor S(Q) of liquid Ni-Cr-W superalloy at 1400 °C (Liquidus temperature) and bright-field image of the microstructures quenched from 1400 °C have been measured by the high-temperature x-ray diffractometer and the transmission electron microscopy (TEM), respectively. The results show that a pre-peak exists on a S(Q) curve at the liquidus temperature. The clusters of atom in rapidly quenched microstructures obtained by isothermal heat treatment at 1400 °C were studied using TEM. Meanwhile, the effect of isothermal different temperatures on rapidly quenched microstructures was studied. The results also show that there are only the globular, equiaxed grains distributed in the solidification structure. These particles are inherited from the medium-range order structure, which is beneficial for grain refinement. The normalized work-hardening rate-strain curve indicates the work-hardening rate of fine grain is higher than that of conventional grain at the same temperature and the same deformation.

Grain Refinement by Authigenic Inoculation Inherited from the Medium-Range Order Structure of Ni-Cr-W Superalloy

NASA Astrophysics Data System (ADS)

Gao, Zhongtang; Hu, Rui; Guo, Wei; Zhang, Chuanwei

2018-05-01

The combination of liquidus casting and thermal control solidification furnace was applied to obtain a fine-grained ingot. A rapid quenching method and x-ray diffraction measurement were used to investigate the effect of authigenic inoculation on grain refinement. The structure factor S( Q) of liquid Ni -Cr-W superalloy at 1400 °C (Liquidus temperature) and bright-field image of the microstructures quenched from 1400 °C have been measured by the high-temperature x-ray diffractometer and the transmission electron microscopy (TEM), respectively. The results show that a pre-peak exists on a S( Q) curve at the liquidus temperature. The clusters of atom in rapidly quenched microstructures obtained by isothermal heat treatment at 1400 °C were studied using TEM. Meanwhile, the effect of isothermal different temperatures on rapidly quenched microstructures was studied. The results also show that there are only the globular, equiaxed grains distributed in the solidification structure. These particles are inherited from the medium-range order structure, which is beneficial for grain refinement. The normalized work-hardening rate-strain curve indicates the work-hardening rate of fine grain is higher than that of conventional grain at the same temperature and the same deformation.

Magnetoresistivity and microstructure of YBa2Cu3Oy prepared using planetary ball milling

NASA Astrophysics Data System (ADS)

Hamrita, A.; Ben Azzouz, F.; Madani, A.; Ben Salem, M.

2012-01-01

We have studied the microstructure and the magnetoresistivity of polycrystalline YBa2Cu3Oy (YBCO or Y-123 for brevity) embedded with nanoparticles of Y-deficient YBCO, generated by the planetary ball milling technique. Bulk samples were synthesized from a precursor YBCO powder, which was prepared from commercial high purity Y2O3, Ba2CO3 and CuO via a one-step annealing process in air at 950 °C. After planetary ball milling of the precursor, the powder was uniaxially pressed and subsequently annealed at 950 °C in air. Phase analysis by X-ray diffraction (XRD), granular structure examination by scanning electron microscopy (SEM), microstructure investigation by transmission electron microscopy (TEM) coupled with energy dispersive X-ray spectroscopy (EDXS) were carried out. TEM analyses show that nanoparticles of Y-deficient YBCO, generated by ball milling, are embedded in the superconducting matrix. Electrical resistance as a function of temperature, ρ(T), revealed that the zero resistance temperature, Tco, is 84.5 and 90 K for the milled and unmilled samples respectively. The milled ceramics exhibit a large magnetoresistance in weak magnetic fields at liquid nitrogen temperature. This attractive effect is of high significance as it makes these materials promising candidates for practical application in magnetic field sensor devices.

Effect of copper concentration in the electrolyte on the surface morphology and the microstructure of CuInSe2 films

NASA Astrophysics Data System (ADS)

Hung, Pin-Kun; Kuo, Ting-Wei; Huang, Kuo-Chan; Wang, Na-Fu; Hsieh, Po-Tsung; Houng, Mau-Phon

2012-07-01

The surface morphology and the microstructure of CuInSe2 precursor films have been investigated by co-electrodeposition with different [Cu2+] concentrations from 2 mM to 4 mM. The characteristic of the precursor films was examined using field-emission scanning electron microscopy (FE-SEM), energy dispersive X-ray spectroscopy (EDS), glancing incidence angle X-ray diffraction (GIXRD) and micro-Raman spectrometer, respectively. The surface morphology of the precursor films become more smoother and compact with choice of appropriate [Cu2+] concentration (3-3.5 mM) in the electrolyte. The relation between surface morphology and [Cu2+] concentration is also considered in terms of electrodeposition nucleation mechanisms using the mathematical models of Scharifker and Hills. It is suggested that the higher [Cu2+] concentrations can provide more numbers of nucleation sites on the surface of the electrode. Results simulated from the Rietveld refinement method suggest that decreasing dCusbnd Se is related to charge transfer from interstitial copper atoms and can affect the film microstructure. Micro-Raman spectrum also shows that the excess Cu atoms in the precursor films does not contribute significantly to large amounts of secondary phases but rather exists in the crystallite structure as other defect types.

Report on the Synchrotron Characterization of U-Mo and U-Zr Alloys and the Modeling Results

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

Okuniewski, Maria A.; Ganapathy, Varsha; Hamilton, Brenden

2016-09-01

ABSTRACT Uranium-molybdenum (U-Mo) and uranium-zirconium (U-Zr) are two promising fuel candidates for nuclear transmutation reactors which burn long-lived minor actinides and fission products within fast spectrum reactors. The objectives of this research are centered on understanding the early stages of fuel performance through the examination of the irradiation induced microstructural changes in U-Zr and U-Mo alloys subjected to low neutron fluences. Specimens that were analyzed include those that were previously irradiated in the Advanced Test Reactor at INL. This most recent work has focused on a sub-set of the irradiated specimens, specifically U-Zr and U-Mo alloys that were irradiated tomore » 0.01 dpa at temperatures ranging from (150-800oC). These specimens were analyzed with two types of synchrotron techniques, including X-ray absorption fine structure and X-ray diffraction. These techniques provide non-destructive microstructural analysis, including phase identification and quantitation, lattice parameters, crystallite sizes, as well as bonding, structure, and chemistry. Preliminary research has shown changes in the phase fractions, crystallite sizes, and lattice parameters as a function of irradiation and temperature. Future data analyses will continue to explore these microstructural changes.« less

Low-Temperature Bainite: A Thermal Stability Study

NASA Astrophysics Data System (ADS)

Santajuana, Miguel A.; Rementeria, Rosalia; Kuntz, Matthias; Jimenez, Jose A.; Caballero, Francisca G.; Garcia-Mateo, Carlos

2018-06-01

The thermal stability of nanobainitic structures obtained by heat treating two different high-carbon high-silicon steels at temperatures between 200 °C and 600 °C has been investigated by means of three complementary techniques, i.e., field emission gun-scanning electron microscopy, X-ray diffraction, and high-resolution dilatometry. Three main stages have been established, each of them characterized by a distinctive microstructure. Furthermore, the nanocrystalline structure generated by the bainite reaction confers the steel with an extraordinary tempering resistance.

Low-Temperature Bainite: A Thermal Stability Study

NASA Astrophysics Data System (ADS)

Santajuana, Miguel A.; Rementeria, Rosalia; Kuntz, Matthias; Jimenez, Jose A.; Caballero, Francisca G.; Garcia-Mateo, Carlos

2018-04-01

The thermal stability of nanobainitic structures obtained by heat treating two different high-carbon high-silicon steels at temperatures between 200 °C and 600 °C has been investigated by means of three complementary techniques, i.e., field emission gun-scanning electron microscopy, X-ray diffraction, and high-resolution dilatometry. Three main stages have been established, each of them characterized by a distinctive microstructure. Furthermore, the nanocrystalline structure generated by the bainite reaction confers the steel with an extraordinary tempering resistance.

Characterization of the Microstructure of the Compositionally Complex Alloy Al1Mo0.5Nb1Ta0.5Ti1Zr1 (Postprint)

DTIC Science & Technology

2016-05-01

limited to X-ray diffraction ( XRD ) and scanning electron microscopy (SEM). The alloy was reported to contain two bcc phases with similar lattice...it appears that the interface between the two phases is fairly coherent. Interestingly, the XRD study described in [8] suggested that there were two...line-scan shown in (h). 3 Distribution A. Approved for public reledifference in lattice parameter measurements realized in bulk samples ( XRD ) vs

Laser sintered thin layer graphene and cubic boron nitride reinforced nickel matrix nanocomposites

NASA Astrophysics Data System (ADS)

Hu, Zengrong; Tong, Guoquan

2015-10-01

Laser sintered thin layer graphene (Gr)-cubic boron nitride (CBN)-Ni nanocomposites were fabricated on AISI 4140 plate substrate. The composites fabricating process, composites microstructure and mechanical properties were studied. Scanning electron microscopy (SEM), X-ray diffraction (XRD) and Raman spectroscopy were employed to study the micro structures and composition of the composites. XRD and Raman tests proved that graphene and CBN were dispersed in the nanocomposites. Nanoindentation test results indicate the significant improvements were achieved in the composites mechanical properties.

Aluminum induced crystallization of amorphous Ge thin films on insulating substrate

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

Singh, Ch. Kishan, E-mail: kisn@igcar.gov.in; Tah, T.; Sunitha, D. T.

2016-05-23

Aluminium (metal) induced crystallization of amorphous Ge in bilayer and multilayer Ge/Al thin films deposited on quartz substrate at temperature well below the crystallization temperature of bulk Ge is reported. The crystallization of poly-Ge proceeds via formations of dendritic crystalline Ge grains in the Al matrix. The observed phases were characterized by Raman spectroscopy and X-ray diffraction. The microstructure of Al thin film layer was found to have a profound influence on such crystallization process and formation of dendritic grains.

Effect of Ca2+ Ions on Electrical Properties of Ba1-x Ca x Ti0.90Sn0.10O3-0.05Y2O3 Ceramics

NASA Astrophysics Data System (ADS)

Chen, Zhi-hui; Li, Zhi-wei; Ding, Jian-ning; Zhao, Tian-xiang; Qiu, Jian-hua; Zhu, Ke-qian; Xu, Jiu-jun; Zhang, Bing

2018-03-01

Ba1-x Ca x Ti0.90Sn0.10O3-0.05Y2O3 (BCTSY) lead-free piezoceramics with x = 0.02 to 0.10 have been fabricated by solid-state sintering method at 1420°C. The effects of Ca2+ ions on the microstructure and electrical properties of the samples were studied. X-ray diffraction analysis showed that all samples possessed pure perovskite structure with Ca2+ ions diffused into the matrix lattice. The rhombohedral phase and tetragonal phase coexisted in the composition range of 0.02 < x < 0.06. The microstructure of BCTSY ceramic became more homogeneous with addition of Ca2+ ions, and the average grain size of the samples decreased from 97 μm (x = 0.02) to 18 μm (x = 0.10). Addition of Ca2+ remarkably improved the piezoelectric properties, enhanced the dielectric frequency dispersion, and increased the Curie temperature of the ceramics. The piezoelectric properties of the ceramics were optimized at x = 0.04 with d 33 and K p values of 579 pC/N and 52.7%, respectively.

Effect of Ca2+ Ions on Electrical Properties of Ba1- x Ca x Ti0.90Sn0.10O3-0.05Y2O3 Ceramics

NASA Astrophysics Data System (ADS)

Chen, Zhi-hui; Li, Zhi-wei; Ding, Jian-ning; Zhao, Tian-xiang; Qiu, Jian-hua; Zhu, Ke-qian; Xu, Jiu-jun; Zhang, Bing

2018-07-01

Ba1- x Ca x Ti0.90Sn0.10O3-0.05Y2O3 (BCTSY) lead-free piezoceramics with x = 0.02 to 0.10 have been fabricated by solid-state sintering method at 1420°C. The effects of Ca2+ ions on the microstructure and electrical properties of the samples were studied. X-ray diffraction analysis showed that all samples possessed pure perovskite structure with Ca2+ ions diffused into the matrix lattice. The rhombohedral phase and tetragonal phase coexisted in the composition range of 0.02 < x < 0.06. The microstructure of BCTSY ceramic became more homogeneous with addition of Ca2+ ions, and the average grain size of the samples decreased from 97 μm ( x = 0.02) to 18 μm ( x = 0.10). Addition of Ca2+ remarkably improved the piezoelectric properties, enhanced the dielectric frequency dispersion, and increased the Curie temperature of the ceramics. The piezoelectric properties of the ceramics were optimized at x = 0.04 with d 33 and K p values of 579 pC/N and 52.7%, respectively.

An image focusing means by using an opaque object to diffract x-rays

DOEpatents

Sommargren, Gary E.; Weaver, H. Joseph

1991-01-01

The invention provides a method and apparatus for focusing and imaging x-rays. An opaque sphere is used as a diffractive imaging element to diffract x-rays from an object so that the divergent x-ray wavefronts are transformed into convergent wavefronts and are brought to focus to form an image of the object with a large depth of field.

Microstructural, Magnetic, and Optical Properties of Pr-Doped Perovskite Manganite La0.67Ca0.33MnO3 Nanoparticles Synthesized via Sol-Gel Process

NASA Astrophysics Data System (ADS)

Xia, Weiren; Wu, Heng; Xue, Piaojie; Zhu, Xinhua

2018-05-01

We report on microstructural, magnetic, and optical properties of Pr-doped perovskite manganite (La1 - xPrx)0.67Ca0.33MnO3 (LPCMO, x = 0.0-0.5) nanoparticles synthesized via sol-gel process. Structural characterizations (X-ray and electron diffraction patterns, (high resolution) TEM images) provide information regarding the phase formation and the single-crystalline nature of the LPCMO systems. X-ray and electron diffraction patterns reveal that all the LPCMO samples crystallize in perovskite crystallography with an orthorhombic structure ( Pnma space group), where the MnO6 octahedron is elongated along the b axis due to the Jahn-Teller effect. That is confirmed by Raman spectra. Crystallite sizes and grain sizes were calculated from XRD and TEM respectively, and the lattice fringes resolved in the high-resolution TEM images of individual LPCMO nanoparticle confirmed its single-crystalline nature. FTIR spectra identify the characteristic Mn-O bond stretching vibration mode near 600 cm- 1, which shifts towards high wavenumbers with increasing post-annealing temperature or Pr-doping concentration, resulting in further distortion of the MnO6 octahedron. XPS revealed dual oxidation states of Mn3+ and Mn4+ in the LPCMO nanoparticles. UV-vis absorption spectra confirm the semiconducting nature of the LPCMO nanoparticles with optical bandgaps of 2.55-2.71 eV. Magnetic measurements as a function of temperature and magnetic field at field cooling and zero-field cooling modes, provided a Curie temperature around 230 K, saturation magnetization of about 81 emu/g, and coercive field of 390 Oe at 10 K. Such magnetic properties and the semiconducting nature of the LPCMO nanoparticles will make them as suitable candidate for magnetic semiconductor spintronics.

One-step fabrication of BaMoO4 microstructures with controlled morphologies via a simple EDTA-mediated route

NASA Astrophysics Data System (ADS)

Yin, Yongkui; Li, Ying; Zhang, Haifeng; Ren, Fengyun; Zhang, Dawei; Feng, Wenxu; Shao, Lili; Li, Kaijun; Liu, Yang; Sun, Zhanpeng; Li, Miaojing; Song, Gaochen; Wang, Guan

2013-03-01

A facile strategy has been developed to synthesize BaMoO4 microcrystals with different morphologies, such as octopus-like, flower-like, and Chinese-cabbage-like, by using ethylenediaminetetraacetic acid as chelating and capping reagent at room temperature. X-ray diffraction, field emission scanning electron microscopy, and Fourier transformer infrared spectroscopy were introduced to characterize the composition, morphology, and chemical information of the as-obtained products. The effects of a series of experimental parameters, such as ethylenediaminetetraacetic acid quantity and the reagent concentrations, on the morphology and photoluminescence properties of the consequential BaMoO4 microcrystals were investigated in detail. The photoluminescence spectra of the obtained BaMoO4 microstructures exhibited different emission intensities. This method could be readily extended to synthesize BaWO4 microstructures with various morphologies.

Effect of austempering temperature and time on mechanical properties of SAE 9260 steel

NASA Astrophysics Data System (ADS)

Dalwatkar, Ranjit; Prabhu, N.; Singh, R. K. P.

2018-04-01

This work describes the effect of austempering heat treatment on microstrcuture and mechanical properties of SAE 9260 steel. Steel samples, austenitized at 900 °C for one hour, were isothermally heat treated in the temperature range 300,325 and 350 °C for different times. Microstructural characterization was carried out using optical and scanning electron microscopes. The microstructure of the austempered samples consisted of bainitic ferrite and retained austenite. The volume fraction of retained austenite was determined using X-ray diffraction. Isothermal heat treatment at 350 °C for 20 min, resulted in a retained austenite content of around 38% in the microstructure. Increase in isothermal transformation temperature led to an increase in the fraction of retained austenite. Also, good combination of strength and ductility was obtained in the samples with increased amounts of retained austenite.

Study of Cold Coiling Spring Steel on Microstructure and Cold Forming Performance

NASA Astrophysics Data System (ADS)

Jiang, Y.; Liang, Y. L.; Ming, Y.; Zhao, F.

2017-09-01

Medium-carbon cold-coiling locomotive spring steels were treated by a novel Q-P-T (quenching-partitioning-tempering) process. Scanning electron microscopy (SEM), transmission electron microscope (TEM) and X-ray diffraction (XRD) were used to characterize the relevant parameters of the steel. Results show that the microstructure of tested steel treated by Q-P-T process is a complex microstructures composed of martensite, bainite and retained austenite. The volume fraction of retained austenite (wt.%) is up to 31%. After pre-deforming and tempering again at 310°C, the plasticity of samples treated by Q-P-T process is still well. Fracture images show that the Q-P-T samples are ductile fracture. It is attributed to the higher volume fraction of the retained austenite and the interactions between the multi-phases in Q-P-T processed sample.

Tensile Deformation Temperature Impact on Microstructure and Mechanical Properties of AISI 316LN Austenitic Stainless Steel

NASA Astrophysics Data System (ADS)

Xiong, Yi; He, Tiantian; Lu, Yan; Ren, Fengzhang; Volinsky, Alex A.; Cao, Wei

2018-03-01

Uniaxial tensile tests were conducted on AISI 316LN austenitic stainless steel from - 40 to 300 °C at a rate of 0.5 mm/min. Microstructure and mechanical properties of the deformed steel were investigated by optical, scanning and transmission electron microscopies, x-ray diffraction, and microhardness testing. The yield strength, ultimate tensile strength, elongation, and microhardness increase with the decrease in the test temperature. The tensile fracture morphology has the dimple rupture feature after low-temperature deformations and turns to a mixture of transgranular fracture and dimple fracture after high-temperature ones. The dominating deformation microstructure evolves from dislocation tangle/slip bands to large deformation twins/slip bands with temperature decrease. The deformation-induced martensite transformation can only be realized at low temperature, and its quantity increases with the decrease in the temperature.

Microstructural and mineralogical characterization of selected shales in support of nuclear waste repository studies

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

Lee, S.Y.; Hyder, L.K.; Alley, P.D.

1988-01-01

Five shales were examined as part of the Sedimentary Rock Program evaluation of this medium as a potential host for a US civilian nuclear waste repository. The units selected for characterization were the Chattanooga Shale from Fentress County, Tennessee; the Pierre Shale from Gregory County, South Dakota; the Green River Formation from Garfield County, Colorado; and the Nolichucky Shale and Pumpkin Valley Shale from Roane County, Tennessee. The micromorphology and structure of the shales were examined by petrographic, scanning electron, and high-resolution transmission electron microscopy. Chemical and mineralogical compositions were studied through the use of energy-dispersive x-ray, neutron activation, atomicmore » absorption, thermal, and x-ray diffraction analysis techniques. 18 refs., 12 figs., 2 tabs.« less

Chrome-free Samarium-based Protective Coatings for Magnesium Alloys

NASA Astrophysics Data System (ADS)

Hou, Legan; Cui, Xiufang; Yang, Yuyun; Lin, Lili; Xiao, Qiang; Jin, Guo

The microstructure of chrome-free samarium-based conversion coating on magnesium alloy was investigated and the corrosion resistance was evaluated as well. The micro-morphology, transverse section, crystal structure and composition of the coating were observed by scanning electron microscopy (SEM), X-ray diffraction (XRD), energy dispersive spectroscopy (EDS) and X- ray photoelectron spectroscopy (XPS), respectively. The corrosion resistance was evaluated by potentiodynamic polarization curve and electrochemical impedance spectroscopy (EIS). The results reveal that the morphology of samarium conversion coating is of crack-mud structure. Tiny cracks distribute in the compact coating deposited by samarium oxides. XRD, EDS and XPS results characterize that the coating is made of amorphous and trivalent-samarium oxides. The potentiodynamic polarization curve, EIS and OCP indicate that the samarium conversion coating can improve the corrosion resistance of magnesium alloys.

X-ray analysis of residual stress gradients in TiN coatings by a Laplace space approach and cross-sectional nanodiffraction: a critical comparison.

PubMed

Stefenelli, Mario; Todt, Juraj; Riedl, Angelika; Ecker, Werner; Müller, Thomas; Daniel, Rostislav; Burghammer, Manfred; Keckes, Jozef

2013-10-01

Novel scanning synchrotron cross-sectional nanobeam and conventional laboratory as well as synchrotron Laplace X-ray diffraction methods are used to characterize residual stresses in exemplary 11.5 µm-thick TiN coatings. Both real and Laplace space approaches reveal a homogeneous tensile stress state and a very pronounced compressive stress gradient in as-deposited and blasted coatings, respectively. The unique capabilities of the cross-sectional approach operating with a beam size of 100 nm in diameter allow the analysis of stress variation with sub-micrometre resolution at arbitrary depths and the correlation of the stress evolution with the local coating microstructure. Finally, advantages and disadvantages of both approaches are extensively discussed.

Nanocrystalline Cs{sub x}WO{sub 3} particles: Effects of N{sub 2} annealing on microstructure and near-infrared shielding characteristics

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

Liu, Jing-Xiao, E-mail: drliu-shi@dlpu.edu.cn; Institute of Multidisciplinary Research for Advanced Material, Tohoku University, Sendai, 980-8577,Japan; Shi, Fei

2013-10-15

In order to further improve the near-infrared shielding properties of cesium tungsten bronze (Cs{sub x}WO{sub 3}) for solar filter applications, Cs{sub x}WO{sub 3} particles were prepared by solvothermal reaction method and the effects of nitrogen annealing on the microstructure and near-infrared shielding properties of Cs{sub x}WO{sub 3} were investigated. The obtained Cs{sub x}WO{sub 3} samples were characterized by X-ray diffraction, scanning electron microscopy, transmission electron microscopy, X-ray photoelectron spectroscopy and spectrophotometer. The results indicate that nanosheet-like Cs{sub x}WO{sub 3} particles with hexagonal structure began to transform into nanorods after annealed at temperature higher than 600 °C. The near-infrared shielding propertiesmore » of Cs{sub x}WO{sub 3} particles could be further improved by N{sub 2} annealing at 500–700 °C. Particularly, the 500 °C-annealed Cs{sub x}WO{sub 3} samples in the N{sub 2} atmosphere showed best near-infrared shielding properties. It was suggested that the excellent near-infrared shielding ability of the 500 °C-annealed Cs{sub x}WO{sub 3} samples is correlated with its minimum O/W atomic ratio and most oxygen vacancies. Highlights: • N{sub 2} annealing could further improve the near-infrared (NIR) shielding of Cs{sub x}WO{sub 3}. • Effects of N{sub 2} annealing on microstructure and NIR shielding of Cs{sub x}WO{sub 3} were studied. • The 500 °C-N{sub 2}-annealed Cs{sub x}WO{sub 3} exhibited minimum O/W ratio and most oxygen vacancies. • The 500 °C-N{sub 2}-annealed Cs{sub x}WO{sub 3} particles exhibited best NIR shielding properties.« less

Soft X-Ray Diffraction Microscopy of a Frozen Hydrated Yeast Cell

DOE PAGES

Huang, Xiaojing; Nelson, Johanna; Kirz, Janos; ...

2009-11-01

We report the first image of an intact, frozen hydrated eukaryotic cell using x-ray diffraction microscopy, or coherent x-ray diffraction imaging. By plunge freezing the specimen in liquid ethane and maintaining it below -170 °C, artifacts due to dehydration, ice crystallization, and radiation damage are greatly reduced. In this example, coherent diffraction data using 520 eV x rays were recorded and reconstructed to reveal a budding yeast cell at a resolution better than 25 nm. This demonstration represents an important step towards high resolution imaging of cells in their natural, hydrated state, without limitations imposed by x-ray optics.

Understanding the initial irreversibility of metal sulfides for sodium-ion batteries via operando techniques

DOE PAGES

Wang, Liguang; Wang, Jiajun; Guo, Fangmin; ...

2018-11-13

Transition metal sulfides are promising high capacity anodes for sodium-ion batteries in terms of the conversion reaction with multiple alkali metal ions. Nonetheless, some inherent challenges such as sluggish sodium ion diffusion kinetics, large volume change, and poor cycle stability limit their implementation. Addressing these issues necessitates a comprehensive understanding the complex sodium ion storage mechanism particularly at the initial cycle. Here, taking nickel subsulfide as a model material, we reveal the complicated conversion reaction mechanism upon the first cycle by combining in operando 2D transmission X-ray microscopy with X-ray absorption spectroscopy, ex-situ 3D nano-tomography, high-energy X-ray diffraction and electrochemicalmore » impedance spectroscopy. This study demonstrates that the microstructure evolution, inherent slow sodium ions diffusion kinetics, and slow ion mobility at the two-phase interface contribute to the high irreversible capacity upon the first cycle. Finally, such understandings are critical for developing the conversion reaction materials with the desired electrochemical activity and stability.« less

Understanding the initial irreversibility of metal sulfides for sodium-ion batteries via operando techniques

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

Wang, Liguang; Wang, Jiajun; Guo, Fangmin

Transition metal sulfides are promising high capacity anodes for sodium-ion batteries in terms of the conversion reaction with multiple alkali metal ions. Nonetheless, some inherent challenges such as sluggish sodium ion diffusion kinetics, large volume change, and poor cycle stability limit their implementation. Addressing these issues necessitates a comprehensive understanding the complex sodium ion storage mechanism particularly at the initial cycle. Here, taking nickel subsulfide as a model material, we reveal the complicated conversion reaction mechanism upon the first cycle by combining in operando 2D transmission X-ray microscopy with X-ray absorption spectroscopy, ex-situ 3D nano-tomography, high-energy X-ray diffraction and electrochemicalmore » impedance spectroscopy. This study demonstrates that the microstructure evolution, inherent slow sodium ions diffusion kinetics, and slow ion mobility at the two-phase interface contribute to the high irreversible capacity upon the first cycle. Finally, such understandings are critical for developing the conversion reaction materials with the desired electrochemical activity and stability.« less

Nanostructured zinc oxide films synthesized by successive chemical solution deposition for gas sensor applications

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

Lupan, O.; Department of Physics, University of Central Florida, 4000 Central Florida Blvd., Orlando, FL 32816-2385; Chow, L.

2009-01-08

Nanostructured ZnO thin films have been deposited using a successive chemical solution deposition method. The structural, morphological, electrical and sensing properties of the films were studied for different concentrations of Al-dopant and were analyzed as a function of rapid photothermal processing temperatures. The films were investigated by X-ray diffraction, scanning electron microscopy, energy dispersive X-ray spectroscopy, X-ray photoelectron and micro-Raman spectroscopy. Electrical and gas sensitivity measurements were conducted as well. The average grain size is 240 and 224 A for undoped ZnO and Al-doped ZnO films, respectively. We demonstrate that rapid photothermal processing is an efficient method for improving themore » quality of nanostructured ZnO films. Nanostructured ZnO films doped with Al showed a higher sensitivity to carbon dioxide than undoped ZnO films. The correlations between material compositions, microstructures of the films and the properties of the gas sensors are discussed.« less

Hard and soft X-ray microscopy and tomography in catalysis: bridging the different time and length scales.

PubMed

Grunwaldt, Jan-Dierk; Schroer, Christian G

2010-12-01

X-ray microscopic techniques are excellent and presently emerging techniques for chemical imaging of heterogeneous catalysts. Spatially resolved studies in heterogeneous catalysis require the understanding of both the macro and the microstructure, since both have decisive influence on the final performance of the industrially applied catalysts. A particularly important aspect is the study of the catalysts during their preparation, activation and under operating conditions, where X-rays have an inherent advantage due to their good penetration length especially in the hard X-ray regime. Whereas reaction cell design for hard X-rays is straightforward, recently smart in situ cells have also been reported for the soft X-ray regime. In the first part of the tutorial review, the constraints from a catalysis view are outlined, then the scanning and full-field X-ray microscopy as well as coherent X-ray diffraction imaging techniques are described together with the challenging design of suitable environmental cells. Selected examples demonstrate the application of X-ray microscopy and tomography to monitor structural gradients in catalytic reactors and catalyst preparation with micrometre resolution but also the possibility to follow structural changes in the sub-100 nm regime. Moreover, the potential of the new synchrotron radiation sources with higher brilliance, recent milestones in focusing of hard X-rays as well as spatiotemporal studies are highlighted. The tutorial review concludes with a view on future developments in the field of X-ray microscopy that will have strong impact on the understanding of catalysts in the future and should be combined with in situ electron microscopic studies on the nanoscale and other spectroscopic studies like microRaman, microIR and microUV-vis on the macroscale.

Assessment of elemental composition, microstructure, and hardness of stainless steel endodontic files and reamers.

PubMed

Darabara, Myrsini; Bourithis, Lefteris; Zinelis, Spiros; Papadimitriou, George D

2004-07-01

The purpose of this study was to determine the elemental composition, microstructure, and hardness of commercially available reamers, K files, and H files. Five instruments of each type from different manufacturers (Antaeos, FKG, Maillefer, Mani, and Micromega) were embedded in epoxy resin along their longitudinal axis. After metallographic grinding and polishing, the specimens were chemically etched and their microstructure investigated under an incident light microscope. The specimens were studied under a scanning electron microscope, and their elemental compositions were determined by energy dispersive X-ray microanalysis. The same surfaces were repolished and X-ray diffraction was performed. The same specimen surface was used for the assessment of the Vickers hardness (HV200) by using a microhardness tester with a 200-g load and 20-s contact time. The hardness results were statistically analyzed with two-way ANOVA and Tukey's test (a = 0.05). All files demonstrated extensively elongated grains parallel to longitudinal file axis because of cold drawing. The elemental composition of Maillefer and Mani reamers, Antaeos K files, and Mani H files were found in the range of AISI 303 SS, whereas all the rest were determined as AISI 304 SS. Two different phases (austenite SSt and martensite SSt) were identified with X-ray diffraction for all files tested. The results of hardness classified reamers in the following decreasing order (HMV200): Micromega = 673 +/- 29, Mani = 662 +/- 24, Maillefer = 601 +/- 34, Antaeos = 586 +/- 18, FKG = 557 +/- 19, and the K files (HV200): FKG = 673 +/- 16, Mani = 647 +/- 19, Maillefer = 603 +/- 41, Antaeos = 566 +/- 21, Micromega = 555 +/- 15, and the H files (HMV200): Mani = 640 +/- 12, FKG = 583 +/- 31, Maillefer = 581 +/- 5, Antaeos = 573 +/- 3, Micromega = 546 +/- 14. Although only two stainless steel alloys were used for the production of endodontic files, the differences in hardness are independent to the alloys used, implying that other factors, such as the production method or the thermomechanical history of the alloys, play an important role on the mechanical properties of endodontic files.

Application of focused-beam flat-sample method to synchrotron powder X-ray diffraction with anomalous scattering effect

NASA Astrophysics Data System (ADS)

Tanaka, M.; Katsuya, Y.; Matsushita, Y.

2013-03-01

The focused-beam flat-sample method (FFM), which is a method for high-resolution and rapid synchrotron X-ray powder diffraction measurements by combination of beam focusing optics, a flat shape sample and an area detector, was applied for diffraction experiments with anomalous scattering effect. The advantages of FFM for anomalous diffraction were absorption correction without approximation, rapid data collection by an area detector and good signal-to-noise ratio data by focusing optics. In the X-ray diffraction experiments of CoFe2O4 and Fe3O4 (By FFM) using X-rays near the Fe K absorption edge, the anomalous scattering effect between Fe/Co or Fe2+/Fe3+ can be clearly detected, due to the change of diffraction intensity. The change of observed diffraction intensity as the incident X-ray energy was consistent with the calculation. The FFM is expected to be a method for anomalous powder diffraction.

Rietveld analysis using powder diffraction data with anomalous scattering effect obtained by focused beam flat sample method

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

Tanaka, Masahiko, E-mail: masahiko@spring8.or.jp; Katsuya, Yoshio, E-mail: katsuya@spring8.or.jp; Sakata, Osami, E-mail: SAKATA.Osami@nims.go.jp

2016-07-27

Focused-beam flat-sample method (FFM) is a new trial for synchrotron powder diffraction method, which is a combination of beam focusing optics, flat shape powder sample and area detectors. The method has advantages for X-ray diffraction experiments applying anomalous scattering effect (anomalous diffraction), because of 1. Absorption correction without approximation, 2. High intensity X-rays of focused incident beams and high signal noise ratio of diffracted X-rays 3. Rapid data collection with area detectors. We applied the FFM to anomalous diffraction experiments and collected synchrotron X-ray powder diffraction data of CoFe{sub 2}O{sub 4} (inverse spinel structure) using X-rays near Fe K absorptionmore » edge, which can distinguish Co and Fe by anomalous scattering effect. We conducted Rietveld analyses with the obtained powder diffraction data and successfully determined the distribution of Co and Fe ions in CoFe{sub 2}O{sub 4} crystal structure.« less

Shear at Twin Domain Boundaries in YBa2Cu3O7-x

NASA Astrophysics Data System (ADS)

Caldwell, W. A.; Tamura, N.; Celestre, R. S.; MacDowell, A. A.; Padmore, H. A.; Geballe, T. H.; Koster, G.; Batterman, B. W.; Patel, J. R.

2004-05-01

The microstructure and strain state of twin domains in YBa2Cu3O7-x are discussed based upon synchrotron white-beam x-ray microdiffraction measurements. Intensity variations of the fourfold twin splitting of Laue diffraction peaks are used to determine the twin domain structure. Strain analysis shows that interfaces between neighboring twin domains are strained in shear, whereas the interior of these domains are regions of low strain. These measurements are consistent with the orientation relationships of twin boundaries within and across domains and show that basal plane shear stresses can exceed 100MPa where twin domains meet. Our results support stress field pinning of magnetic flux vortices by twin domain boundaries.

Multiscale tomographic analysis of heterogeneous cast Al-Si-X alloys.

PubMed

Asghar, Z; Requena, G; Sket, F

2015-07-01

The three-dimensional microstructure of cast AlSi12Ni and AlSi10Cu5Ni2 alloys is investigated by laboratory X-ray computed tomography, synchrotron X-ray computed microtomography, light optical tomography and synchrotron X-ray computed microtomography with submicrometre resolution. The results obtained with each technique are correlated with the size of the scanned volumes and resolved microstructural features. Laboratory X-ray computed tomography is sufficient to resolve highly absorbing aluminides but eutectic and primary Si remain unrevealed. Synchrotron X-ray computed microtomography at ID15/ESRF gives better spatial resolution and reveals primary Si in addition to aluminides. Synchrotron X-ray computed microtomography at ID19/ESRF reveals all the phases ≥ ∼1 μm in volumes about 80 times smaller than laboratory X-ray computed tomography. The volumes investigated by light optical tomography and submicrometre synchrotron X-ray computed microtomography are much smaller than laboratory X-ray computed tomography but both techniques provide local chemical information on the types of aluminides. The complementary techniques applied enable a full three-dimensional characterization of the microstructure of the alloys at length scales ranging over six orders of magnitude. © 2015 The Authors Journal of Microscopy © 2015 Royal Microscopical Society.

Microstructural, dielectric and magnetic properties of multiferroic composite system barium strontium titanate – nickel cobalt ferrite

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

Pahuja, Poonam, E-mail: poonampahuja123@gmail.com; Tandon, R. P., E-mail: ram-tandon@hotmail.com

2015-05-15

Multiferroic composites (1-x) Ba{sub 0.95}Sr{sub 0.05}TiO{sub 3} + (x) Ni{sub 0.8}Co{sub 0.2}Fe{sub 2}O{sub 4} (where x = 0.1, 0.2, 0.3, 0.4) has been prepared by solid state reaction method. X-ray diffraction analysis of the composite samples confirmed the presence of both barium strontium titanate (BST) and nickel cobalt ferrite (NCF) phases. FESEM images indicated the well dispersion of NCF grains among BST grains. Dielectric constant and loss of the composite samples decreases with increase in frequency following Maxwell-Wagner relaxation mechanism. Composite sample with highest ferrite content possesses highest values of remanent and saturation magnetization.

Dynamical effects in Bragg coherent x-ray diffraction imaging of finite crystals

NASA Astrophysics Data System (ADS)

Shabalin, A. G.; Yefanov, O. M.; Nosik, V. L.; Bushuev, V. A.; Vartanyants, I. A.

2017-08-01

We present simulations of Bragg coherent x-ray diffractive imaging (CXDI) data from finite crystals in the frame of the dynamical theory of x-ray diffraction. The developed approach is based on a numerical solution of modified Takagi-Taupin equations and can be applied for modeling of a broad range of x-ray diffraction experiments with finite three-dimensional crystals of arbitrary shape also in the presence of strain. We performed simulations for nanocrystals of a cubic and hemispherical shape of different sizes and provided a detailed analysis of artifacts in the Bragg CXDI reconstructions introduced by the dynamical diffraction. Based on our theoretical analysis we developed an analytical procedure to treat effects of refraction and absorption in the reconstruction. Our results elucidate limitations for the kinematical approach in the Bragg CXDI and suggest a natural criterion to distinguish between kinematical and dynamical cases in coherent x-ray diffraction on a finite crystal.

Thermoelectric Properties of Self Assembled TiO2/SnO2 Nanocomposites

NASA Technical Reports Server (NTRS)

Dynys, Fred; Sayir, Ali; Sehirlioglu, Alp

2008-01-01

Recent advances in improving efficiency of thermoelectric materials are linked to nanotechnology. Thermodynamically driven spinodal decomposition was utilized to synthesize bulk nanocomposites. TiO2/SnO2 system exhibits a large spinodal region, ranging from 15 to 85 mole % TiO2. The phase separated microstructures are stable up to 1400 C. Semiconducting TiO2/SnO2 powders were synthesized by solid state reaction between TiO2 and SnO2. High density samples were fabricated by pressureless sintering. Self assemble nanocomposites were achieved by annealing at 1000 to 1350 C. X-ray diffraction reveal phase separation of (Ti(x)Sn(1-x))O2 type phases. The TiO2/SnO2 nanocomposites exhibit n-type behavior; a power factor of 70 W/mK2 at 1000 C has been achieved with penta-valent doping. Seebeck, thermal conductivity, electrical resistivity and microstructure will be discussed in relation to composition and doping.

Thermoelectric Properties of Self Assemble TiO2/SnO2 Nanocomposites

NASA Technical Reports Server (NTRS)

Dynys, Fred; Sayir, Ali; Sehirlioglu, Alp

2008-01-01

Recent advances in improving efficiency of thermoelectric materials are linked to nanotechnology. Thermodynamically driven spinodal decomposition was utilized to synthesize bulk nanocomposites. TiO2/SnO2 system exhibits a large spinodal region, ranging from 15 to 85 mole % TiO2. The phase separated microstructures are stable up to 1400 C. Semiconducting TiO2/SnO2 powders were synthesized by solid state reaction between TiO2 and SnO2. High density samples were fabricated by pressureless sintering. Self assemble nanocomposites were achieved by annealing at 1000 to 1350 C. X-ray diffraction reveal phase separation of (Ti(x)Sn(1-x))O2 type phases. The TiO2/SnO2 nanocomposites exhibit n-type behavior; a power factor of 70 (mu)W/m sq K at 1000 C has been achieved with penta-valent doping. Seebeck, thermal conductivity, electrical resistivity and microstructure will be discussed in relation to composition and doping.

High-power laser interaction with low-density C–Cu foams

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

Pérez, F.; Colvin, J. D.; May, M. J.

2015-11-15

We study the propagation of high-power laser beams in micro-structured carbon foams by monitoring the x-ray output from deliberately introduced Cu content. In particular, we characterize this phenomenon measuring absolute time-resolved x-ray yields, time-resolved x-ray imaging, and x-ray spectroscopy. New experimental results for C–Cu foams show a faster heat front velocity than simulation that assumed homogeneous plasma. We suggest the foam micro-structure may explain this trend.

High-power laser interaction with low-density C–Cu foams

DOE PAGES

Pérez, F.; Colvin, J. D.; May, M. J.; ...

2015-11-19

Here, we study the propagation of high-power laser beams in micro-structured carbon foams by monitoring the x-ray output from deliberately introduced Cu content. In particular, we characterize this phenomenon measuring absolute time-resolved x-ray yields, time-resolved x-ray imaging, and x-ray spectroscopy. New experimental results for C–Cu foams show a faster heat front velocity than simulation that assumed homogeneous plasma. We suggest the foam micro-structure may explain this trend.

The Investigation of Strain-Induced Martensite Reverse Transformation in AISI 304 Austenitic Stainless Steel

NASA Astrophysics Data System (ADS)

Cios, G.; Tokarski, T.; Żywczak, A.; Dziurka, R.; Stępień, M.; Gondek, Ł.; Marciszko, M.; Pawłowski, B.; Wieczerzak, K.; Bała, P.

2017-10-01

This paper presents a comprehensive study on the strain-induced martensitic transformation and reversion transformation of the strain-induced martensite in AISI 304 stainless steel using a number of complementary techniques such as dilatometry, calorimetry, magnetometry, and in-situ X-ray diffraction, coupled with high-resolution microstructural transmission Kikuchi diffraction analysis. Tensile deformation was applied at temperatures between room temperature and 213 K (-60 °C) in order to obtain a different volume fraction of strain-induced martensite (up to 70 pct). The volume fraction of the strain-induced martensite, measured by the magnetometric method, was correlated with the total elongation, hardness, and linear thermal expansion coefficient. The thermal expansion coefficient, as well as the hardness of the strain-induced martensitic phase was evaluated. The in-situ thermal treatment experiments showed unusual changes in the kinetics of the reverse transformation (α' → γ). The X-ray diffraction analysis revealed that the reverse transformation may be stress assisted—strains inherited from the martensitic transformation may increase its kinetics at the lower annealing temperature range. More importantly, the transmission Kikuchi diffraction measurements showed that the reverse transformation of the strain-induced martensite proceeds through a displacive, diffusionless mechanism, maintaining the Kurdjumov-Sachs crystallographic relationship between the martensite and the reverted austenite. This finding is in contradiction to the results reported by other researchers for a similar alloy composition.

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

Frequency dependent dielectric properties of combustion synthesized Dy2Ti2O7 pyrochlore oxide

NASA Astrophysics Data System (ADS)

Jeyasingh, T.; Saji, S. K.; Kavitha, V. T.; Wariar, P. R. S.

2018-05-01

Nanocrystalline pyrochlore material Dysprosium Titanate (Dy2Ti2O7) has been synthesized through a single step optimized combustion route. The phase purity and phase formation of the combustion product has been characterized using X-Ray diffraction analysis (XRD) and Fourier Transform Infrared Spectroscopy (FT-IR) analysis. X-Ray diffraction analysis (XRD) reveal that Dy2Ti2O7 is highly crystalline in nature with cubic structure in the Fd3m space group. The microstructures and average particle size of the prepared nanopowder were examined by High Resolution Transmission Electron Microscopy (HR-TEM). The optical band gap of the Dy2Ti2O7 nanoparticles is determined from the absorption spectrum, was attributed to direct allowed transitions through optical band gap of 3.98 eV. The frequency dependent dielectric measurements have been carried out on the sintered pellet in the frequency range 1 Hz-10 MHz. The measured value of dielectric constant (ℇ') was ˜ 43 and loss tangent (tan δ) was 4×10-3 at 1 MHz, at room temperature.

Structural and magnetic properties of Ni0.8M0.2Fe2O4 (M = Cu, Co) nano-crystalline ferrites

NASA Astrophysics Data System (ADS)

Vijaya Babu, K.; Satyanarayana, G.; Sailaja, B.; Santosh Kumar, G. V.; Jalaiah, K.; Ravi, M.

2018-06-01

Nano-crystalline nickel ferrites are interesting materials due to their large physical and magnetic properties. In the present work, two kinds of spinel ferrites Ni0.8M0.2Fe2O4 (M = Cu, Co) are synthesized by using sol-gel auto-combustion method and the results are compared with NiFe2O4. The structural properties of synthesized ferrites are determined by using X-ray powder diffraction; scanning electron microscope and Fourier transform infrared spectroscopy. The cation distribution obtained from X-ray diffraction show that cobalt/copper occupies only tetrahedral site in spinel lattice. The lattice constant increases with the substitution of cobalt/copper. The structural parameters like bond lengths, tetrahedral and octahedral edges have been varied with the substitution. The microstructural study is carried out by using SEM technique and the average grain size is increased with nickel ferrite. The initial permeability (μi) is improving with the substitution. The observed g-value from ESR is approximately equal to standard value.

Ultrathin Cr added Ru film as a seedless Cu diffusion barrier for advanced Cu interconnects

NASA Astrophysics Data System (ADS)

Hsu, Kuo-Chung; Perng, Dung-Ching; Yeh, Jia-Bin; Wang, Yi-Chun

2012-07-01

A 5 nm thick Cr added Ru film has been extensively investigated as a seedless Cu diffusion barrier. High-resolution transmission electron microscopy micrograph, X-ray diffraction (XRD) pattern and Fourier transform-electron diffraction pattern reveal that a Cr contained Ru (RuCr) film has a glassy microstructure and is an amorphous-like film. XRD patterns and sheet resistance data show that the RuCr film is stable up to 650 °C, which is approximately a 200 °C improvement in thermal stability as compared to that of the pure Ru film. X-ray photoelectron spectroscopy depth profiles show that the RuCr film can successfully block Cu diffusion, even after a 30-min 650 °C annealing. The leakage current of the Cu/5 nm RuCr/porous SiOCH/Si stacked structure is about two orders of magnitude lower than that of a pristine Ru sample for electric field below 1 MV/cm. The RuCr film can be a promising Cu diffusion barrier for advanced Cu metallization.

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

Zia-ul-Mustafa, M., E-mail: engr.ziamustafa@gmail.com; Ahmad, Faiz; Megat-Yusoff, Puteri S. M.

In this study, intumescent fire retardant coatings (IFRC) were developed to investigate the synergistic effects of reinforced mica and wollastonite fillers based IFRC towards heat shielding, char expansion, char composition and char morphology. Ammonium poly-phosphate (APP) was used as acid source, expandable graphite (EG) as carbon source, melamine as blowing agent, boric acid as additive and Hardener H-2310 polyamide amine in bisphenol A epoxy resin BE-188(BPA) was used as curing agent. Bunsen burner fire test was used for thermal performance according to UL-94 for 1 h. Field Emission Scanning Electron Microscopy (FESEM) was used to observe char microstructure. X-Ray Diffraction (XRD)more » and Fourier transform infrared spectroscopy (FTIR) were used to analyse char composition. The results showed that addition of clay filler in IFRC enhanced the fire protection performance of intumescent coating. X-Ray Diffraction (XRD) and Fourier transform infrared spectroscopy (FTIR) results showed the presence of boron phosphate, silicon phosphate oxide, aluminium borate in the char that improved the thermal performance of intumescent fire retardant coating (IFRC). Resultantly, the presence of these developed compounds enhanced the Integrity of structural steel upto 500°C.« less

[Effect of Eu(Pr) substitution at Ba sites on microstructure and superconductivity in EuBa2Cu3O7-delta ceramics].

PubMed

Peng, Zhen-sheng; Wang, Zhi-he

2004-04-01

Ceramics of Eu1+xBa2-xCu3O7-delta with x = 0.0, 0.05, 0.1, 0.2, 0.3, 0.4, 0.5 and EuBa2-xPrxCu3O7-delta with x=0.0, 0.05, 0.1, 0.2, 0.3, 0.4 have been synthesized and investigated by X-ray diffraction, resistivity, and Raman spectroscopy. The results show that the transition of crystal structure from orthorhombic to tetragonal occurs and the criticaltemperature decreases withthe increase in doping concentration x. The Raman spectra show that the frequency of the Cu(1)-O(4) stretching mode andthe Cu(2)-(2, 3) out-of-phase mode shifts to higher wave number with increasing doping concentration x.

Instrument and method for X-ray diffraction, fluorescence, and crystal texture analysis without sample preparation

NASA Technical Reports Server (NTRS)

Gendreau, Keith (Inventor); Martins, Jose Vanderlei (Inventor); Arzoumanian, Zaven (Inventor)

2010-01-01

An X-ray diffraction and X-ray fluorescence instrument for analyzing samples having no sample preparation includes a X-ray source configured to output a collimated X-ray beam comprising a continuum spectrum of X-rays to a predetermined coordinate and a photon-counting X-ray imaging spectrometer disposed to receive X-rays output from an unprepared sample disposed at the predetermined coordinate upon exposure of the unprepared sample to the collimated X-ray beam. The X-ray source and the photon-counting X-ray imaging spectrometer are arranged in a reflection geometry relative to the predetermined coordinate.

Single and multi-layered core-shell structures based on ZnO nanorods obtained by aerosol assisted chemical vapor deposition

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

Sáenz-Trevizo, A.; Amézaga-Madrid, P.; Pizá-Ruiz, P.

2015-07-15

Core–shell nanorod structures were prepared by a sequential synthesis using an aerosol assisted chemical vapor deposition technique. Several samples consisting of ZnO nanorods were initially grown over TiO{sub 2} film-coated borosilicate glass substrates, following the synthesis conditions reported elsewhere. Later on, a uniform layer consisting of individual Al, Ni, Ti or Fe oxides was grown onto ZnO nanorod samples forming the so-called single MO{sub x}/ZnO nanorod core–shell structures, where MO{sub x} was the metal oxide shell. Additionally, a three-layer core–shell sample was developed by growing Fe, Ti and Fe oxides alternately, onto the ZnO nanorods. The microstructure of the core–shellmore » materials was characterized by grazing incidence X-ray diffraction, scanning and transmission electron microscopy. Energy dispersive X-ray spectroscopy was employed to corroborate the formation of different metal oxides. X-ray diffraction outcomes for single core–shell structures showed solely the presence of ZnO as wurtzite and TiO{sub 2} as anatase. For the multi-layered shell sample, the existence of Fe{sub 2}O{sub 3} as hematite was also detected. Morphological observations suggested the existence of an outer material grown onto the nanorods and further microstructural analysis by HR-STEM confirmed the development of core–shell structures in all cases. These studies also showed that the individual Al, Fe, Ni and Ti oxide layers are amorphous; an observation that matched with X-ray diffraction analysis where no apparent extra oxides were detected. For the multi-layered sample, the development of a shell consisting of three different oxide layers onto the nanorods was found. Overall results showed that no alteration in the primary ZnO core was produced during the growth of the shells, indicating that the deposition technique used herein was and it is suitable for the synthesis of homogeneous and complex nanomaterials high in quality and purity. In addition, materials absorptance determined from the total transmittance and reflectance spectra revealed a broader absorption interval including visible light, indicating potential uses of these nanostructures on solar energy appliances. - Graphical abstract: Display Omitted - Highlights: • Uniform ZnO nanorods (core)–metal oxide (shell) were obtained sequentially by AACVD. • Shells were structured of homogeneous single or multi-layered non-mixed metal oxides. • ZnO nanorod core was preserved during the shell synthesis. • Optical absorptance revealed visible interval absorption for FeO{sub x} shell samples. • Materials can be suitable for photocatalytic or photovoltaic applications.« less

Grid-enhanced X-ray coded aperture microscopy with polycapillary optics

PubMed Central

Sowa, Katarzyna M.; Last, Arndt; Korecki, Paweł

2017-01-01

Polycapillary devices focus X-rays by means of multiple reflections of X-rays in arrays of bent glass capillaries. The size of the focal spot (typically 10–100 μm) limits the resolution of scanning, absorption and phase-contrast X-ray imaging using these devices. At the expense of a moderate resolution, polycapillary elements provide high intensity and are frequently used for X-ray micro-imaging with both synchrotrons and X-ray tubes. Recent studies have shown that the internal microstructure of such an optics can be used as a coded aperture that encodes high-resolution information about objects located inside the focal spot. However, further improvements to this variant of X-ray microscopy will require the challenging fabrication of tailored devices with a well-defined capillary microstructure. Here, we show that submicron coded aperture microscopy can be realized using a periodic grid that is placed at the output surface of a polycapillary optics. Grid-enhanced X-ray coded aperture microscopy with polycapillary optics does not rely on the specific microstructure of the optics but rather takes advantage only of its focusing properties. Hence, submicron X-ray imaging can be realized with standard polycapillary devices and existing set-ups for micro X-ray fluorescence spectroscopy. PMID:28322316

Grid-enhanced X-ray coded aperture microscopy with polycapillary optics.

PubMed

Sowa, Katarzyna M; Last, Arndt; Korecki, Paweł

2017-03-21

Polycapillary devices focus X-rays by means of multiple reflections of X-rays in arrays of bent glass capillaries. The size of the focal spot (typically 10-100 μm) limits the resolution of scanning, absorption and phase-contrast X-ray imaging using these devices. At the expense of a moderate resolution, polycapillary elements provide high intensity and are frequently used for X-ray micro-imaging with both synchrotrons and X-ray tubes. Recent studies have shown that the internal microstructure of such an optics can be used as a coded aperture that encodes high-resolution information about objects located inside the focal spot. However, further improvements to this variant of X-ray microscopy will require the challenging fabrication of tailored devices with a well-defined capillary microstructure. Here, we show that submicron coded aperture microscopy can be realized using a periodic grid that is placed at the output surface of a polycapillary optics. Grid-enhanced X-ray coded aperture microscopy with polycapillary optics does not rely on the specific microstructure of the optics but rather takes advantage only of its focusing properties. Hence, submicron X-ray imaging can be realized with standard polycapillary devices and existing set-ups for micro X-ray fluorescence spectroscopy.

Philip A. Parilla | NREL

Science.gov Websites

atomic layer deposition for applications. He also manages the majority of X-ray characterization equipment at NREL, specifically X-ray diffraction and X-ray fluorescence instrumentation. Additionally, he for EERE's Hydrogen Storage program. He is also an expert in X-ray diffraction and X-ray fluorescence

Study on Composition, Microstructure and Wear Behavior of Fe-B-C Wear-Resistant Surfacing Alloys

NASA Astrophysics Data System (ADS)

Zhuang, Minghui; Li, Muqin; Wang, Jun; Ma, Zhen; Yuan, Shidan

2017-12-01

Fe-B-C alloy layers with various microstructures were welded on Q235 steel plates using welding powders/H08Mn2Si and welding wires composite surfacing technology. The relationship existing between the chemical composition, microstructure and wear resistance of the surfacing alloy layers was investigated by scanning electron microscopy, x-ray diffraction, electron backscatter diffraction and wear tests. The results demonstrated that the volume fractions and morphologies of the microstructures in the surfacing alloy layers could be controlled by adjusting the boron and carbon contents in the welding powders, which could further regulate the wear resistance of the surfacing alloy layers. The typical microstructures of the Fe-B-C surfacing alloy layers included dendritic Fe, rod-like Fe2B, fishbone-like Fe2B and daisy-like Fe3(C, B). The wear resistance of the alloy layers with various morphologies differed. The wear resistance order of the different microstructures was: rod-like Fe2B > fishbone-like Fe2B > daisy-like Fe3(C, B) > dendritic Fe. A large number of rod-like Fe2B with high microhardness could be obtained at the boron content of 5.70 5.90 wt.% and the carbon content of 0.50 0.60wt.%. The highest wear resistance of the Fe-B-C alloy layers reached the value of 24.1 g-1, which demonstrates the main microscopic cutting wear mechanism of the Fe-B-C alloy layers.

Histological, chemical, and morphological reexamination of the ``heart'' of a small Late Cretaceous Thescelosaurus

NASA Astrophysics Data System (ADS)

Cleland, Timothy P.; Stoskopf, Michael K.; Schweitzer, Mary H.

2011-03-01

A three-dimensional, iron-cemented structure found in the anterior thoracic cavity of articulated Thescelosaurus skeletal remains was hypothesized to be the fossilized remains of the animal's four-chambered heart. This was important because the finding could be interpreted to support a hypothesis that non-avian dinosaurs were endothermic. Mammals and birds, the only extant organisms with four-chambered hearts and single aortae, are endotherms. The hypothesis that this Thescelosaurus has a preserved heart was controversial, and therefore, we reexamined it using higher-resolution computed tomography, paleohistological examination, X-ray diffraction analysis, X-ray photoelectron spectroscopy, and scanning electron microscopy. This suite of analyses allows for detailed morphological and chemical examination beyond what was provided in the original work. Neither the more detailed examination of the gross morphology and orientation of the thoracic "heart" nor the microstructural studies supported the hypothesis that the structure was a heart. The more advanced computed tomography showed the same three areas of low density as the earlier studies with no evidence of additional low-density areas as might be expected from examinations of an ex situ ostrich heart. Microstructural examination of a fragment taken from the "heart" was consistent with cemented sand grains, and no chemical signal consistent with a biological origin was detected. However, small patches of cell-like microstructures were preserved in the sandstone matrix of the thoracic structure. A possible biological origin for these microstructures is the focus of ongoing investigation.

Microstructure, Phase Occurrence, and Corrosion Behavior of As-Solidified and As-Annealed Al-Pd Alloys

NASA Astrophysics Data System (ADS)

Ďuriška, Libor; Palcut, Marián; Špoták, Martin; Černičková, Ivona; Gondek, Ján; Priputen, Pavol; Čička, Roman; Janičkovič, Dušan; Janovec, Jozef

2018-02-01

In the present work, we studied the microstructure, phase constitution, and corrosion performance of Al88Pd12, Al77Pd23, Al72Pd28, and Al67Pd33 alloys (metal concentrations are given in at.%). The alloys were prepared by repeated arc melting of Al and Pd granules in argon atmosphere. The as-solidified samples were further annealed at 700 °C for 500 h. The microstructure and phase constitution of the as-solidified and as-annealed alloys were studied by scanning electron microscopy, energy-dispersive x-ray spectroscopy, and x-ray diffraction. The alloys were found to consist of (Al), ɛ n ( Al3Pd), and δ (Al3Pd2) in various fractions. The corrosion testing of the alloys was performed in aqueous NaCl (0.6 M) using a standard 3-electrode cell monitored by potentiostat. The corrosion current densities and corrosion potentials were determined by Tafel extrapolation. The corrosion potentials of the alloys were found between - 763 and - 841 mV versus Ag/AgCl. An active alloy dissolution has been observed, and it has been found that (Al) was excavated, whereas Al in ɛ n was de-alloyed. The effects of bulk chemical composition, phase occurrence and microstructure on the corrosion behavior are evaluated. The local nobilities of ɛ n and δ are discussed. Finally, the conclusions about the alloy's corrosion resistance in saline solutions are provided.

Characterization of ZnAl cast alloys with Na addition

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

Gancarz, Tomasz, E-mail: t.gancarz@imim.pl; Cempura, Grzegorz; Skuza, Wojciech

2016-01-15

This study was aimed at evaluating the microstructural change and thermal, electrical and mechanical properties with the addition of Na to eutectic ZnAl alloys. Solders based on eutectic ZnAl containing 0.2 to 3.0 (wt.%) of Na were developed for high temperature solder. Differential scanning calorimetry (DSC) measurements were performed to determine the melting temperatures of the alloys. Thermal linear expansion and electrical resistivity measurements were performed over − 50 °C to 300 °C and 30 °C to 300 °C temperature ranges, respectively. The microstructure of the specimens was analyzed using scanning (SEM) and transmission electron microscopy (TEM) techniques. Chemical microanalysismore » was performed by energy-dispersive X-ray spectroscopy (EDS) on SEM and TEM. The precipitates of NaZn{sub 13} were confirmed by X-ray diffraction (XRD) measurements and selected area electron diffraction (SAED) techniques. The addition of Na to eutectic ZnAl alloy increased the electrical resistivity and reduced the coefficient of thermal expansion; however, the melting point did not change. The mechanical properties, strain and microhardness increased with Na content in alloys. - Highlights: • High temperature soldering materials of ZnAl with Na were designed and characterized. • Precipitates of NaZn{sub 13}were observed and confirmed using TEM and XRD. • Addition of Na to eutectic ZnAl cussed increased mechanical properties. • NaZn{sub 13} caused increased electrical resistivity and microhardness, and reduced the CTE.« less

Simulations of X-ray diffraction of shock-compressed single-crystal tantalum with synchrotron undulator sources.

PubMed

Tang, M X; Zhang, Y Y; E, J C; Luo, S N

2018-05-01

Polychromatic synchrotron undulator X-ray sources are useful for ultrafast single-crystal diffraction under shock compression. Here, simulations of X-ray diffraction of shock-compressed single-crystal tantalum with realistic undulator sources are reported, based on large-scale molecular dynamics simulations. Purely elastic deformation, elastic-plastic two-wave structure, and severe plastic deformation under different impact velocities are explored, as well as an edge release case. Transmission-mode diffraction simulations consider crystallographic orientation, loading direction, incident beam direction, X-ray spectrum bandwidth and realistic detector size. Diffraction patterns and reciprocal space nodes are obtained from atomic configurations for different loading (elastic and plastic) and detection conditions, and interpretation of the diffraction patterns is discussed.

Simulations of X-ray diffraction of shock-compressed single-crystal tantalum with synchrotron undulator sources

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

Tang, M. X.; Zhang, Y. Y.; E, J. C.

Polychromatic synchrotron undulator X-ray sources are useful for ultrafast single-crystal diffraction under shock compression. Here, simulations of X-ray diffraction of shock-compressed single-crystal tantalum with realistic undulator sources are reported, based on large-scale molecular dynamics simulations. Purely elastic deformation, elastic–plastic two-wave structure, and severe plastic deformation under different impact velocities are explored, as well as an edge release case. Transmission-mode diffraction simulations consider crystallographic orientation, loading direction, incident beam direction, X-ray spectrum bandwidth and realistic detector size. Diffraction patterns and reciprocal space nodes are obtained from atomic configurations for different loading (elastic and plastic) and detection conditions, and interpretation of themore » diffraction patterns is discussed.« less

Coherent X-ray diffraction imaging of nanoengineered polymeric capsules

NASA Astrophysics Data System (ADS)

Erokhina, S.; Pastorino, L.; Di Lisa, D.; Kiiamov, A. G.; Faizullina, A. R.; Tayurskii, D. A.; Iannotta, S.; Erokhin, V.

2017-10-01

For the first time, nanoengineered polymeric capsules and their architecture have been studied with coherent X-ray diffraction imaging technique. The use of coherent X-ray diffraction imaging technique allowed us to analyze the samples immersed in a liquid. We report about the significant difference between polymeric capsule architectures under dry and liquid conditions.

A high-transparency, micro-patternable chip for X-ray diffraction analysis of microcrystals under native growth conditions

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

Murray, Thomas D.; Johns Hopkins University School of Medicine, Baltimore, MD 21205; Lyubimov, Artem Y.

A highly X-ray-transparent, silicon nitride-based device has been designed and fabricated to harvest protein microcrystals for high-resolution X-ray diffraction data collection using microfocus beamlines and XFELs. Microcrystals present a significant impediment to the determination of macromolecular structures by X-ray diffraction methods. Although microfocus synchrotron beamlines and X-ray free-electron lasers (XFELs) can enable the collection of interpretable diffraction data from microcrystals, there is a need for efficient methods of harvesting small volumes (<2 µl) of microcrystals grown under common laboratory formats and delivering them to an X-ray beam source under native growth conditions. One approach that shows promise in overcoming themore » challenges intrinsic to microcrystal analysis is to pair so-called ‘fixed-target’ sample-delivery devices with microbeam-based X-ray diffraction methods. However, to record weak diffraction patterns it is necessary to fabricate devices from X-ray-transparent materials that minimize background scattering. Presented here is the design of a new micro-diffraction device consisting of three layers fabricated from silicon nitride, photoresist and polyimide film. The chip features low X-ray scattering and X-ray absorption properties, and uses a customizable blend of hydrophobic and hydrophilic surface patterns to help localize microcrystals to defined regions. Microcrystals in their native growth conditions can be loaded into the chips with a standard pipette, allowing data collection at room temperature. Diffraction data collected from hen egg-white lysozyme microcrystals (10–15 µm) loaded into the chips yielded a complete, high-resolution (<1.6 Å) data set sufficient to determine a high-quality structure by molecular replacement. The features of the chip allow the rapid and user-friendly analysis of microcrystals grown under virtually any laboratory format at microfocus synchrotron beamlines and XFELs.« less

Microstructure and Mechanical Behavior of 17-4 Precipitation Hardenable Steel Processed by Selective Laser Melting

NASA Astrophysics Data System (ADS)

Rafi, H. Khalid; Pal, Deepankar; Patil, Nachiket; Starr, Thomas L.; Stucker, Brent E.

2014-12-01

The mechanical behavior and the microstructural evolution of 17-4 precipitation hardenable (PH) stainless steel processed using selective laser melting have been studied. Test coupons were produced from 17-4 PH stainless steel powder in argon and nitrogen atmospheres. Characterization studies were carried out using mechanical testing, optical microscopy, scanning electron microscopy, and x-ray diffraction. The results show that post-process heat treatment is required to obtain typically desired tensile properties. Columnar grains of smaller diameters (<2 µm) emerged within the melt pool with a mixture of martensite and retained austenite phases. It was found that the phase content of the samples is greatly influenced by the powder chemistry, processing environment, and grain diameter.

Comparative examination of the microstructure and high temperature oxidation performance of NiCrBSi flame sprayed and pack cementation coatings

NASA Astrophysics Data System (ADS)

Chaliampalias, D.; Vourlias, G.; Pavlidou, E.; Skolianos, S.; Chrissafis, K.; Stergioudis, G.

2009-01-01

Coatings formed from NiCrBSi powder were deposited by thermal spray and pack cementation processes on low carbon steel. The microstructure and morphology of the coatings were studied by scanning electron microscopy (SEM) and X-ray diffraction analysis (XRD). Flame sprayed coatings exhibited high porosity and were mechanically bonded to the substrate while pack cementation coatings were more compact and chemically bonded to the substrate. The microhardness and the high temperature oxidation resistance of the coated samples were evaluated by a Vickers microhardness tester and by thermogravimetric measurements (TG), respectively. Pack cementation coatings showed higher hardness and were more protective to high temperature environments than the flame sprayed coatings.

Mechanism of solid state amorphization of glucose upon milling.

PubMed

Dujardin, N; Willart, J F; Dudognon, E; Danède, F; Descamps, M

2013-02-07

Crystalline α-glucose is known to amorphize upon milling at -15 °C while it remains structurally invariant upon milling at room temperature. We have taken advantage of this behavior to compare the microstructural evolutions of the material in both conditions in order to identify the essential microstructural features which drive the amorphization process upon milling. The investigations have been performed by differential scanning calorimetry and by powder X-ray diffraction. The results indicate that two different amorphization mechanisms occur upon milling: an amorphization at the surface of crystallites due to the mechanical shocks and a spontaneous amorphization of the crystallites as they reach a critical size, which is close to 200 Å in the particular case of α-glucose.

Effects of Laser Shock Processing on Morphologies and Mechanical Properties of ANSI 304 Stainless Steel Weldments Subjected to Cavitation Erosion

PubMed Central

Zhang, Lei; Lu, Jin-Zhong; Zhang, Yong-Kang; Ma, Hai-Le; Luo, Kai-Yu; Dai, Feng-Ze

2017-01-01

Effects of laser shock processing (LSP) on the cavitation erosion resistance of laser weldments were investigated by optical microscope (OM), scanning electron microscope (SEM) observations, roughness tester, micro hardness tester, and X-ray diffraction (XRD) technology. The morphological microstructures were characterized. Cumulative mass loss, incubation period, erosion rate, and damaged surface areas were monitored during cavitation erosion. Surface roughness, micro-hardness, and residual stress were measured in different zones. Results showed that LSP could improve the damage of morphological microstructures and mechanical properties after cavitation erosion. The compressive residual stresses were generated during the process of LSP, which was an effective guarantee for the improvement of the above mentioned properties. PMID:28772652

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.

Microstructure and Mechanical Properties of Graphene-Reinforced Titanium Matrix/Nano-Hydroxyapatite Nanocomposites.

PubMed

Li, Feng; Jiang, Xiaosong; Shao, Zhenyi; Zhu, Degui; Zhu, Minhao

2018-04-16

Biomaterial composites made of titanium and hydroxyapatite (HA) powder are among the most important biomedicalmaterials due to their good mechanical properties and biocompatibility. In this work, graphene-reinforced titanium matrix/nano-hydroxyapatite nanocomposites were prepared by vacuum hot-pressing sintering. The microstructure and mechanical properties of graphene-reinforced titanium matrix/nano-hydroxyapatite nanocomposites with different graphene content were systematically investigated. Microstructures of the nanocomposites were examined by X-ray diffraction (XRD), back scattered electron imaging (BSE), scanning electron microscope (SEM) equipped with energy dispersive spectrometer (EDS), electron probe microanalyzer (EPMA), and transmission electron microscope (TEM). The mechanical properties were determined from microhardness, shear strength, and compressive strength. Results showed that during the high-temperature sintering process, complex chemical reactions occurred, resulting in new phases of nucleation such as Ca₃(PO₄)₂, Ti x P y , and Ti₃O.The new phases, which easily dropped off under the action of external force, could hinder the densification of sintering and increase the brittleness of the nanocomposites. Results demonstrated that graphene had an impact on the microstructure and mechanical properties of the nanocomposites. Based on the mechanical properties and microstructure of the nanocomposites, the strengthening and fracture mechanisms of the graphene-reinforced titanium matrix/nano-hydroxyapatite nanocomposites with different graphene content were analyzed.

X-Ray Structure determination of the Glycine Cleavage System Protein H of Mycobacterium tuberculosis Using An Inverse Compton Synchrotron X-Ray Source

PubMed Central

Abendroth, Jan; McCormick, Michael S.; Edwards, Thomas E.; Staker, Bart; Loewen, Roderick; Gifford, Martin; Rifkin, Jeff; Mayer, Chad; Guo, Wenjin; Zhang, Yang; Myler, Peter; Kelley, Angela; Analau, Erwin; Hewitt, Stephen Nakazawa; Napuli, Alberto J.; Kuhn, Peter; Ruth, Ronald D.; Stewart, Lance J.

2010-01-01

Structural genomics discovery projects require ready access to both X-ray and NMR instrumentation which support the collection of experimental data needed to solve large numbers of novel protein structures. The most productive X-ray crystal structure determination laboratories make extensive frequent use of tunable synchrotron X-ray light to solve novel structures by anomalous diffraction methods. This requires that frozen cryo-protected crystals be shipped to large government-run synchrotron facilities for data collection. In an effort to eliminate the need to ship crystals for data collection, we have developed the first laboratory-scale synchrotron light source capable of performing many of the state-of-the-art synchrotron applications in X-ray science. This Compact Light Source is a first-in-class device that uses inverse Compton scattering to generate X-rays of sufficient flux, tunable wavelength and beam size to allow high-resolution X-ray diffraction data collection from protein crystals. We report on benchmarking tests of X-ray diffraction data collection with hen egg white lysozyme, and the successful high-resolution X-ray structure determination of the Glycine cleavage system protein H from Mycobacterium tuberculosis using diffraction data collected with the Compact Light Source X-ray beam. PMID:20364333

Evolution of thermo-physical properties and annealing of fast neutron irradiated boron carbide

NASA Astrophysics Data System (ADS)

Gosset, Dominique; Kryger, Bernard; Bonal, Jean-Pierre; Verdeau, Caroline; Froment, Karine

2018-03-01

Boron carbide is widely used as a neutron absorber in most nuclear reactors, in particular in fast neutron ones. The irradiation leads to a large helium production (up to 1022/cm3) together with a strong decrease of the thermal conductivity. In this paper, we have performed thermal diffusivity measurements and X-ray diffraction analyses on boron carbide samples coming from control rods of the French Phenix LMFBR reactor. The burnups range from 1021 to 8.1021/cm3. We first confirm the strong decrease of the thermal conductivity at the low burnup, together with high microstructural modifications: swelling, large micro-strains, high defects density, and disordered-like material conductivity. We observe the microstructural parameters are highly anisotropic, with high micro-strains and flattened coherent diffracting domains along the (00l) direction of the hexagonal structure. Performing heat treatments up to high temperature (2200 °C) allows us to observe the material thermal conductivity and microstructure restoration. It then appears the thermal conductivity healing is correlated to the micro-strain relaxation. We then assume the defects responsible for most of the damage are the helium bubbles and the associated stress fields.

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.

Anti-contamination device for cryogenic soft X-ray diffraction microscopy

DOE PAGES

Huang, Xiaojing; Miao, Huijie; Nelson, Johanna; ...

2011-05-01

Cryogenic microscopy allows one to view frozen hydrated biological and soft matter specimens with good structural preservation and a high degree of stability against radiation damage. We describe a liquid nitrogen-cooled anti-contamination device for cryogenic X-ray diffraction microscopy. The anti-contaminator greatly reduces the buildup of ice layers on the specimen due to condensation of residual water vapor in the experimental vacuum chamber. We show by coherent X-ray diffraction measurements that this leads to fivefold reduction of background scattering, which is important for far-field X-ray diffraction microscopy of biological specimens.

Composition and microstructure of MTA and Aureoseal Plus: XRF, EDS, XRD and FESEM evaluation.

PubMed

Cianconi, L; Palopoli, P; Campanella, V; Mancini, M

2016-12-01

The aim of this study was to determine the chemical composition and the phases' microstructure of Aureoseal Plus (OGNA, Italy) and ProRoot MTA (Dentsply Tulsa Dental, USA) and to compare their characteristics. Study Design: Comparing Aureoseal Plus and ProRoot MTA microstructure by means of several analyses type. The chemical analysis of the two cements was assessed following the UNI EN ISO 196-2 norm. X-Ray fluorescence (XRF) was used to determine the element composition. The crystalline structure was analysed quantitatively using x-ray diffraction (XRD). Powders morphology was evaluated using a scanning electron microscope (SEM) with backscattering detectors, and a field emission scanning electron microscope (FESEM). Elemental analysis was performed by energy dispersive x-ray analysis (EDS). The semi-quantitative XRF analysis showed the presence of heavy metal oxides in both cements. The XRD spectra of the two cements reported the presence of dicalcium silicate, tricalcium silicate, tricalcium aluminate, tetracalcium aluminoferrite, bismuth oxide and gypsum. SEM analysis showed that ProRoot MTA powder is less coarse and more homogeneous than Aureoseal. Both powders are formed by particles of different shapes: round, prismatic and oblong. The EDS analysis showed that some ProRoot MTA particles, differently from Aureoseal, contain Ca, Si, Al and Fe. Oblong particles in ProRoot and Aureoseal are rich of bismuth. The strong interest in developing new Portland cement-based endodontic sealers will create materials with increased handling characteristics and physicochemical properties. A thorough investigation on two cement powders was carried out by using XRF, XRD, SEM and EDS analysis. To date there was a lack of studies on Aureoseal Plus. This cement is similar in composition to ProRoot MTA. Despite that it has distinctive elements that could improve its characteristics, resulting in a good alternative to MTA.

A microstructural study of fault rocks from the SAFOD: Implications for the deformation mechanisms and strength of the creeping segment of the San Andreas Fault

NASA Astrophysics Data System (ADS)

Hadizadeh, Jafar; Mittempergher, Silvia; Gratier, Jean-Pierre; Renard, Francois; Di Toro, Giulio; Richard, Julie; Babaie, Hassan A.

2012-09-01

The San Andreas Fault zone in central California accommodates tectonic strain by stable slip and microseismic activity. We study microstructural controls of strength and deformation in the fault using core samples provided by the San Andreas Fault Observatory at Depth (SAFOD) including gouge corresponding to presently active shearing intervals in the main borehole. The methods of study include high-resolution optical and electron microscopy, X-ray fluorescence mapping, X-ray powder diffraction, energy dispersive X-ray spectroscopy, white light interferometry, and image processing. The fault zone at the SAFOD site consists of a strongly deformed and foliated core zone that includes 2-3 m thick active shear zones, surrounded by less deformed rocks. Results suggest deformation and foliation of the core zone outside the active shear zones by alternating cataclasis and pressure solution mechanisms. The active shear zones, considered zones of large-scale shear localization, appear to be associated with an abundance of weak phases including smectite clays, serpentinite alteration products, and amorphous material. We suggest that deformation along the active shear zones is by a granular-type flow mechanism that involves frictional sliding of microlithons along phyllosilicate-rich Riedel shear surfaces as well as stress-driven diffusive mass transfer. The microstructural data may be interpreted to suggest that deformation in the active shear zones is strongly displacement-weakening. The fault creeps because the velocity strengthening weak gouge in the active shear zones is being sheared without strong restrengthening mechanisms such as cementation or fracture sealing. Possible mechanisms for the observed microseismicity in the creeping segment of the SAF include local high fluid pressure build-ups, hard asperity development by fracture-and-seal cycles, and stress build-up due to slip zone undulations.

Microstructure anisotropy of nanocrystalline titanium produced by cryomechanical grain fragmentation

NASA Astrophysics Data System (ADS)

Pohribnaya, Yu. M.; Moskalenko, V. A.; Braude, I. S.

2018-05-01

Using X-ray diffraction analysis, a systematic study was undertaken of the parameters of the deformation microstructure formed in commercially pure VT1-0 titanium as a result of cryogenic rolling at a temperature of 77 K at different degrees of compression. In order to ascertain the anisotropy of the microstructure, a comparative analysis of diffraction patterns, dimensions of crystallites (coherent scattering regions) L and microdeformation values ⟨" separators="| ɛ2 ⟩ 1 / 2 in the rolling plane and in a plane perpendicular to the rolling direction was performed by comparison with the relative activity of deformation modes. As a result, anisotropy was detected in the distribution of integral intensities of diffraction peaks for mutually perpendicular planes. The established difference in the dimensions of crystallites in the rolling plane and in the plane perpendicular to the rolling direction indicates the shape anisotropy of the crystallites. The effect of morphological anisotropy of crystallites/grains is most pronounced for the nanocrystalline state. The observed complex variation in the microdeformation values ⟨" separators="| ɛ2 ⟩ 1 / 2 ( e ) with compression deformation is well correlated with relative slip and twinning activity, which affect the level of local internal stresses and the possibility of their relaxation. The observed anisotropy with respect to the magnitude of microdeformations may be attributed to the presence of oriented grain boundaries associated with the shape anisotropy of crystallites/grains.

Observation of electromigration in a Cu thin line by in situ coherent x-ray diffraction microscopy

NASA Astrophysics Data System (ADS)

Takahashi, Yukio; Nishino, Yoshinori; Furukawa, Hayato; Kubo, Hideto; Yamauchi, Kazuto; Ishikawa, Tetsuya; Matsubara, Eiichiro

2009-06-01

Electromigration (EM) in a 1-μm-thick Cu thin line was investigated by in situ coherent x-ray diffraction microscopy (CXDM). Characteristic x-ray speckle patterns due to both EM-induced voids and thermal deformation in the thin line were observed in the coherent x-ray diffraction patterns. Both parts of the voids and the deformation were successfully visualized in the images reconstructed from the diffraction patterns. This result not only represents the first demonstration of the visualization of structural changes in metallic materials by in situ CXDM but is also an important step toward studying the structural dynamics of nanomaterials using x-ray free-electron lasers in the near future.

Measuring Three-Dimensional Strain and Structural Defects in a Single InGaAs Nanowire Using Coherent X-ray Multiangle Bragg Projection Ptychography

DOE PAGES

Hill, Megan O.; Calvo-Almazan, Irene; Allain, Marc; ...

2018-01-08

III - As nanowires are candidates for near-infrared light emitters and detectors that can be directly integrated onto silicon. However, nanoscale to microscale variations in structure, composition, and strain within a given nanowire, as well as variations between nanowires, pose challenges to correlating microstructure with device performance. In this work, we utilize coherent nanofocused X-rays to characterize stacking defects and strain in a single InGaAs nanowire supported on Si. By reconstructing diffraction patterns from the 2110 Bragg peak, we show that the lattice orientation varies along the length of the wire, while the strain field along the cross-section is largelymore » unaffected, leaving the band structure unperturbed. Diffraction patterns from the 0110 Bragg peak are reproducibly reconstructed to create three-dimensional images of stacking defects and associated lattice strains, revealing sharp planar boundaries between different crystal phases of wurtzite (WZ) structure that contribute to charge carrier scattering. Phase retrieval is made possible by developing multiangle Bragg projection ptychography (maBPP) to accommodate coherent nanodiffraction patterns measured at arbitrary overlapping positions at multiple angles about a Bragg peak, eliminating the need for scan registration at different angles. The penetrating nature of X-ray radiation, together with the relaxed constraints of maBPP, will enable the in operando imaging of nanowire devices.« less

Measuring Three-Dimensional Strain and Structural Defects in a Single InGaAs Nanowire Using Coherent X-ray Multiangle Bragg Projection Ptychography

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

Hill, Megan O.; Calvo-Almazan, Irene; Allain, Marc

III - As nanowires are candidates for near-infrared light emitters and detectors that can be directly integrated onto silicon. However, nanoscale to microscale variations in structure, composition, and strain within a given nanowire, as well as variations between nanowires, pose challenges to correlating microstructure with device performance. In this work, we utilize coherent nanofocused X-rays to characterize stacking defects and strain in a single InGaAs nanowire supported on Si. By reconstructing diffraction patterns from the 2110 Bragg peak, we show that the lattice orientation varies along the length of the wire, while the strain field along the cross-section is largelymore » unaffected, leaving the band structure unperturbed. Diffraction patterns from the 0110 Bragg peak are reproducibly reconstructed to create three-dimensional images of stacking defects and associated lattice strains, revealing sharp planar boundaries between different crystal phases of wurtzite (WZ) structure that contribute to charge carrier scattering. Phase retrieval is made possible by developing multiangle Bragg projection ptychography (maBPP) to accommodate coherent nanodiffraction patterns measured at arbitrary overlapping positions at multiple angles about a Bragg peak, eliminating the need for scan registration at different angles. The penetrating nature of X-ray radiation, together with the relaxed constraints of maBPP, will enable the in operando imaging of nanowire devices.« less

Improvement microstructural and damage characterization of ceramic composites Y{sub 2}O{sub 3} – V{sub 2}O{sub 5} with MgO nano particles

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

Issa, T. T., E-mail: alazbrh@yahoo.com; Hasan, J. M.; Abdullah, E. T.

2016-04-21

Compacted samples of Y{sub 2}O{sub 3}-V{sub 2}O{sub 5} – MgO Nano – particles wt. % sintered at different sintering temperature (700, 900, 1100, 1300) ) C° for 2 hours under static air were investigated by x-ray diffraction and differential thermal analysis(DTA), to identify the phase present .Microstructure examination achieved by scanning electron microscopy .Sintered density and porosity were measured for all sintered samples .Compression was tested too and the Brake down voltage and dielectric strength were measure for all sintered samples .The clear improvement were noticed in both microstructure and damage characterization respectively after existing the MgO Nano-particles, by increasingmore » in about 30% in sintered density and 25% for the compressive strength .The improvement also noticed on both brake down voltage and dielectric strength.« less

Microstructures define melting of molybdenum at high pressures

NASA Astrophysics Data System (ADS)

Hrubiak, Rostislav; Meng, Yue; Shen, Guoyin

2017-03-01

High-pressure melting anchors the phase diagram of a material, revealing the effect of pressure on the breakdown of the ordering of atoms in the solid. An important case is molybdenum, which has long been speculated to undergo an exceptionally steep increase in melting temperature when compressed. On the other hand, previous experiments showed nearly constant melting temperature as a function of pressure, in large discrepancy with theoretical expectations. Here we report a high-slope melting curve in molybdenum by synchrotron X-ray diffraction analysis of crystalline microstructures, generated by heating and subsequently rapidly quenching samples in a laser-heated diamond anvil cell. Distinct microstructural changes, observed at pressures up to 130 gigapascals, appear exclusively after melting, thus offering a reliable melting criterion. In addition, our study reveals a previously unsuspected transition in molybdenum at high pressure and high temperature, which yields highly textured body-centred cubic nanograins above a transition temperature.

Gradient microstructure and microhardness in a nitrided 18CrNiMo7-6 gear steel

NASA Astrophysics Data System (ADS)

Yang, R.; Wu, G. L.; Zhang, X.; Fu, W. T.; Huang, X.

2017-07-01

A commercial gear steel (18CrNiMo7-6) containing a tempered martensite structure was nitrided using a pressurized gas nitriding process under a pressure of 5 atm at 530 °C for 5 hours. The mechanical properties and microstructure of the nitrided sample were characterized by Vickers hardness measurements, X-ray diffraction, and backscatter electron imaging in a scanning electron microscope. A micro-hardness gradient was identified over a distance of 500 μm with hardness values of 900 HV at the top surface and 300 HV in the core. This micro-hardness gradient corresponds to a gradient in the microstructure that changes from a nitride compound layer at the top surface (∼ 20 μm thick) to a diffusion zone with a decreasing nitrogen concentration and precipitate density with distance from the surface, finally reaching the core matrix layer with a recovered martensite structure.

Metallurgical characterization of melt-spun ribbons of U-5.4 wt%Nb alloy

NASA Astrophysics Data System (ADS)

Ma, Rong; Ren, Zhiyong; Tang, Qingfu; Chen, Dong; Liu, Tingyi; Su, Bin; Wang, Zhenhong; Luo, Chao

2018-06-01

The microstructures and micro-mechanical properties of the melt-spun ribbons of U-5.4 wt%Nb alloy were characterized using optical microscopy, scanning electron microscopy, X-ray diffraction and nanoindentation. Observed variations in microstructures and properties are related to the changes in ribbon thicknesses and cooling rates. The microstructures of the melt-spun ribbon consist of fine-scale columnar grains (∼1 μm) adjacent to the chill surface and coarse cellular grains in the remainder of the ribbon. In addition, the formation of inclusions in the ribbon is suppressed kinetically due to the high cooling rate during melt spinning. Compared with the water-quenched specimen prepared by traditional gravity casting and solution heat treatment, the elastic modulus values of the U-5.4 wt%Nb alloy were examined to vary with grain size and exhibited diverse energy dissipation capacities.

Microstructure Evolution and Failure Analysis of an Aluminum-Copper Cathode Conductive Head Produced by Explosive Welding

NASA Astrophysics Data System (ADS)

Wei, Yanni; Luo, Yongguang; Qu, Hongtao; Zou, Juntao; Liang, Shuhua

2017-12-01

In this paper, microstructure evolution and failure analysis of the aluminum-copper interface of cathode conductive heads during their use were studied. The interface morphologies, compositions, conductivity and mechanical properties were investigated and analyzed. Obvious corrosion was found on the surface of the contact interface, which was more prevalent on an Al matrix. The crack increased sharply in the local metallurgical bonding areas on the interface, with the compound volume having no significant change. The phase transformation occurred on the interface during use, which was investigated using the elemental composition and x-ray diffraction pattern. The microhardness near the interface increased accordingly. An obvious electrical conductivity decrease appeared on the Al/Cu interface of the cathode conductive head after use over a specific time interval. Therefore, the deterioration of the microstructures and corrosion are the primary factors that affect the electrical conductivity and effective bonding, which will lead to eventual failure.

Microstructure and properties of 17-4PH steel plasma nitrocarburized with a carrier gas containing rare earth elements

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

Liu, R.L., E-mail: ruiliangliu@126.com; Yan, M.F., E-mail: yanmufu@hit.edu.cn; Wu, Y.Q.

2010-01-15

The effect of rare earth addition in the carrier gas on plasma nitrocarburizing of 17-4PH steel was studied. The microstructure and crystallographically of the phases in the surface layer as well as surface morphology of the nitrocarburized specimens were characterized by optical microscope, X-ray diffraction and scanning tunneling microscope, respectively. The hardness of the surface layer was measured by using a Vickers hardness test. The results show that the incorporation of rare earth elements in the carrier gas can increase the nitrocarburized layer thickness up to 55%, change the phase proportion in the nitrocarburized layer, refine the nitrides in surfacemore » layer, and increase the layer hardness above 100HV. The higher surface hardening effect after rare earth addition is caused by improvement in microstructure and change in the phase proportion of the nitrocarburized layer.« less

Microstructures define melting of molybdenum at high pressures

PubMed Central

Hrubiak, Rostislav; Meng, Yue; Shen, Guoyin

2017-01-01

High-pressure melting anchors the phase diagram of a material, revealing the effect of pressure on the breakdown of the ordering of atoms in the solid. An important case is molybdenum, which has long been speculated to undergo an exceptionally steep increase in melting temperature when compressed. On the other hand, previous experiments showed nearly constant melting temperature as a function of pressure, in large discrepancy with theoretical expectations. Here we report a high-slope melting curve in molybdenum by synchrotron X-ray diffraction analysis of crystalline microstructures, generated by heating and subsequently rapidly quenching samples in a laser-heated diamond anvil cell. Distinct microstructural changes, observed at pressures up to 130 gigapascals, appear exclusively after melting, thus offering a reliable melting criterion. In addition, our study reveals a previously unsuspected transition in molybdenum at high pressure and high temperature, which yields highly textured body-centred cubic nanograins above a transition temperature. PMID:28248309

Crystallization Kinetics in Fluorochloroziroconate Glass-Ceramics

NASA Astrophysics Data System (ADS)

Alvarez, Carlos J.

Annealing fluorochlorozirconate (FCZ) glasses nucleates BaCl2 nanocrystals in the glass matrix, resulting in a nanocomposite glass-ceramic that has optical properties suitable for use as a medical X-ray imaging plate. Understanding the way in which the BaCl¬2 nanocrystal nucleation, growth and phase transformation processes proceed is critical to controlling the optical behavior. However, there is a very limited amount of information about the formation, morphology, and distribution of the nanocrystalline particles in FCZ glass-ceramics. In this thesis, the correlation between the microstructure and the crystallization kinetics of FCZ glass-ceramics, are studied in detail. In situ X-ray diffraction and transmission electron microscopy annealing experiments are used to analyze the crystal structure, size and distribution of BaCl 2 nanocrystals in FCZ glass-ceramics as a function of annealing rate and temperature. Microstructural analysis of the early stages on nucleation identified the formation of both BaCl2 and BaF2 nanocrystals. Annealing FCZ glass-ceramics above 280°C can cause the formation of additional glass matrix phase crystals, their microstructure and the annealing parameters required for their growth are identified. As the crystalline phases grow directly from the glass, small variations in processing of the glass can have a profound influence on the crystallization process. The information obtained from these experiments improves the understanding of the nucleation, growth and phase transformation process of the BaCl¬2 nanocrystals and additional crystalline phases that form in FCZ glass-ceramics, and may help expedite the implementation of FCZ glass-ceramics as next-generation X-ray detectors. Lastly, as these glass-ceramics may one day be commercialized, an investigation into their degradation in different environmental conditions was also performed. The effects of direct contact with water or prolonged exposure to humid environments on the microstructure and the optical properties for FCZ glasses and glass-ceramics was explored.

Microstructural evolution of bainitic steel severely deformed by equal channel angular pressing.

PubMed

Nili-Ahmadabadi, M; Haji Akbari, F; Rad, F; Karimi, Z; Iranpour, M; Poorganji, B; Furuhara, T

2010-09-01

High Si bainitic steel has been received much of interest because of combined ultra high strength, good ductility along with high wear resistance. In this study a high Si bainitic steel (Fe-0.22C-2.0Si-3.0Mn) was used with a proper microstructure which could endure severe plastic deformation. In order to study the effect of severe plastic deformation on the microstructure and properties of bainitic steel, Equal Channel Angular Pressing was performed in two passes at room temperature. Optical, SEM and TEM microscopies were used to examine the microstructure of specimens before and after Equal Channel Angular Pressing processing. X-ray diffraction was used to measure retained austenite after austempering and Equal Channel Angular Pressing processing. It can be seen that retained austenite picks had removed after Equal Channel Angular Pressing which could attributed to the transformation of austenite to martensite during severe plastic deformation. Enhancement of hardness values by number of Equal Channel Angular Pressing confirms this idea.

The effect of heat treatments applied to superstructure porcelain on the mechanical properties and microstructure of lithium disilicate glass ceramics.

PubMed

Özdemir, Hatice; Özdoğan, Alper

2018-01-30

The aim of this study was to investigate that heat treatments with different numbers applied to superstructure porcelain whether effects microstructure and mechanical properties of lithium disilicate ceramic (LDC). Eighty disc-shaped specimens were fabricated from IPS e.max Press. Specimens were fired at heating values of porcelain in different numbers and divided four groups (n=5). Initial Vickers hardness were measured and X-ray diffraction (XRD) analysis was performed. Different surface treatment were applied and then Vickers hardness, surface roughness and environmental scanning electron microscopy (ESEM) analysis were performed. Data were analyzed with Varyans analysis and Tukey HSD test (α=0.05). Initial hardness among groups was no significant different (p>0.05), but hardness and surface roughness after surface treatments were significant different (p<0.05). Lithium disilicate (LD) peaks decrease depended on firing numbers. ESEM observations showed that firing number and surface treatments effect microstructure of LDC. Increasing firing numbers and surface treatments effect the microstructure of LDC.

Note: application of a pixel-array area detector to simultaneous single crystal X-ray diffraction and X-ray absorption spectroscopy measurements.

PubMed

Sun, Cheng-Jun; Zhang, Bangmin; Brewe, Dale L; Chen, Jing-Sheng; Chow, G M; Venkatesan, T; Heald, Steve M

2014-04-01

X-ray diffraction (XRD) and X-ray absorption spectroscopy (XAS) are two main x-ray techniques in synchrotron radiation facilities. In this Note, we present an experimental setup capable of performing simultaneous XRD and XAS measurements by the application of a pixel-array area detector. For XRD, the momentum transfer in specular diffraction was measured by scanning the X-ray energy with fixed incoming and outgoing x-ray angles. By selecting a small fixed region of the detector to collect the XRD signal, the rest of the area was available for collecting the x-ray fluorescence for XAS measurements. The simultaneous measurement of XRD and X-ray absorption near edge structure for Pr0.67Sr0.33MnO3 film was demonstrated as a proof of principle for future time-resolved pump-probe measurements. A static sample makes it easy to maintain an accurate overlap of the X-ray spot and laser pump beam.

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.

Diffraction based method to reconstruct the spectrum of the Thomson scattering x-ray source

NASA Astrophysics Data System (ADS)

Chi, Zhijun; Yan, Lixin; Zhang, Zhen; Zhou, Zheng; Zheng, Lianmin; Wang, Dong; Tian, Qili; Wang, Wei; Nie, Zan; Zhang, Jie; Du, Yingchao; Hua, Jianfei; Shi, Jiaru; Pai, Chihao; Lu, Wei; Huang, Wenhui; Chen, Huaibi; Tang, Chuanxiang

2017-04-01

As Thomson scattering x-ray sources based on the collision of intense laser and relativistic electrons have drawn much attention in various scientific fields, there is an increasing demand for the effective methods to reconstruct the spectrum information of the ultra-short and high-intensity x-ray pulses. In this paper, a precise spectrum measurement method for the Thomson scattering x-ray sources was proposed with the diffraction of a Highly Oriented Pyrolytic Graphite (HOPG) crystal and was demonstrated at the Tsinghua Thomson scattering X-ray source. The x-ray pulse is diffracted by a 15 mm (L) ×15 mm (H)× 1 mm (D) HOPG crystal with 1° mosaic spread. By analyzing the diffraction pattern, both x-ray peak energies and energy spectral bandwidths at different polar angles can be reconstructed, which agree well with the theoretical value and simulation. The higher integral reflectivity of the HOPG crystal makes this method possible for single-shot measurement.

Diffraction based method to reconstruct the spectrum of the Thomson scattering x-ray source.

PubMed

Chi, Zhijun; Yan, Lixin; Zhang, Zhen; Zhou, Zheng; Zheng, Lianmin; Wang, Dong; Tian, Qili; Wang, Wei; Nie, Zan; Zhang, Jie; Du, Yingchao; Hua, Jianfei; Shi, Jiaru; Pai, Chihao; Lu, Wei; Huang, Wenhui; Chen, Huaibi; Tang, Chuanxiang

2017-04-01

As Thomson scattering x-ray sources based on the collision of intense laser and relativistic electrons have drawn much attention in various scientific fields, there is an increasing demand for the effective methods to reconstruct the spectrum information of the ultra-short and high-intensity x-ray pulses. In this paper, a precise spectrum measurement method for the Thomson scattering x-ray sources was proposed with the diffraction of a Highly Oriented Pyrolytic Graphite (HOPG) crystal and was demonstrated at the Tsinghua Thomson scattering X-ray source. The x-ray pulse is diffracted by a 15 mm (L) ×15 mm (H)× 1 mm (D) HOPG crystal with 1° mosaic spread. By analyzing the diffraction pattern, both x-ray peak energies and energy spectral bandwidths at different polar angles can be reconstructed, which agree well with the theoretical value and simulation. The higher integral reflectivity of the HOPG crystal makes this method possible for single-shot measurement.

Precipitation and Dislocation Strengthening Behaviour of Grade X80 Steel for Pipeline with Strain Based Design

NASA Astrophysics Data System (ADS)

Sun, Weihua; Hu, Shu-e.; Li, Guobao; Yu, Hao

This paper analyzes precipitation and dislocation strengthening behaviors of a 27mm thick Niobium-bearing Grade X80 steel plate for strain based design line pipe manufacture. The steel is produced by thermal-mechanical processing (TMCP) and is characterized with granular bainite and polygonal ferrite microstructure. Mechanical properties of both the steel and the UOE pipe are briefly introduced. Transmission electron microscope (TEM) is used to investigate the fine grain structure, distribution of the precipitates and dislocations in the steel. Precipitate morphologies, volume fractions of M(C,N), M3C, CaS, AlN and Cu are extensively studied respectively by Electrolytic Chemical Phase Analysis (ECPA) and X-ray Small Angle Diffraction (X-ray SAD). Dislocations in the steel are characterized with Positron Annihilation analysis. The results prove that precipitation hardening reveal a 58.1MPa strengthening contribution by the precipitates less than 20nm in size. Dislocation hardening is approximately 176MPa to the present studied steel and 198MPa to the pipe.

Microwave absorption properties of Ni/(C, silicides) nanocapsules

PubMed Central

2012-01-01

The microwave absorption properties of Ni/(C, silicides) nanocapsules prepared by an arc discharge method have been studied. The composition and the microstructure of the Ni/(C, silicides) nanocapsules were determined by means of X-ray diffraction, X-ray photoelectric spectroscopy, and transmission electron microscope observations. Silicides, in the forms of SiOx and SiC, mainly exist in the shells of the nanocapsules and result in a large amount of defects at the ‘core/shell’ interfaces as well as in the shells. The complex permittivity and microwave absorption properties of the Ni/(C, silicides) nanocapsules are improved by the doped silicides. Compared with those of Ni/C nanocapsules, the positions of maximum absorption peaks of the Ni/(C, silicides) nanocapsules exhibit large red shifts. An electric dipole model is proposed to explain this red shift phenomenon. PMID:22548846

Irradiation induced formation of VN in CrN thin films

NASA Astrophysics Data System (ADS)

Novaković, M.; Popović, M.; Zhang, K.; Mitrić, M.; Bibić, N.

2015-09-01

Reactively sputtered CrN layer, deposited on Si(1 0 0) wafer, was implanted at room temperature with 80-keV V+ ions to the fluence of 2 × 1017 ions/cm2. After implantation the sample was annealed in a vacuum, for 2 h at 700 °C. The microstructure and chemical composition of CrN films was investigated using Rutherford backscattering spectroscopy, X-ray photoelectron spectroscopy, X-ray diffraction and cross-sectional transmission electron microscopy (conventional and high-resolution), together with fast Fourier transformation analyses. It was found that vanadium atoms are distributed in the sub-surface region of CrN layer, with the maximum concentration at ∼20 nm. After annealing the formation of VN nanoparticles was observed. The nanoparticles are spherical shaped with a size of 8-20 nm in diameter.

Direct laser sintered WC-10Co/Cu nanocomposites

NASA Astrophysics Data System (ADS)

Gu, Dongdong; Shen, Yifu

2008-04-01

In the present work, the direct metal laser sintering (DMLS) process was used to prepare the WC-Co/Cu nanocomposites in bulk form. The WC reinforcing nanoparticles were added in the form of WC-10 wt.% Co composite powder. The microstructural features and mechanical properties of the laser-sintered sample were characterized by X-ray diffraction (XRD), atomic force microscope (AFM), scanning electron microscope (SEM), energy dispersive X-ray spectroscope (EDX), and nanoindentation tester. It showed that the original nanometric nature of the WC reinforcing particulates was well retained without appreciable grain growth after laser processing. A homogeneous distribution of the WC reinforcing nanoparticles with a coherent particulate/matrix interfacial bonding was obtained in the laser-sintered structure. The 94.3% dense nanocomposites have a dynamic nanohardness of 3.47 GPa and a reduced elastic modulus of 613.42 GPa.

Structural characterization and mechanical performance of calcium phosphate scaffolds and natural bones: a comparative study.

PubMed

Fuentes, Elena; Sáenz de Viteri, Virginia; Igartua, Amaya; Martinetti, Roberta; Dolcini, Laura; Barandika, Gotzone

2010-01-01

The knowledge of the mechanical response of bones and their substitutes is pertinent to numerous medical problems. Understanding the effects of mechanical influence on the body is the first step toward developing innovative treatment and rehabilitation concepts for orthopedic disorders. This was a comparative study of 5 synthetic scaffolds based on porous calcium phosphates and natural bones, with regard to their microstructural, chemical, and mechanical characterizations. The structural and chemical characterizations of the scaffolds were examined by means of X-ray diffraction, scanning electron microscopy, and X-ray spectroscopy analysis. The mechanical characterization of bones and bone graft biomaterials was carried out through compression tests using samples with noncomplex geometry. Analysis of the chemical composition, surface features, porosity, and compressive strength indicates that hydroxyapatite-based materials and trabecular bone have similar properties.

Specific physical and chemical properties of two modifications of poly(N-vinylcaprolcatam)

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

Chihacheva, I. P.; Timaeva, O. I.; Kuz’micheva, G. M., E-mail: galina-kuzmicheva@list.ru

2016-05-15

Two modifications of poly(N-vinylcaprolactam)—PVCL25 and PVCL40 (drying of a PVCL solution at 25 and 40°C, respectively)—as powdered films and their solutions were systematically investigated for the first time. Powders were studied by X-ray diffraction, IR spectroscopy, scanning electron microscopy, low-temperature krypton adsorption, and differential scanning calorimetry. Solutions were studied by smallangle X-ray scattering and dynamic light scattering. It was demonstrated that powders of PVCL25 and PVCL40 differ in the characteristics of the sub- and microstructure and in the water content and the solutions differ in the particle size. The relationships between the characteristics of the systems in the solid andmore » liquid state and between the hydrodynamic diameter of PVCL particles in solution and their coagulation time were found.« less

Morphology and structure of Ti-doped diamond films prepared by microwave plasma chemical vapor deposition

NASA Astrophysics Data System (ADS)

Liu, Xuejie; Lu, Pengfei; Wang, Hongchao; Ren, Yuan; Tan, Xin; Sun, Shiyang; Jia, Huiling

2018-06-01

Ti-doped diamond films were deposited through a microwave plasma chemical vapor deposition (MPCVD) system for the first time. The effects of the addition of Ti on the morphology, microstructure and quality of diamond films were systematically investigated. Secondary ion mass spectrometry results show that Ti can be added to diamond films through the MPCVD system using tetra n-butyl titanate as precursor. The spectra from X-ray diffraction, Raman spectroscopy, and X-ray photoelectron spectroscopy and the images from scanning electron microscopy of the deposited films indicate that the diamond phase clearly exists and dominates in Ti-doped diamond films. The amount of Ti added obviously influences film morphology and the preferred orientation of the crystals. Ti doping is beneficial to the second nucleation and the growth of the (1 1 0) faceted grains.

X-ray and neutron diffraction studies of crystallinity in hydroxyapatite coatings.

PubMed

Girardin, E; Millet, P; Lodini, A

2000-02-01

To standardize industrial implant production and make comparisons between different experimental results, we have to be able to quantify the crystallinity of hydroxyapatite. Methods of measuring crystallinity ratio were developed for various HA samples before and after plasma spraying. The first series of methods uses X-ray diffraction. The advantage of these methods is that X-ray diffraction equipment is used widely in science and industry. In the second series, a neutron diffraction method is developed and the results recorded are similar to those obtained by the modified X-ray diffraction methods. The advantage of neutron diffraction is the ability to obtain measurements deep inside a component. It is a nondestructive method, owing to the very low absorption of neutrons in most materials. Copyright 2000 John Wiley & Sons, Inc.

X-ray Diffraction Gratings for Astrophysics

NASA Astrophysics Data System (ADS)

Paerels, Frits

2010-12-01

Over the past year, we have celebrated the tenth anniversary of the Chandra and XMM-Newton X-ray observatories. Both carry powerful, novel diffraction grating spectrometers, which have opened true X-ray spectroscopy for astrophysics. I will describe the design and operation of these instruments, as the background to some of the beautiful results they have produced. But these designs do not exhaust the versatility and essential simplicity of diffraction grating spectrometers, and I will discuss applications for the International X-ray Observatory IXO.

Influence of Sn doping in BaSnxTi1-xO3 ceramics on microstructural and dielectric properties

NASA Astrophysics Data System (ADS)

Ansari, Mohd. Azaj; Sreenivas, K.

2018-05-01

BaSnxTi1-x O3 solid solutions with varying Sn content (x = 0.00, 0.05, 0.15, 0.25) prepared by solid state reaction method have been studied for their structural and dielectric properties. X-ray diffraction and Raman spectroscopic analysis show composition induced modifications in the crystallographic structure, and with increasing Sn content the structure changes from tetragonal to cubic structure. The tetragonal distortion decreases with increasing Sn, and the structure becomes purely cubic for x =0.25. Changes in the structure are reflected in the temperature dependent dielectric properties. For increasing Sn content the peak dielectric constant is found to increase and the phase transition temperature (Tc) decreases to lower temperature. The purely cubic structure with x=0.25 shows a diffused phased transition.

Amorphous boron gasket in diamond anvil cell research

NASA Astrophysics Data System (ADS)

Lin, Jung-Fu; Shu, Jinfu; Mao, Ho-kwang; Hemley, Russell J.; Shen, Guoyin

2003-11-01

Recent advances in high-pressure diamond anvil cell experiments include high-energy synchrotron x-ray techniques as well as new cell designs and gasketing procedures. The success of high-pressure experiments usually depends on a well-prepared sample, in which the gasket plays an important role. Various gasket materials such as diamond, beryllium, rhenium, and stainless steel have been used. Here we introduce amorphous boron as another gasket material in high-pressure diamond anvil cell experiments. We have applied the boron gasket for laser-heating x-ray diffraction, radial x-ray diffraction, nuclear resonant inelastic x-ray scattering, and inelastic x-ray scattering. The high shear strength of the amorphous boron maximizes the thickness of the sample chamber and increases the pressure homogeneity, improving the quality of high-pressure data. Use of amorphous boron avoids unwanted x-ray diffraction peaks and reduces the absorption of incident and x rays exiting the gasket material. The high quality of the diffraction patterns makes it possible to refine the cell parameters with powder x-ray diffraction data under high pressure and high temperature. The reactivity of boron prevents its use at high temperatures, however. When heated, boron may also react with the specimen to produce unwanted phases. The relatively porous boron starting material at ambient conditions also poses some challenges for sample preparation.

Phase separation within NiSiN coatings during reactive HiPIMS discharges: A new pathway to grow NixSi nanocrystals composites at low temperature

NASA Astrophysics Data System (ADS)

Keraudy, J.; Boyd, R. D.; Shimizu, T.; Helmersson, U.; Jouan, P.-Y.

2018-10-01

The precise control of the growth nanostructured thin films at low temperature is critical for the continued development of microelectronic enabled devices. In this study, nanocomposite Ni-Si-N thin films were deposited at low temperature by reactive high-power impulse magnetron sputtering. A composite Ni-Si target (15 at.% Si) in combination with a Ar/N2 plasma were used to deposit films onto Si(0 0 1) substrates, without any additional substrate heating or any post-annealing. The films microstructure changes from a polycrystalline to nanocomposite structure when the nitrogen content exceeds 16 at.%. X-ray diffraction and (scanning) transmission electron microscopy analyses reveal that the microstructure consists of nanocrystals, NixSi (x > 1) 7-8 nm in size, embedded in an amorphous SiNx matrix. It is proposed that this nanostructure is formed at low temperatures due to the repeated-nucleation of NixSi nanocrystals, the growth of which is restricted by the formation of the SiNx phase. X-ray photoelectron spectroscopy revealed the trace presence of a ternary solid solution mainly induced by the diffusion of Ni into the SiNx matrix. Four-probe electrical measurements reveal all the deposited films are electrically conducting.

X-Ray Sum Frequency Diffraction for Direct Imaging of Ultrafast Electron Dynamics

NASA Astrophysics Data System (ADS)

Rouxel, Jérémy R.; Kowalewski, Markus; Bennett, Kochise; Mukamel, Shaul

2018-06-01

X-ray diffraction from molecules in the ground state produces an image of their charge density, and time-resolved x-ray diffraction can thus monitor the motion of the nuclei. However, the density change of excited valence electrons upon optical excitation can barely be monitored with regular diffraction techniques due to the overwhelming background contribution of the core electrons. We present a nonlinear x-ray technique made possible by novel free electron laser sources, which provides a spatial electron density image of valence electron excitations. The technique, sum frequency generation carried out with a visible pump and a broadband x-ray diffraction pulse, yields snapshots of the transition charge densities, which represent the electron density variations upon optical excitation. The technique is illustrated by ab initio simulations of transition charge density imaging for the optically induced electronic dynamics in a donor or acceptor substituted stilbene.

Characterization of beryllium deformation using in-situ x-ray diffraction

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

Magnuson, Eric Alan; Brown, Donald William; Clausen, Bjorn

2015-08-24

Beryllium’s unique mechanical properties are extremely important in a number of high performance applications. Consequently, accurate models for the mechanical behavior of beryllium are required. However, current models are not sufficiently microstructure aware to accurately predict the performance of beryllium under a range of processing and loading conditions. Previous experiments conducted using the SMARTS and HIPPO instruments at the Lujan Center(LANL), have studied the relationship between strain rate and texture development, but due to the limitations of neutron diffraction studies, it was not possible to measure the response of the material in real-time. In-situ diffraction experiments conducted at the Advancedmore » Photon Source have allowed the real time measurement of the mechanical response of compressed beryllium. Samples of pre-strained beryllium were reloaded orthogonal to their original load path to show the reorientation of already twinned grains. Additionally, the in-situ experiments allowed the real time tracking of twin evolution in beryllium strained at high rates. The data gathered during these experiments will be used in the development and validation of a new, microstructure aware model of the constitutive behavior of beryllium.« less

Mn-coatings on the micro-pore formed Ti-29Nb-xHf alloys by RF-magnetron sputtering for dental applications

NASA Astrophysics Data System (ADS)

Park, Seon-Yeong; Choe, Han-Cheol

2018-02-01

In this study, Mn-coatings on the micro-pore formed Ti-29Nb-xHf alloys by RF-magnetrons sputtering for dental applications were studied using different experimental techniques. Mn coating films were formed on Ti-29Nb-xHf alloys by a radio frequency magnetron sputtering technique for 0, 1, 3, and 5 min at 45 W. The microstructure, composition, and phase structure of the coated alloys were examined by optical microscopy, field emission scanning electron microscopy, X-ray diffraction, and energy-dispersive X-ray spectroscopy. The microstructure of Ti-29Nb alloy showed α" phase in the needle-like structure and Ti-29Nb-15Hf alloy showed β phase in the equiaxed structure. As the sputtering time increased, the circular particles of Mn coatings on the Ti-29Nb alloy increased at inside and outside surfaces. As the sputtering time increased, [Mn + Ca/P] ratio of the plasma electrolytic oxidized films in Ti- 29Nb-xHf alloys increased. The corrosion potential (Ecorr) of Mn coatings on the Ti-29Nb alloy showed higher than that of Mn coatings on the Ti-29Nb-15Hf alloy. The passive current density (Ipass) of the Mn coating on the Ti-29Nb alloy and Mn coatings on the Ti-29Nb-15Hf alloy was less noble than the non-Mn coated Ti-29Nb and Ti-29Nb-15Hf alloys surface.

Bottom electrodes dependence of microstructures and dielectric properties of compositionally graded (Ba{sub 1-x}Sr{sub x})TiO{sub 3} thin films

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

Zhang Tianjin; Wang Jinzhao; Zhang Baishun

2008-03-04

Compositionally graded (Ba{sub 1-x}Sr{sub x})TiO{sub 3} (BST) thin films, with x decreasing from 0.3 to 0, were deposited on Pt/Ti/SiO{sub 2}/Si and Ru/SiO{sub 2}/Si substrates by radio frequency magnetron sputtering technology. The microstructure and dielectric properties of the graded BST thin films were investigated. It was found that the films on Ru electrode have better crystallization, and that RuO{sub 2} is present between the Ru bottom electrode and the graded BST thin films by X-ray diffraction and SEM analysis. Dielectric measurement reveals that the graded BST thin films deposited on Ru bottom electrode have higher dielectric constant and tunability. Themore » enhanced dielectric behavior is attributed to better crystallization as well as smaller space charge capacitance width and the formation of RuO{sub 2} that is more compatible with the BST films. The graded BST films on Ru electrode show higher leakage current due to lower barrier height and rougher surface of bottom electrode.« less

Effect of Friction Stir Processing on Microstructure and Mechanical Properties of AZ91C Magnesium Cast Alloy Weld Zone

NASA Astrophysics Data System (ADS)

Hassani, Behzad; Karimzadeh, Fathallah; Enayati, Mohammad Hossein; Sabooni, Soheil; Vallant, Rudolf

2016-07-01

In this study, friction stir processing (FSP) was applied to the GTAW (TIG)-welded AZ91C cast alloy to refine the microstructure and optimize the mechanical properties of the weld zone. Microstructural investigation of the samples was performed by optical microscopy and the phases in the microstructure were determined by x-ray diffraction (XRD). The microstructural evaluations showed that FSP destroys the coarse dendritic microstructure. Furthermore, it dissolves the secondary hard and brittle β-Mg17Al12 phase existing at grain boundaries of the TIG weld zone. The closure and decrease in amount of porosities along with the elimination of the cracks in the microstructure were observed. These changes were followed by a significant grain refinement to an average value of 11 µm. The results showed that the hardness values increased to the mean ones, respectively, for as-cast (63 Hv), TIG weld zone (67 Hv), and stir zone (79 Hv). The yield and ultimate strength were significantly enhanced after FSP. The fractography evaluations, by scanning electron microscopy (SEM), indicated to a transition from brittle to ductile fracture surface after applying FSP to the TIG weld zone.

Texture and structure contribution to low-temperature plasticity enhancement of Mg-Al-Zn-Mn Alloy MA2-1hp after ECAP and annealing

NASA Astrophysics Data System (ADS)

Serebryany, V. N.; D'yakonov, G. S.; Kopylov, V. I.; Salishchev, G. A.; Dobatkin, S. V.

2013-05-01

Equal channel angular pressing (ECAP) in magnesium alloys due to severe plastic shear deformations provides both grain refinement and the slope of the initial basal texture at 40°-50° to the pressing direction. These changes in microstructure and texture contribute to the improvement of low-temperature plasticity of the alloys. Quantitative texture X-ray diffraction analysis and diffraction of backscattered electrons are used to study the main textural and structural factors responsible for enhanced low-temperature plasticity based on the example of magnesium alloy MA2-1hp of the Mg-Al-Zn-Mn system. The possible mechanisms of deformation that lead to this positive effect are discussed.

Improvement of critical current density in thallium-based (Tl,Bi)Sr(1.6)Ba(0.4)Ca2Cu3O(x) superconductors

NASA Technical Reports Server (NTRS)

Ren, Z. F.; Wang, C. A.; Wang, J. H.; Miller, D. J.; Goretta, K. C.

1995-01-01

Epitaxial (Tl,Bi)Sr(1.6)Ba(0.4)Ca2Cu3O(x) ((Tl,Bi)-1223) thin films on (100) single crystal LaAlO3 substrates were synthesized by a two-step procedure. Phase development, microstructure, and relationships between film and substrate were studied by X-ray diffraction (XRD), scanning electron microscopy (SEM), and transmission electron microscopy (TEM). Resistance versus temperature, zero-field-cooled and field cooled magnetization, and transport critical current density (J(sub c)) were measured. The zero-resistance temperature was 105-111 K. J(sub c) at 77 K and zero field was greater than 2 x 10(exp 6) A/sq cm. The films exhibited good flux pinning properties.

Direct bandgap materials based on the thin films of SexTe100 − x nanoparticles

PubMed Central

2012-01-01

In this study, we fabricated thin films of SexTe100 − x (x = 0, 3, 6, 9, 12, and 24) nanoparticles using thermal evaporation technique. The results obtained by X-ray diffraction show that the as-synthesized nanoparticles have polycrystalline structure, but their crystallinity decreases by increasing the concentration of Se. They were found to have direct bandgap (Eg), whose value increases by increasing the Se content. These results are completely different than those obtained in the films of SexTe100 − x microstructure counterparts. Photoluminescence and Raman spectra for these films were also demonstrated. The remarkable results obtained in these nanoparticles specially their controlled direct bandgap might be useful for the development of optical disks and other semiconductor devices. PMID:22978714

Effect of processing induced particle alignment on the fracture toughness and fracture behavior of multiphase dental ceramics.

PubMed

Gonzaga, Carla C; Okada, Cristina Yuri; Cesar, Paulo F; Miranda, Walter G; Yoshimura, Humberto N

2009-11-01

To investigate the processing induced particle alignment on fracture behavior of four multiphase dental ceramics (one porcelain, two glass-ceramics and a glass-infiltrated-alumina composite). Disks (Ø12 mm x 1.1mm-thick) and bars (3 mm x 4 mm x 20 mm) of each material were processed according to manufacturer instructions, machined and polished. Fracture toughness (K(Ic)) was determined by the indentation strength method using 3-point bending and biaxial flexure fixtures for the fracture of bars and disks, respectively. Microstructural and fractographic analyses were performed with scanning electron microscopy, energy dispersive spectroscopy and X-ray diffraction. The isotropic microstructure of the porcelain and the leucite-based glass-ceramic resulted in similar fracture toughness values regardless of the specimen geometry. On the other hand, materials containing second-phase particles with high aspect ratio (lithium disilicate glass-ceramic and glass-infiltrated-alumina composite) showed lower fracture toughness for disk specimens compared to bars. For the lithium disilicate glass-ceramic disks, it was demonstrated that the occurrence of particle alignment during the heat-pressing procedure resulted in an unfavorable pattern that created weak microstructural paths during the biaxial test. For the glass-infiltrated-alumina composite, the microstructural analysis showed that the large alumina platelets tended to align their large surfaces perpendicularly to the direction of particle deposition during slip casting of green preforms. The fracture toughness of dental ceramics with anisotropic microstructure should be determined by means of biaxial testing, since it results in lower values.

Surface-engineered core-shell nano-size ferrites and their antimicrobial activity

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

Baraliya, Jagdish D., E-mail: jdbaraliya@yahoo.co.in; Joshi, Hiren H., E-mail: jdbaraliya@yahoo.co.in

We report the results of biological study on core-shell structured MFe{sub 2}O{sub 4} (where M = Co, Mn, Ni) nanoparticles and influence of silica- DEG dual coating on their antimicrobial activity. Spherical MFe{sub 2}O{sub 4} nanoparticles were prepared via a Co-precipitation method. The microstructures and morphologies of these nanoparticles were studied by x-ray diffraction and FTIR. The antimicrobial activity study carried out in nutrient agar medium with addition of antimicrobial synthesis compound which is tested for its activity against different types of bacteria.

Application of Laser Treatment for Hardening Parts of Gas Turbine Engines from Titanium Alloys

NASA Astrophysics Data System (ADS)

Girzhon, V. V.; Ovchinnikov, A. V.

2017-03-01

X-ray diffraction analysis and light microscopy are used to study the structure of surface layers of helically extruded specimens of titanium alloy VT25U after laser fusion of the surface. It is shown that the rates of cooling of the melt promote formation of a martensitic α″-phase in the zone of laser fusion and of a submicrocrystalline microstructure. The microhardness in the zone of fusion of the initial specimens exceeds the microhardness of the specimens after the extrusion.

Effect of preparation conditions on the nanostructure of hydroxyapatite and brushite phases

NASA Astrophysics Data System (ADS)

Mansour, S. F.; El-dek, S. I.; Ahmed, M. A.; Abd-Elwahab, S. M.; Ahmed, M. K.

2016-10-01

Hydroxyapatite (HAP) and dicalcium phosphate dihydrate (brushite) nanoparticles were prepared by co-precipitation method. The obtained products were characterized by X-ray powder diffraction (XRD), Fourier transformation infra-red spectroscopy (FTIR) and thermo-gravimetric analysis (TGA). Scanning electron microscopy (SEM) and transmission electron microscope (TEM) were used to investigate the morphology of the powdered samples as well as their microstructure, respectively. Brushite samples were obtained in a spherical shape, while hydroxyapatite was formed in a needle and rice shape depending on the pH value.

Nondestructive evaluation of plasma-sprayed thermal barrier coatings

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

Andrews, D.J.; Taylor, J.A.T.

Acoustic emission has been used as a nondestructive evaluation technique to examine the thermal shock response of thermal barrier coatings. In this study, samples of partially stabilized zirconia powder were sprayed and acoustic emission (AE) data were taken in a series of thermal shock tests in an effort to correlate AE with a given failure mechanism. Microstructural evidence was examined using parallel beam x-ray diffraction and optical microscopy. The AE data are discussed in terms of cumulative amplitude distributions and the use of this technique to characterize fracture events.

Surface modification of 17-4PH stainless steel by DC plasma nitriding and titanium nitride film duplex treatment

NASA Astrophysics Data System (ADS)

Qi, F.; Leng, Y. X.; Huang, N.; Bai, B.; Zhang, P. Ch.

2007-04-01

17-4PH stainless steel was modified by direct current (DC) plasma nitriding and titanium nitride film duplex treatment in this study. The microstructure, wear resistance and corrosion resistance were characterized by X-ray diffraction (XRD), pin-on-disk tribological test and polarization experiment. The results revealed that the DC plasma nitriding pretreatment was in favor of improving properties of titanium nitride film. The corrosion resistance and wear resistance of duplex treatment specimen was more superior to that of only coated titanium nitride film.

Surface-engineered core-shell nano-size ferrites and their antimicrobial activity

NASA Astrophysics Data System (ADS)

Baraliya, Jagdish D.; Joshi, Hiren H.

2014-04-01

We report the results of biological study on core-shell structured MFe2O4 (where M = Co, Mn, Ni) nanoparticles and influence of silica- DEG dual coating on their antimicrobial activity. Spherical MFe2O4 nanoparticles were prepared via a Co-precipitation method. The microstructures and morphologies of these nanoparticles were studied by x-ray diffraction and FTIR. The antimicrobial activity study carried out in nutrient agar medium with addition of antimicrobial synthesis compound which is tested for its activity against different types of bacteria.

Development of an adaptable coherent x-ray diffraction microscope with the emphasis on imaging hydrated specimens.

PubMed

Nam, Daewoong; Park, Jaehyun; Gallagher-Jones, Marcus; Shimada, Hiroki; Kim, Sangsoo; Kim, Sunam; Kohmura, Yoshiki; Ishikawa, Tetsuya; Song, Changyong

2013-11-01

This paper describes the development of a versatile coherent x-ray diffraction microscope capable of imaging biological specimens in solution. The microscope is a flexible platform accommodating various conditions, from low vacuum (10(-2) Pa) to helium gas filled ambient pressure. This flexibility greatly expands the application area, from in situ materials science to biology systems in their native state, by significantly relaxing restrictions to the sample environment. The coherent diffraction microscope has been used successfully to image a yeast cell immersed in buffer solution. We believe that the design of this coherent diffraction microscope can be directly adapted to various platforms such as table top soft x-ray laser, synchrotron x-ray sources, and x-ray free electron laser with minor relevant adjustments.

Development of an adaptable coherent x-ray diffraction microscope with the emphasis on imaging hydrated specimens

NASA Astrophysics Data System (ADS)

Nam, Daewoong; Park, Jaehyun; Gallagher-Jones, Marcus; Shimada, Hiroki; Kim, Sangsoo; Kim, Sunam; Kohmura, Yoshiki; Ishikawa, Tetsuya; Song, Changyong

2013-11-01

This paper describes the development of a versatile coherent x-ray diffraction microscope capable of imaging biological specimens in solution. The microscope is a flexible platform accommodating various conditions, from low vacuum (10-2 Pa) to helium gas filled ambient pressure. This flexibility greatly expands the application area, from in situ materials science to biology systems in their native state, by significantly relaxing restrictions to the sample environment. The coherent diffraction microscope has been used successfully to image a yeast cell immersed in buffer solution. We believe that the design of this coherent diffraction microscope can be directly adapted to various platforms such as table top soft x-ray laser, synchrotron x-ray sources, and x-ray free electron laser with minor relevant adjustments.

Graded Microstructure and Mechanical Performance of Ti/N-Implanted M50 Steel with Polyenergy.

PubMed

Jie, Jin; Shao, Tianmin

2017-10-19

M50 bearing steels were alternately implanted with Ti⁺ and N⁺ ions using solid and gas ion sources of implantation system, respectively. N-implantation was carried out at an energy of about 80 keV and a fluence of 2 × 10 17 ions/cm², and Ti-implantation at an energy of about 40-90 keV and a fluence of 2 × 10 17 ions/cm². The microstructures of modification layers were analyzed by grazing-incidence X-ray diffraction, auger electron spectroscopy, X-ray photoelectron spectroscopy, and transmission electron microscopy. The results showed that the gradient structure was formed under the M50 bearing steel subsurface, along the ion implantation influence zone composed of amorphous, nanocrystalline, and gradient-refinement phases. A layer of precipitation compounds like TiN is formed. In addition, nano-indentation hardness and tribological properties of the gradient structure subsurface were examined using a nano-indenter and a friction and wear tester. The nano-indentation hardness of N + Ti-co-implanted sample is above 12 GPa, ~1.3 times than that of pristine samples. The friction coefficient is smaller than 0.2, which is 22.2% of that of pristine samples. The synergism between precipitation-phase strengthening and gradient microstructure is the main mechanism for improving the mechanical properties of M50 materials.

Graded Microstructure and Mechanical Performance of Ti/N-Implanted M50 Steel with Polyenergy

PubMed Central

Jie, Jin; Shao, Tianmin

2017-01-01

M50 bearing steels were alternately implanted with Ti+ and N+ ions using solid and gas ion sources of implantation system, respectively. N-implantation was carried out at an energy of about 80 keV and a fluence of 2 × 1017 ions/cm2, and Ti-implantation at an energy of about 40–90 keV and a fluence of 2 × 1017 ions/cm2. The microstructures of modification layers were analyzed by grazing-incidence X-ray diffraction, auger electron spectroscopy, X-ray photoelectron spectroscopy, and transmission electron microscopy. The results showed that the gradient structure was formed under the M50 bearing steel subsurface, along the ion implantation influence zone composed of amorphous, nanocrystalline, and gradient-refinement phases. A layer of precipitation compounds like TiN is formed. In addition, nano-indentation hardness and tribological properties of the gradient structure subsurface were examined using a nano-indenter and a friction and wear tester. The nano-indentation hardness of N + Ti-co-implanted sample is above 12 GPa, ~1.3 times than that of pristine samples. The friction coefficient is smaller than 0.2, which is 22.2% of that of pristine samples. The synergism between precipitation-phase strengthening and gradient microstructure is the main mechanism for improving the mechanical properties of M50 materials. PMID:29048360

Thin Film Research. Volume 1

DTIC Science & Technology

1985-05-30

Order (FECO) ......... 23 3. X -Ray Diffraction ............................... 26 4. Transmission Electron Microscopy (TEM) ............... 26 5...remained amorphous after bombardment, as evidenced by X - ray diffraction, and showed no other changes. 0 (2) For Sb203, the crystallite size was reduced...main effect on MgF2 was the reduction in crystallite size. The films were too thir. for meaningful x - ray diffraction analysis. Durability and

X-Ray Diffraction and the Discovery of the Structure of DNA

ERIC Educational Resources Information Center

Crouse, David T.

2007-01-01

A method is described for teaching the analysis of X-ray diffraction of DNA through a series of steps utilizing the original methods used by James Watson, Francis Crick, Maurice Wilkins and Rosalind Franklin. The X-ray diffraction pattern led to the conclusion of the basic helical structure of DNA and its dimensions while basic chemical principles…

High Resolution X-Ray Diffraction of Macromolecules with Synchrotron Radiation

NASA Technical Reports Server (NTRS)

Stojanoff, Vivian; Boggon, Titus; Helliwell, John R.; Judge, Russell; Olczak, Alex; Snell, Edward H.; Siddons, D. Peter; Rose, M. Franklin (Technical Monitor)

2000-01-01

We recently combined synchrotron-based monochromatic X-ray diffraction topography methods with triple axis diffractometry and rocking curve measurements: high resolution X-ray diffraction imaging techniques, to better understand the quality of protein crystals. We discuss these methods in the light of results obtained on crystals grown under different conditions. These non destructive techniques are powerful tools in the characterization of the protein crystals and ultimately will allow to improve, develop, and understand protein crystal growth. High resolution X-ray diffraction imaging methods will be discussed in detail in light of recent results obtained on Hen Egg White Lysozyme crystals and other proteins.

Hard X-ray polarizer to enable simultaneous three-dimensional nanoscale imaging of magnetic structure and lattice strain

DOE PAGES

Logan, Jonathan; Harder, Ross; Li, Luxi; ...

2016-01-01

Recent progress in the development of dichroic Bragg coherent diffractive imaging, a new technique for simultaneous three-dimensional imaging of strain and magnetization at the nanoscale, is reported. This progress includes the installation of a diamond X-ray phase retarder at beamline 34-ID-C of the Advanced Photon Source. Here, the performance of the phase retarder for tuning X-ray polarization is demonstrated with temperature-dependent X-ray magnetic circular dichroism measurements on a gadolinium foil in transmission and on a Gd 5Si 2Ge 2crystal in diffraction geometry with a partially coherent, focused X-ray beam. Feasibility tests for dichroic Bragg coherent diffractive imaging are presented. Thesemore » tests include (1) using conventional Bragg coherent diffractive imaging to determine whether the phase retarder introduces aberrations using a nonmagnetic gold nanocrystal as a control sample, and (2) collecting coherent diffraction patterns of a magnetic Gd 5Si 2Ge 2nanocrystal with left- and right-circularly polarized X-rays. Future applications of dichroic Bragg coherent diffractive imaging for the correlation of strain and lattice defects with magnetic ordering and inhomogeneities are considered.« less

Influence of yttrium content on the location of rare earth ions in LYSO:Ce crystals

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

Ding, Dongzhou, E-mail: dongzhou_ding@mail.sic.ac.cn; R and D Center of Shanghai Institute of Ceramics, No. 588 Heshuo Road, Shanghai 201899; Weng, Linhong

2014-01-15

Single-crystal X-ray diffraction (SCD), X-ray fluorescence (XRF), inductively coupled plasma optical emission spectroscopy (ICP-OES) and X-ray excited luminescence (XEL) measurements were performed to investigate structure details and segregation coefficients of (Lu{sub 1−x}Y{sub x}){sub 2}SiO{sub 5}:Ce (x=0 at%, 8.7 at%, 25.7 at%, 44.7 at%, 65.7 at%, 87.9 at% and 100 at%). Y{sup 3+} cations were found to have a preferential occupation for RE1 site (7-oxygen-coordinated) over RE2 site (6-oxygen-coordinated), which results in a greater increase of cell parameter c than that of a with increase in Y content due to LYSO's microstructure characteristics. Results presented here revealed that the less themore » difference in electronegativity and effective ionic radius between the two ions, the easier substitution of one ion by the other, and hence the higher segregation coefficients. Besides, the contribution of luminescence of Ce1 and Ce2 in the whole XEL was evaluated, and the location of Ce{sup 3+} ion was discussed. - Graphical abstract: Segregation coefficients of (Lu{sub 1−x}Y{sub x}){sub 2}SiO{sub 5}:Cce:italic> at RT/ce:italic>. Display Omitted.« less

Effects of gamma-ray irradiation on the optical properties of amorphous Se100-xHgx thin films

NASA Astrophysics Data System (ADS)

Ahmad, Shabir; Islam, Shama; Nasir, Mohd.; Asokan, K.; Zulfequar, M.

2018-06-01

In this study, the thermal quenching technique was employed to prepare bulk samples of Se100-xHgx (x = 0, 5, 10, 15). Thin films with a thickness of ∼250 nm were deposited on glass substrates using the thermal evaporation technique. These films were irradiated with gamma rays at doses of 25-100 kGy. The elemental compositions of the as-deposited thin films were confirmed by energy dispersive X-ray analysis and Rutherford backscattering spectrometry. X-ray diffraction analysis confirmed the crystalline nature of these thin films upto the dose of 75 kGy. Fourier transform-infrared spectroscopy showed that the concentration of defects decreased after gamma irradiation. Microstructural analysis by field emission scanning electron microscopy indicated that the grain size increases after irradiation. Optical study based on spectrophotometry showed that the optical band gap values of these films increase after the addition of Hg whereas they decrease after gamma irradiation. We found that the absorption coefficient increases with doses up to 75 kGy but decreases at higher doses. These remarkable shifts in the optical band gap and absorption coefficient values are interpreted in terms of the creation and annihilation of defects, which are the main effects produced by gamma irradiation.

Three Dimensional Variable-Wavelength X-Ray Bragg Coherent Diffraction Imaging

DOE PAGES

Cha, W.; Ulvestad, A.; Allain, M.; ...

2016-11-23

Here, we present and demonstrate a formalism by which three-dimensional (3D) Bragg x-ray coherent diffraction imaging (BCDI) can be implemented without moving the sample by scanning the energy of the incident x-ray beam. This capability is made possible by introducing a 3D Fourier transform that accounts for x-ray wavelength variability. We also demonstrate the approach by inverting coherent Bragg diffraction patterns from a gold nanocrystal measured with an x-ray energy scan. Furthermore, variable-wavelength BCDI will expand the breadth of feasible in situ 3D strain imaging experiments towards more diverse materials environments, especially where sample manipulation is difficult.

Synchrotron X-Ray Diffraction Analysis of Meteorites in Thin Section: Preliminary Results

NASA Technical Reports Server (NTRS)

Treiman, A. H.; Lanzirotti, A.; Xirouchakis, D.

2004-01-01

X-ray diffraction is the pre-eminent technique for mineral identification and structure determination, but is difficult to apply to grains in thin section, the standard meteorite preparation. Bright focused X-ray beams from synchrotrons have been used extensively in mineralogy and have been applied to extraterrestrial particles. The intensity and small spot size achievable in synchrotron X-ray beams makes them useful for study of materials in thin sections. Here, we describe Synchrotron X-ray Diffraction (SXRD) in thin section as done at the National Synchrotron Light Source, and cite examples of its value for studies of meteorites in thin section.

Three Dimensional Variable-Wavelength X-Ray Bragg Coherent Diffraction Imaging

NASA Astrophysics Data System (ADS)

Cha, W.; Ulvestad, A.; Allain, M.; Chamard, V.; Harder, R.; Leake, S. J.; Maser, J.; Fuoss, P. H.; Hruszkewycz, S. O.

2016-11-01

We present and demonstrate a formalism by which three-dimensional (3D) Bragg x-ray coherent diffraction imaging (BCDI) can be implemented without moving the sample by scanning the energy of the incident x-ray beam. This capability is made possible by introducing a 3D Fourier transform that accounts for x-ray wavelength variability. We demonstrate the approach by inverting coherent Bragg diffraction patterns from a gold nanocrystal measured with an x-ray energy scan. Variable-wavelength BCDI will expand the breadth of feasible in situ 3D strain imaging experiments towards more diverse materials environments, especially where sample manipulation is difficult.

Three Dimensional Variable-Wavelength X-Ray Bragg Coherent Diffraction Imaging.

PubMed

Cha, W; Ulvestad, A; Allain, M; Chamard, V; Harder, R; Leake, S J; Maser, J; Fuoss, P H; Hruszkewycz, S O

2016-11-25

We present and demonstrate a formalism by which three-dimensional (3D) Bragg x-ray coherent diffraction imaging (BCDI) can be implemented without moving the sample by scanning the energy of the incident x-ray beam. This capability is made possible by introducing a 3D Fourier transform that accounts for x-ray wavelength variability. We demonstrate the approach by inverting coherent Bragg diffraction patterns from a gold nanocrystal measured with an x-ray energy scan. Variable-wavelength BCDI will expand the breadth of feasible in situ 3D strain imaging experiments towards more diverse materials environments, especially where sample manipulation is difficult.

In-situ X-ray diffraction system using sources and detectors at fixed angular positions

DOEpatents

Gibson, David M [Voorheesville, NY; Gibson, Walter M [Voorheesville, NY; Huang, Huapeng [Latham, NY

2007-06-26

An x-ray diffraction technique for measuring a known characteristic of a sample of a material in an in-situ state. The technique includes using an x-ray source for emitting substantially divergent x-ray radiation--with a collimating optic disposed with respect to the fixed source for producing a substantially parallel beam of x-ray radiation by receiving and redirecting the divergent paths of the divergent x-ray radiation. A first x-ray detector collects radiation diffracted from the sample; wherein the source and detector are fixed, during operation thereof, in position relative to each other and in at least one dimension relative to the sample according to a-priori knowledge about the known characteristic of the sample. A second x-ray detector may be fixed relative to the first x-ray detector according to the a-priori knowledge about the known characteristic of the sample, especially in a phase monitoring embodiment of the present invention.

Quantum Dots Microstructured Optical Fiber for X-Ray Detection

NASA Technical Reports Server (NTRS)

DeHaven, S. L.; Williams, P. A.; Burke, E. R.

2015-01-01

A novel concept for the detection of x-rays with microstructured optical fibers containing quantum dots scintillation material comprised of zinc sulfide nanocrystals doped with magnesium sulfide is presented. These quantum dots are applied inside the microstructured optical fibers using capillary action. The x-ray photon counts of these fibers are compared to the output of a collimated CdTe solid state detector over an energy range from 10 to 40 keV. The results of the fiber light output and associated effects of an acrylate coating and the quantum dots application technique are discussed.

The effect of exit beam phase aberrations on parallel beam coherent x-ray reconstructions

NASA Astrophysics Data System (ADS)

Hruszkewycz, S. O.; Harder, R.; Xiao, X.; Fuoss, P. H.

2010-12-01

Diffraction artifacts from imperfect x-ray windows near the sample are an important consideration in the design of coherent x-ray diffraction measurements. In this study, we used simulated and experimental diffraction patterns in two and three dimensions to explore the effect of phase imperfections in a beryllium window (such as a void or inclusion) on the convergence behavior of phasing algorithms and on the ultimate reconstruction. A predictive relationship between beam wavelength, sample size, and window position was derived to explain the dependence of reconstruction quality on beryllium defect size. Defects corresponding to this prediction cause the most damage to the sample exit wave and induce signature error oscillations during phasing that can be used as a fingerprint of experimental x-ray window artifacts. The relationship between x-ray window imperfection size and coherent x-ray diffractive imaging reconstruction quality explored in this work can play an important role in designing high-resolution in situ coherent imaging instrumentation and will help interpret the phasing behavior of coherent diffraction measured in these in situ environments.

The effect of exit beam phase aberrations on parallel beam coherent x-ray reconstructions.

PubMed

Hruszkewycz, S O; Harder, R; Xiao, X; Fuoss, P H

2010-12-01

Diffraction artifacts from imperfect x-ray windows near the sample are an important consideration in the design of coherent x-ray diffraction measurements. In this study, we used simulated and experimental diffraction patterns in two and three dimensions to explore the effect of phase imperfections in a beryllium window (such as a void or inclusion) on the convergence behavior of phasing algorithms and on the ultimate reconstruction. A predictive relationship between beam wavelength, sample size, and window position was derived to explain the dependence of reconstruction quality on beryllium defect size. Defects corresponding to this prediction cause the most damage to the sample exit wave and induce signature error oscillations during phasing that can be used as a fingerprint of experimental x-ray window artifacts. The relationship between x-ray window imperfection size and coherent x-ray diffractive imaging reconstruction quality explored in this work can play an important role in designing high-resolution in situ coherent imaging instrumentation and will help interpret the phasing behavior of coherent diffraction measured in these in situ environments.

Radiation-induced changes in electrical conductivity and structure of BaPbO3 after γ-irradiation

NASA Astrophysics Data System (ADS)

Shan, Qing; Cai, Pingkun; Zhang, Xinlei; Li, Jiatong; Chu, Shengnan; Jia, Wenbao

2015-11-01

Several barium plumbate (BaPbO3) solid samples, made from PbO and BaCO3 powder by chemistry liquid-phase coprecipitation, were investigated before and after γ-irradiation. The solid samples were irradiated by a 60Co γ-irradiation source whose dose rate is about 0.7 kGy per hour. The irradiation times were 0, 72, 144, 216, 288 and 360 h. Then, the four-probe method, X-ray diffraction (XRD), scanning electron microscope (SEM) and X-ray photoelectron spectroscopy (XPS) were used to indicate the changes in electrical conductivity and microstructure of BaPbO3 after γ-irradiation. The XRD results indicated that the content of PbO was reduced as the irradiation dose was increased and eventually vanished from the surface of samples. However, there was no new obvious substance phase found from the XRD atlas. It seems that the PbO transformed into nearly amorphous Pb5O8. The conjecture could be proved by the results of annealing experiment and SEM. The XPS results seem to show that the microstructure of BaPbO3 was slightly changed.

In-situ characterization of highly reversible phase transformation by synchrotron X-ray Laue microdiffraction

DOE PAGES

Chen, Xian; Tamura, Nobumichi; MacDowell, Alastair; ...

2016-05-23

The alloy Cu 25 Au 30 Zn 45 undergoes a huge first-order phase transformation (6% strain) and shows a high reversibility under thermal cycling and an unusual martensitc microstructure in sharp contrast to its nearby compositions. We discovered this alloy by systematically tuning the composition so that its lattice parameters satisfy the cofactor conditions (i.e., the kinematic conditions of compatibility between phases). It was conjectured that satisfaction of these conditions is responsible for the enhanced reversibility as well as the observed unusual fluid-like microstructure during transformation, but so far, there has been no direct evidence confirming that these observed microstructuresmore » are those predicted by the cofactor conditions. In order to verify this hypothesis, we use synchrotron X-ray Laue microdiffraction to measure the orientations and structural parameters of variants and phases near the austenite/martensite interface. The areas consisting of both austenite and multi-variants of martensite are scanned by microLaue diffraction. The cofactor conditions have been examined from the kinematic relation of lattice vectors across the interface. The continuity condition of the interface is precisely verified from the correspondent lattice vectors between two phases.« less

Synthesis of Carbon-Coated ZnO Composite and Varistor Properties Study

NASA Astrophysics Data System (ADS)

Sun, Wei-Jie; Liu, Jin-Ran; Yao, Da-Chuan; Chen, Yong; Wang, Mao-Hua

2017-03-01

In this article, monodisperse ZnO composite nanoparticles were successfully prepared by sol-gel mixed precursor method. Subsequently, carbon as the shell was homogeneously coated on the surface of the ZnO composite nanoparticles via a simple adsorption and calcination process. Microstructural studies of the as-obtained powders were carried out using the techniques of the x-ray powder diffraction, scanning electron microscopy, field emission scanning electron microscopy, transmission electron microscopy with energy dispersive x-ray spectroscopy, and Fourier transform infrared spectroscopy. The results show that the pink ZnO composite powders were fully coated by carbon. Based on the results, the effect of glucose content on the microstructure of the synthesized composites and the electrical properties of the ZnO varistors sintered in air at 1150°C for 2 h were also fully studied. As the amount of glucose increased, the thickness of carbon can be increased from 2.5 nm to 5 nm. In particular, the ZnO varistor fabricated with the appropriate thickness of the carbon coating (5 nm) leads to the superior electrical performance, with present high breakdown voltage ( V b = 420 V/mm) and excellent nonlinear coefficient ( α = 61.7), compared with the varistors obtained without carbon coating.

High-efficiency and conveniently recyclable photo-catalysts for dye degradation based on urchin-like CuO microparticle/polymer hybrid composites

NASA Astrophysics Data System (ADS)

Liu, Xiong; Cheng, Yuming; Li, Xuefeng; Dong, Jinfeng

2018-05-01

In this work, we developed a new type of photo-catalysts composed of the urchin-like cupric oxide (CuO) microparticle and polyvinylidene fluoride (PVDF) hybrid composites by the convenient organic-inorganic hybrid strategy, which show high-efficiency and conveniently recyclable for dye degradation including methylene blue (MB), Congo red (CR), and malachite green (MG) by visible light irradiation. The micro-structural characteristics of urchin-like CuO microparticles are crucial and dominant over the photo-degrading efficiency of hybrid catalyst because of their highly exposed {0 0 2} facet and larger specific surface area. Simultaneously, the intrinsic porous framework of PVDF membrane not only remains the excellent photo-catalytic activity of urchin-like CuO microparticles but also facilitates the enrichment of dyes on the membrane, and thereby synergistically contributing to the photo-catalytic efficiency. The microstructures of both urchin-like CuO microparticles and hybrid catalysts are systematically characterized by various techniques including scanning electron microscopy (SEM), transmission electron microscope (TEM), high-resolution transmission electron microscope (HRTEM), powder X-ray diffraction (XRD), X-ray photoelectron spectroscopy (XPS), Fourier transform infrared spectroscopy (FTIR), and nitrogen adsorption/desorption isotherms, which evidently support the mentioned mechanism.

Fabrication of nano-structured super-hydrophobic film on aluminum by controllable immersing method

NASA Astrophysics Data System (ADS)

Wu, Ruomei; Liang, Shuquan; Pan, Anqiang; Yuan, Zhiqing; Tang, Yan; Tan, Xiaoping; Guan, Dikai; Yu, Ya

2012-06-01

Aluminum alloy surface can be etched easily in acid environment, but the microstructure of alloy surface hardly meets the customers' demand. In this work, a facile acidic-assistant surface oxidation technique has been employed to form reproducible super-hydrophobic surfaces on aluminum alloy plates. The samples immersed in three different acid solutions at ambient temperatures are studied and the results demonstrated that the aqueous mixture solution of oxalic acid and hydrochloric is easier to produce better faces and better stability. Scanning electron microscopy (SEM), X-ray diffraction (XRD), Raman spectrometer, X-ray photoelectron spectroscopy (XPS) and water contact angle measurement are used to investigate the morphologies, microstructures, chemical compositions and hydrophobicity of the produced films on aluminum substrates. The surfaces, configured of a labyrinth structure with convexity and concavity, are in different roughness and gloss because of the different recipe acid solutions used. Better roughness of the surface can be obtained by adjusting the concentration of Clˉ and oxalate ions in acid solutions. The present research work provides a new strategy for the controllable preparation super-hydrophobic films of general materials on aluminum alloy for practical industrial applications.

An Investigation of Fiber Reinforced Chemically Bonded Phosphate Ceramic Composites at Room Temperature.

PubMed

Ding, Zhu; Li, Yu-Yu; Lu, Can; Liu, Jian

2018-05-21

In this study, chemically bonded phosphate ceramic (CBPC) fiber reinforced composites were made at indoor temperatures. The mechanical properties and microstructure of the CBPC composites were studied. The CBPC matrix of aluminum phosphate binder, metakaolin, and magnesia with different Si/P ratios was prepared. The results show that when the Si/P ratio was 1.2, and magnesia content in the CBPC was 15%, CBPC reached its maximum flexural strength. The fiber reinforced CBPC composites were prepared by mixing short polyvinyl alcohol (PVA) fibers or unidirectional continuous carbon fiber sheets. Flexural strength and dynamic mechanical properties of the composites were determined, and the microstructures of specimens were analyzed by scanning electron micrography, X-ray diffraction, and micro X-ray computed tomography. The flexural performance of continuous carbon fiber reinforced CBPC composites was better than that of PVA fiber composites. The elastic modulus, loss modulus, and loss factor of the fiber composites were measured through dynamic mechanical analysis. The results showed that fiber reinforced CBPC composites are an inorganic polymer viscoelastic material with excellent damping properties. The reaction of magnesia and phosphate in the matrix of CBPC formed a different mineral, newberyite, which was beneficial to the development of the CBPC.

Monotropic polymorphism in a glass-forming metallic alloy

NASA Astrophysics Data System (ADS)

Pogatscher, S.; Leutenegger, D.; Schawe, J. E. K.; Maris, P.; Schäublin, R.; Uggowitzer, P. J.; Löffler, J. F.

2018-06-01

This study investigates the crystallization and phase transition behavior of the amorphous metallic alloy Au70Cu5.5Ag7.5Si17. This alloy has been recently shown to exhibit a transition of a metastable to a more stable crystalline state, occurring via metastable melting under strong non-equilibrium conditions. Such behavior had so far not been observed in other metallic alloys. In this investigation fast differential scanning calorimetry (FDSC) is used to explore crystallization and the solid–liquid–solid transition upon linear heating and during isothermal annealing, as a function of the conditions under which the metastable phase is formed. It is shown that the occurrence of the solid–liquid–solid transformation in FDSC depends on the initial conditions; this is explained by a history-dependent nucleation of the stable crystalline phase. The microstructure was investigated by scanning and transmission electron microscopy and x-ray diffraction. Chemical mapping was performed by energy dispersive x-ray spectrometry. The relationship between the microstructure and the phase transitions observed in FSDC is discussed with respect to the possible kinetic paths of the solid–liquid–solid transition, which is a typical phenomenon in monotropic polymorphism.

Influence of ageing time on hardness, microstructure and wear behaviour of AISI2507 super duplex stainless steel

NASA Astrophysics Data System (ADS)

Davanageri, Mahesh; Narendranath, S.; Kadoli, Ravikiran

2017-08-01

The effect of ageing time on hardness, microstructure and wear behaviour of super duplex stainless AISI 2507 is examined. The material was solution treated at 1050 °C and water quenched, further the ageing has been carried out at 850 °C for 30 min, 60 min and 90 min. The chromium (Cr) and molybdenum (Mo) enriched intermetallic sigma phase (σ) were found to precipitate at the ferrite/austenite interface and within the ferrite region. The concentration of intermetallic sigma phase (σ), which was quantified by a combination of scanning electron microscopy and image analysis, increases with increasing ageing time, leading to significant increase in the hardness. The x-ray diffraction (XRD) and energy dispersive x-ray (EDX) was employed to investigate the element distribution and phase identification. Wear characterstics of the aged super duplex stainless steel were measured by varying normal loads, sliding speeds, sliding distance and compared with solution treated (as-cast) specimens. Scanning electron microscopy was used to assist in analysis of worn out surfaces. The outcomes suggested that the increase in percentage of sigma phase increases hardness and wear resistance in heat-treated specimens compared to solution treated specimens (as-cast).

Femtosecond X-ray Diffraction From Two-Dimensional Protein Crystals

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

Frank, Matthias; Carlson, David B.; Hunter, Mark

2014-02-28

Here we present femtosecond x-ray diffraction patterns from two-dimensional (2-D) protein crystals using an x-ray free electron laser (XFEL). To date it has not been possible to acquire x-ray diffraction from individual 2-D protein crystals due to radiation damage. However, the intense and ultrafast pulses generated by an XFEL permits a new method of collecting diffraction data before the sample is destroyed. Utilizing a diffract-before-destroy methodology at the Linac Coherent Light Source, we observed Bragg diffraction to better than 8.5 Å resolution for two different 2-D protein crystal samples that were maintained at room temperature. These proof-of-principle results show promisemore » for structural analysis of both soluble and membrane proteins arranged as 2-D crystals without requiring cryogenic conditions or the formation of three-dimensional crystals.« less

Influence of gamma ray irradiation on stoichiometry of hydrothermally synthesized bismuth telluride nanoparticles

NASA Astrophysics Data System (ADS)

Abishek, N. S.; Naik, K. Gopalakrishna

2018-05-01

Bismuth telluride (Bi2Te3) nanoparticles were synthesized by the hydrothermal method at 200 °C for 24 h. The synthesized Bi2Te3 nanoparticles were irradiated with gamma rays at doses of 50 kGy and 100 kGy. The structural characterization of the pre-irradiated and post-irradiated samples was carried out by X-ray diffraction technique and was found to have rhombohedral phase having R3 ¯m (166) space group. The X-ray diffraction peaks were found to shift towards lower diffraction angle with gamma ray irradiation. The morphologies and compositions of the grown Bi2Te3 nanoparticles were studied using Field Emission Scanning Electron Microscope and X-ray energy dispersive analysis, respectively. The possible cause for the shift in the X-ray diffraction peaks with gamma ray irradiation has been discussed in the present work.

High Power Optical Coatings by Atomic Layer Deposition and Signatures of Laser-Induced Damage

DTIC Science & Technology

2012-08-28

diffraction angle 0 into crystal lattice spacing d by the Bragg condition, mX = 2d sin 0. Here X is the x - ray wavelength... angle x - ray diffraction (GAXRD) measurements, which were made at a fixed shallow incidence angle of 0.5°. Detector scans were done to measure the...was finished with 200 hafnia cycles m the fmal half period rather than 400. Crystallinity was measured by x - ray diffraction (XRD) with

Materials identification using a small-scale pixellated x-ray diffraction system

NASA Astrophysics Data System (ADS)

O'Flynn, D.; Crews, C.; Drakos, I.; Christodoulou, C.; Wilson, M. D.; Veale, M. C.; Seller, P.; Speller, R. D.

2016-05-01

A transmission x-ray diffraction system has been developed using a pixellated, energy-resolving detector (HEXITEC) and a small-scale, mains operated x-ray source (Amptek Mini-X). HEXITEC enables diffraction to be measured without the requirement of incident spectrum filtration, or collimation of the scatter from the sample, preserving a large proportion of the useful signal compared with other diffraction techniques. Due to this efficiency, sufficient molecular information for material identification can be obtained within 5 s despite the relatively low x-ray source power. Diffraction data are presented from caffeine, hexamine, paracetamol, plastic explosives and narcotics. The capability to determine molecular information from aspirin tablets inside their packaging is demonstrated. Material selectivity and the potential for a sample classification model is shown with principal component analysis, through which each different material can be clearly resolved.

Dynamic X-ray diffraction sampling for protein crystal positioning

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

Scarborough, Nicole M.; Godaliyadda, G. M. Dilshan P.; Ye, Dong Hye

A sparse supervised learning approach for dynamic sampling (SLADS) is described for dose reduction in diffraction-based protein crystal positioning. Crystal centering is typically a prerequisite for macromolecular diffraction at synchrotron facilities, with X-ray diffraction mapping growing in popularity as a mechanism for localization. In X-ray raster scanning, diffraction is used to identify the crystal positions based on the detection of Bragg-like peaks in the scattering patterns; however, this additional X-ray exposure may result in detectable damage to the crystal prior to data collection. Dynamic sampling, in which preceding measurements inform the next most information-rich location to probe for image reconstruction,more » significantly reduced the X-ray dose experienced by protein crystals during positioning by diffraction raster scanning. The SLADS algorithm implemented herein is designed for single-pixel measurements and can select a new location to measure. In each step of SLADS, the algorithm selects the pixel, which, when measured, maximizes the expected reduction in distortion given previous measurements. Ground-truth diffraction data were obtained for a 5 µm-diameter beam and SLADS reconstructed the image sampling 31% of the total volume and only 9% of the interior of the crystal greatly reducing the X-ray dosage on the crystal. Furthermore, by usingin situtwo-photon-excited fluorescence microscopy measurements as a surrogate for diffraction imaging with a 1 µm-diameter beam, the SLADS algorithm enabled image reconstruction from a 7% sampling of the total volume and 12% sampling of the interior of the crystal. When implemented into the beamline at Argonne National Laboratory, without ground-truth images, an acceptable reconstruction was obtained with 3% of the image sampled and approximately 5% of the crystal. The incorporation of SLADS into X-ray diffraction acquisitions has the potential to significantly minimize the impact of X-ray exposure on the crystal by limiting the dose and area exposed for image reconstruction and crystal positioning using data collection hardware present in most macromolecular crystallography end-stations.« less

Dynamic X-ray diffraction sampling for protein crystal positioning

DOE PAGES

Scarborough, Nicole M.; Godaliyadda, G. M. Dilshan P.; Ye, Dong Hye; ...

2017-01-01

A sparse supervised learning approach for dynamic sampling (SLADS) is described for dose reduction in diffraction-based protein crystal positioning. Crystal centering is typically a prerequisite for macromolecular diffraction at synchrotron facilities, with X-ray diffraction mapping growing in popularity as a mechanism for localization. In X-ray raster scanning, diffraction is used to identify the crystal positions based on the detection of Bragg-like peaks in the scattering patterns; however, this additional X-ray exposure may result in detectable damage to the crystal prior to data collection. Dynamic sampling, in which preceding measurements inform the next most information-rich location to probe for image reconstruction,more » significantly reduced the X-ray dose experienced by protein crystals during positioning by diffraction raster scanning. The SLADS algorithm implemented herein is designed for single-pixel measurements and can select a new location to measure. In each step of SLADS, the algorithm selects the pixel, which, when measured, maximizes the expected reduction in distortion given previous measurements. Ground-truth diffraction data were obtained for a 5 µm-diameter beam and SLADS reconstructed the image sampling 31% of the total volume and only 9% of the interior of the crystal greatly reducing the X-ray dosage on the crystal. Furthermore, by usingin situtwo-photon-excited fluorescence microscopy measurements as a surrogate for diffraction imaging with a 1 µm-diameter beam, the SLADS algorithm enabled image reconstruction from a 7% sampling of the total volume and 12% sampling of the interior of the crystal. When implemented into the beamline at Argonne National Laboratory, without ground-truth images, an acceptable reconstruction was obtained with 3% of the image sampled and approximately 5% of the crystal. The incorporation of SLADS into X-ray diffraction acquisitions has the potential to significantly minimize the impact of X-ray exposure on the crystal by limiting the dose and area exposed for image reconstruction and crystal positioning using data collection hardware present in most macromolecular crystallography end-stations.« less

Dynamic X-ray diffraction sampling for protein crystal positioning

PubMed Central

Scarborough, Nicole M.; Godaliyadda, G. M. Dilshan P.; Ye, Dong Hye; Kissick, David J.; Zhang, Shijie; Newman, Justin A.; Sheedlo, Michael J.; Chowdhury, Azhad U.; Fischetti, Robert F.; Das, Chittaranjan; Buzzard, Gregery T.; Bouman, Charles A.; Simpson, Garth J.

2017-01-01

A sparse supervised learning approach for dynamic sampling (SLADS) is described for dose reduction in diffraction-based protein crystal positioning. Crystal centering is typically a prerequisite for macromolecular diffraction at synchrotron facilities, with X-ray diffraction mapping growing in popularity as a mechanism for localization. In X-ray raster scanning, diffraction is used to identify the crystal positions based on the detection of Bragg-like peaks in the scattering patterns; however, this additional X-ray exposure may result in detectable damage to the crystal prior to data collection. Dynamic sampling, in which preceding measurements inform the next most information-rich location to probe for image reconstruction, significantly reduced the X-ray dose experienced by protein crystals during positioning by diffraction raster scanning. The SLADS algorithm implemented herein is designed for single-pixel measurements and can select a new location to measure. In each step of SLADS, the algorithm selects the pixel, which, when measured, maximizes the expected reduction in distortion given previous measurements. Ground-truth diffraction data were obtained for a 5 µm-diameter beam and SLADS reconstructed the image sampling 31% of the total volume and only 9% of the interior of the crystal greatly reducing the X-ray dosage on the crystal. Using in situ two-photon-excited fluorescence microscopy measurements as a surrogate for diffraction imaging with a 1 µm-diameter beam, the SLADS algorithm enabled image reconstruction from a 7% sampling of the total volume and 12% sampling of the interior of the crystal. When implemented into the beamline at Argonne National Laboratory, without ground-truth images, an acceptable reconstruction was obtained with 3% of the image sampled and approximately 5% of the crystal. The incorporation of SLADS into X-ray diffraction acquisitions has the potential to significantly minimize the impact of X-ray exposure on the crystal by limiting the dose and area exposed for image reconstruction and crystal positioning using data collection hardware present in most macromolecular crystallography end-stations. PMID:28009558

Dynamic X-ray diffraction sampling for protein crystal positioning.

PubMed

Scarborough, Nicole M; Godaliyadda, G M Dilshan P; Ye, Dong Hye; Kissick, David J; Zhang, Shijie; Newman, Justin A; Sheedlo, Michael J; Chowdhury, Azhad U; Fischetti, Robert F; Das, Chittaranjan; Buzzard, Gregery T; Bouman, Charles A; Simpson, Garth J

2017-01-01

A sparse supervised learning approach for dynamic sampling (SLADS) is described for dose reduction in diffraction-based protein crystal positioning. Crystal centering is typically a prerequisite for macromolecular diffraction at synchrotron facilities, with X-ray diffraction mapping growing in popularity as a mechanism for localization. In X-ray raster scanning, diffraction is used to identify the crystal positions based on the detection of Bragg-like peaks in the scattering patterns; however, this additional X-ray exposure may result in detectable damage to the crystal prior to data collection. Dynamic sampling, in which preceding measurements inform the next most information-rich location to probe for image reconstruction, significantly reduced the X-ray dose experienced by protein crystals during positioning by diffraction raster scanning. The SLADS algorithm implemented herein is designed for single-pixel measurements and can select a new location to measure. In each step of SLADS, the algorithm selects the pixel, which, when measured, maximizes the expected reduction in distortion given previous measurements. Ground-truth diffraction data were obtained for a 5 µm-diameter beam and SLADS reconstructed the image sampling 31% of the total volume and only 9% of the interior of the crystal greatly reducing the X-ray dosage on the crystal. Using in situ two-photon-excited fluorescence microscopy measurements as a surrogate for diffraction imaging with a 1 µm-diameter beam, the SLADS algorithm enabled image reconstruction from a 7% sampling of the total volume and 12% sampling of the interior of the crystal. When implemented into the beamline at Argonne National Laboratory, without ground-truth images, an acceptable reconstruction was obtained with 3% of the image sampled and approximately 5% of the crystal. The incorporation of SLADS into X-ray diffraction acquisitions has the potential to significantly minimize the impact of X-ray exposure on the crystal by limiting the dose and area exposed for image reconstruction and crystal positioning using data collection hardware present in most macromolecular crystallography end-stations.

Fixture for supporting and aligning a sample to be analyzed in an x-ray diffraction apparatus

DOEpatents

Green, L.A.; Heck, J.L. Jr.

1985-04-23

A fixture is provided for supporting and aligning small samples of material on a goniometer for x-ray diffraction analysis. A sample-containing capillary is accurately positioned for rotation in the x-ray beam by selectively adjusting the fixture to position the capillary relative to the x and y axes thereof to prevent wobble and position the sample along the z axis or the axis of rotation. By employing the subject fixture relatively small samples of materials can be analyzed in an x-ray diffraction apparatus previously limited to the analysis of much larger samples.

Fixture for supporting and aligning a sample to be analyzed in an X-ray diffraction apparatus

DOEpatents

Green, Lanny A.; Heck, Jr., Joaquim L.

1987-01-01

A fixture is provided for supporting and aligning small samples of material on a goniometer for X-ray diffraction analysis. A sample-containing capillary is accurately positioned for rotation in the X-ray beam by selectively adjusting the fixture to position the capillary relative to the x and y axes thereof to prevent wobble and position the sample along the z axis or the axis of rotation. By employing the subject fixture relatively small samples of materials can be analyzed in an X-ray diffraction apparatus previously limited to the analysis of much larger samples.

Ceramics

NASA Astrophysics Data System (ADS)

Zhang, Bo; Chang, Aimin; Zhao, Qing; Ye, Haitao; Wu, Yiquan

2014-11-01

The microstructure and thermoelectric properties of Yb-doped Ca0.9- x Yb x La0.1 MnO3 (0 ≤ x ≤ 0.05) ceramics prepared by using the Pechini method derived powders have been investigated. X-ray diffraction analysis has shown that all samples exhibit single phase with orthorhombic perovskite structure. All ceramic samples possess high relative densities, ranging from 97.04% to 98.65%. The Seebeck coefficient is negative, indicating n-type conduction in all samples. The substitution of Yb for Ca leads to a marked decrease in the electrical resistivity, along with a moderate decrease in the absolute value of the Seebeck coefficient. The highest power factor is obtained for the sample with x = 0.05. The electrical conduction in these compounds is due to electrons hopping between Mn3+ and Mn4+, which is enhanced by increasing Yb content.

X-ray and optical crystallographic parameters investigations of high frequency induction melted Al-(alpha-Al(2)O(3)) alloys.

PubMed

Bourbia, A; Draissia, M; Bedboudi, H; Boulkhessaim, S; Debili, M Y

2010-01-01

This article deals with the microstructural strengthening mechanisms of aluminium by means of hard alpha-Al(2)O(3) alumina fine particles. A broad of understanding views covering materials preparations, elaboration process, characterization techniques and associated microstructural characteristic parameters measurements is given. In order to investigate the microstructural characteristic parameters and the mechanical strengthening mechanisms of pure aluminium by hard fine particles, a set of Al-(alpha-Al(2)O(3)) alloys samples were made under vacuum by high fusion temperature melting, the high frequency (HF) process, and rapidly solidified under ambient temperature from a mixture of cold-compacted high-pure fine Al and alpha-Al(2)O(3) powders. The as-solidified Al-(alpha-Al(2)O(3)) alloys were characterized by means of X-ray diffraction (XRD) analyses, optical microscopy observations and Vickers microhardness tests in both brut and heat-treated states. It was found that the as-solidified HF Al-(alpha-Al(2)O(3)) alloys with compositions below 4 wt.% (alpha-Al(2)O(3)) are single-phase microstructures of the solid solution FCC Al phase and over two-phase microstructures of the solid solution FCC Al and the Rhombohedral alpha-Al(2)O(3) phases. The optical micrographs reveal the presence of a grain size refinement in these alloys. Vickers microhardness of the as-solidified Al-(alpha-Al(2)O(3)) is increased by means of pure fine alpha-Al(2)O(3) alumina particles. These combined effects of strengthening and grain size refinement observed in the as-solidified Al-(alpha-Al(2)O(3)) alloys are essentially due to a strengthening of Al by the alpha-Al(2)O(3) alumina particles insertion in the (HF) melted and rapidly solidified alloys.

JMFA2—a graphically interactive Java program that fits microfibril angle X-ray diffraction data

Treesearch

Steve P. Verrill; David E. Kretschmann; Victoria L. Herian

2006-01-01

X-ray diffraction techniques have the potential to decrease the time required to determine microfibril angles dramatically. In this paper, we discuss the latest version of a curve-fitting toll that permits us to reduce the time required to evaluate MFA X-ray diffraction patterns. Further, because this tool reflects the underlying physics more accurately than existing...

Synthesis, Characterization, and Gas-Sensing Properties of Mesoporous Nanocrystalline Sn(x)Ti(1-x)O2.

PubMed

Zhong, Cheng; Lin, Zhidong; Guo, Fei; Wang, Xuehua

2015-06-01

A nanocomposite mesoporous material composed by SnO2 and TiO2 with the size of -5-9 nm were prepared via a facile wet-chemical approach combining with an annealing process. The microstructure of obtained Sn(x)Ti(1-x)O2 powders were characterized by X-ray diffraction, X-ray Photo-electronic Spectroscopy, scanning electron microscope, transmission electron microscope and nitrogen adsorption-desorption experiment. The gas sensing performances to several gases of the mesoporous material were studied. The sensors of Sn(x)Ti(1-x)O2 (ST10, with 9.1% Ti) exhibited very high responses to volatile organic compounds at 160 degrees C. The order of the responses to volatile gases based on ST10 was ethanol > formaldehyde > acetone > toluene > benzene > methane. Sensor based on ST10 displays a highest sensitivity to hydrogen at 200 degrees C. Sensor responses to H2 at 200 degrees C have been measured and analyzed in a wide concentration range from 5 to 2000 ppm. The solid solution Sn(x)Ti(1-x)O2 can be served as a potential gas-sensing material for a broad range of future sensor applications.

A novel ion-exchange strategy for the fabrication of high strong BiOI/BiOBr heterostructure film coated metal wire mesh with tunable visible-light-driven photocatalytic reactivity.

PubMed

Wang, Yi; Long, Yang; Yang, Zhiqing; Zhang, Dun

2018-06-05

Visible-light-driven (VLD) BiOI/BiOBr heterostructure films with hierarchical microstructure have been firstly fabricated on 304 stainless steel wire mesh (304SSWM) substrates through a novel ion-exchange method using the BiOI film as precursor. The concentration of tetrabutylammonium bromide (TBAB) is the key factor to control the composition and microstructure of BiOI/BiOBr films. Physical, chemical, and optical properties of BiOI/BiOBr heterostructure films were characterized by X-ray diffraction, scanning electron microscope, energy-dispersive X-ray spectroscopy, high resolution transmittance electron microscopy, X-ray photoelectron spectroscopy, UV-vis diffuse reflectance absorption, and fluorescence spectrophotometer, respectively. The VLD photocatalytic ability of the BiOI/BiOBr heterostructure film coated 304SSWM was studied by degrading rhodamine B and pIRES2-EGFP plasmid as target water organic pollutants and pathogenic bacteria genetic materials. The BiOI/BiOBr heterostructure film coated 304SSWM fabricated with 50 mM TBAB has excellent photocatalytic activity, stability, and reusability in the cycled experiments. The reasons for these unique features can be ascribed to the formation of heterojuction structure and the open framework structure of the 304SSWM. The current work can provide new strategies to construct novel VLD photoactive functional films for water purification and disinfection. Copyright © 2018 Elsevier B.V. All rights reserved.

A high-transparency, micro-patternable chip for X-ray diffraction analysis of microcrystals under native growth conditions

DOE PAGES

Murray, Thomas D.; Lyubimov, Artem Y.; Ogata, Craig M.; ...

2015-08-11

Microcrystals present a significant impediment to the determination of macromolecular structures by X-ray diffraction methods. Although microfocus synchrotron beamlines and X-ray free-electron lasers (XFELs) can enable the collection of interpretable diffraction data from microcrystals, there is a need for efficient methods of harvesting small volumes (<2 µl) of microcrystals grown under common laboratory formats and delivering them to an X-ray beam source under native growth conditions. One approach that shows promise in overcoming the challenges intrinsic to microcrystal analysis is to pair so-called `fixed-target' sample-delivery devices with microbeam-based X-ray diffraction methods. However, to record weak diffraction patterns it is necessarymore » to fabricate devices from X-ray-transparent materials that minimize background scattering. Presented here is the design of a new micro-diffraction device consisting of three layers fabricated from silicon nitride, photoresist and polyimide film. The chip features low X-ray scattering and X-ray absorption properties, and uses a customizable blend of hydrophobic and hydrophilic surface patterns to help localize microcrystals to defined regions. Microcrystals in their native growth conditions can be loaded into the chips with a standard pipette, allowing data collection at room temperature. Diffraction data collected from hen egg-white lysozyme microcrystals (10–15 µm) loaded into the chips yielded a complete, high-resolution (<1.6 Å) data set sufficient to determine a high-quality structure by molecular replacement. In addition, the features of the chip allow the rapid and user-friendly analysis of microcrystals grown under virtually any laboratory format at microfocus synchrotron beamlines and XFELs.« less

A high-transparency, micro-patternable chip for X-ray diffraction analysis of microcrystals under native growth conditions

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

Murray, Thomas D.; Lyubimov, Artem Y.; Ogata, Craig M.

Microcrystals present a significant impediment to the determination of macromolecular structures by X-ray diffraction methods. Although microfocus synchrotron beamlines and X-ray free-electron lasers (XFELs) can enable the collection of interpretable diffraction data from microcrystals, there is a need for efficient methods of harvesting small volumes (<2 µl) of microcrystals grown under common laboratory formats and delivering them to an X-ray beam source under native growth conditions. One approach that shows promise in overcoming the challenges intrinsic to microcrystal analysis is to pair so-called `fixed-target' sample-delivery devices with microbeam-based X-ray diffraction methods. However, to record weak diffraction patterns it is necessarymore » to fabricate devices from X-ray-transparent materials that minimize background scattering. Presented here is the design of a new micro-diffraction device consisting of three layers fabricated from silicon nitride, photoresist and polyimide film. The chip features low X-ray scattering and X-ray absorption properties, and uses a customizable blend of hydrophobic and hydrophilic surface patterns to help localize microcrystals to defined regions. Microcrystals in their native growth conditions can be loaded into the chips with a standard pipette, allowing data collection at room temperature. Diffraction data collected from hen egg-white lysozyme microcrystals (10–15 µm) loaded into the chips yielded a complete, high-resolution (<1.6 Å) data set sufficient to determine a high-quality structure by molecular replacement. In addition, the features of the chip allow the rapid and user-friendly analysis of microcrystals grown under virtually any laboratory format at microfocus synchrotron beamlines and XFELs.« less

A high-transparency, micro-patternable chip for X-ray diffraction analysis of microcrystals under native growth conditions

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

Murray, Thomas D.; Lyubimov, Artem Y.; Ogata, Craig M.

Microcrystals present a significant impediment to the determination of macromolecular structures by X-ray diffraction methods. Although microfocus synchrotron beamlines and X-ray free-electron lasers (XFELs) can enable the collection of interpretable diffraction data from microcrystals, there is a need for efficient methods of harvesting small volumes (<2µl) of microcrystals grown under common laboratory formats and delivering them to an X-ray beam source under native growth conditions. One approach that shows promise in overcoming the challenges intrinsic to microcrystal analysis is to pair so-called `fixed-target' sample-delivery devices with microbeam-based X-ray diffraction methods. However, to record weak diffraction patterns it is necessary tomore » fabricate devices from X-ray-transparent materials that minimize background scattering. Presented here is the design of a new micro-diffraction device consisting of three layers fabricated from silicon nitride, photoresist and polyimide film. The chip features low X-ray scattering and X-ray absorption properties, and uses a customizable blend of hydrophobic and hydrophilic surface patterns to help localize microcrystals to defined regions. Microcrystals in their native growth conditions can be loaded into the chips with a standard pipette, allowing data collection at room temperature. Diffraction data collected from hen egg-white lysozyme microcrystals (10–15µm) loaded into the chips yielded a complete, high-resolution (<1.6Å) data set sufficient to determine a high-quality structure by molecular replacement. The features of the chip allow the rapid and user-friendly analysis of microcrystals grown under virtually any laboratory format at microfocus synchrotron beamlines and XFELs.« less

A high-transparency, micro-patternable chip for X-ray diffraction analysis of microcrystals under native growth conditions

PubMed Central

Murray, Thomas D.; Lyubimov, Artem Y.; Ogata, Craig M.; Vo, Huy; Uervirojnangkoorn, Monarin; Brunger, Axel T.; Berger, James M.

2015-01-01

Microcrystals present a significant impediment to the determination of macromolecular structures by X-ray diffraction methods. Although microfocus synchrotron beamlines and X-ray free-electron lasers (XFELs) can enable the collection of interpretable diffraction data from microcrystals, there is a need for efficient methods of harvesting small volumes (<2 µl) of microcrystals grown under common laboratory formats and delivering them to an X-ray beam source under native growth conditions. One approach that shows promise in overcoming the challenges intrinsic to microcrystal analysis is to pair so-called ‘fixed-target’ sample-delivery devices with microbeam-based X-ray diffraction methods. However, to record weak diffraction patterns it is necessary to fabricate devices from X-ray-transparent materials that minimize background scattering. Presented here is the design of a new micro-diffraction device consisting of three layers fabricated from silicon nitride, photoresist and polyimide film. The chip features low X-ray scattering and X-ray absorption properties, and uses a customizable blend of hydrophobic and hydrophilic surface patterns to help localize microcrystals to defined regions. Microcrystals in their native growth conditions can be loaded into the chips with a standard pipette, allowing data collection at room temperature. Diffraction data collected from hen egg-white lysozyme microcrystals (10–15 µm) loaded into the chips yielded a complete, high-resolution (<1.6 Å) data set sufficient to determine a high-quality structure by molecular replacement. The features of the chip allow the rapid and user-friendly analysis of microcrystals grown under virtually any laboratory format at microfocus synchrotron beamlines and XFELs. PMID:26457423

High-resolution x-ray diffraction microscopy of specifically labeled yeast cells

PubMed Central

Nelson, Johanna; Huang, Xiaojing; Steinbrener, Jan; Shapiro, David; Kirz, Janos; Marchesini, Stefano; Neiman, Aaron M.; Turner, Joshua J.; Jacobsen, Chris

2010-01-01

X-ray diffraction microscopy complements other x-ray microscopy methods by being free of lens-imposed radiation dose and resolution limits, and it allows for high-resolution imaging of biological specimens too thick to be viewed by electron microscopy. We report here the highest resolution (11–13 nm) x-ray diffraction micrograph of biological specimens, and a demonstration of molecular-specific gold labeling at different depths within cells via through-focus propagation of the reconstructed wavefield. The lectin concanavalin A conjugated to colloidal gold particles was used to label the α-mannan sugar in the cell wall of the yeast Saccharomyces cerevisiae. Cells were plunge-frozen in liquid ethane and freeze-dried, after which they were imaged whole using x-ray diffraction microscopy at 750 eV photon energy. PMID:20368463

High-resolution x-ray diffraction microscopy of specifically labeled yeast cells

DOE PAGES

Nelson, Johanna; Huang, Xiaojing; Steinbrener, Jan; ...

2010-04-20

X-ray diffraction microscopy complements other x-ray microscopy methods by being free of lens-imposed radiation dose and resolution limits, and it allows for high-resolution imaging of biological specimens too thick to be viewed by electron microscopy. We report here the highest resolution (11-13 nm) x-ray diffraction micrograph of biological specimens, and a demonstration of molecular-specific gold labeling at different depths within cells via through-focus propagation of the reconstructed wavefield. The lectin concanavalin A conjugated to colloidal gold particles was used to label the α-mannan sugar in the cell wall of the yeast Saccharomyces cerevisiae. Cells were plunge-frozen in liquid ethane andmore » freeze-dried, after which they were imaged whole using x-ray diffraction microscopy at 750 eV photon energy.« less

Additive Manufacturing of AlSi10Mg Alloy Using Direct Energy Deposition: Microstructure and Hardness Characterization

NASA Astrophysics Data System (ADS)

Javidani, M.; Arreguin-Zavala, J.; Danovitch, J.; Tian, Y.; Brochu, M.

2017-04-01

This paper aims to study the manufacturing of the AlSi10Mg alloy with direct energy deposition (DED) process. Following fabrication, the macro- and microstructural evolution of the as-processed specimens was initially investigated using optical microscopy and scanning electron microscopy. Columnar dendritic structure was the dominant solidification feature of the deposit; nevertheless, detailed microstructural analysis revealed cellular morphology near the substrate and equiaxed dendrites at the top end of the deposit. Moreover, the microstructural morphology in the melt pool boundary of the deposit differed from the one in the core of the layers. The remaining porosity of the deposit was evaluated by Archimedes' principle and by image analysis of the polished surface. Crystallographic texture in the deposit was also assessed using electron backscatter diffraction and x-ray diffraction analysis. The dendrites were unidirectionally oriented at an angle of 80° to the substrate. EPMA line scans were performed to evaluate the compositional variation and elemental segregation in different locations. Eventually, microhardness (HV) tests were conducted in order to study the hardness gradient in the as-DED-processed specimen along the deposition direction. The presented results, which exhibited a deposit with an almost defect free structure, indicate that the DED process can suitable for the deposition of Al-Si-based alloys with a highly consolidated structure.

Phase stability, porosity distribution and microstructural evolution of amorphous Al{sub 50}Ti{sub 50} powders consolidated by electrical resistance sintering

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

Urban, P., E-mail: purban@us.es; Montes, J. M.; Cintas, J.

2015-03-30

The effect of intensity and duration of the electrical resistance sintering process on the phase stability, porosity distribution and microstructural evolution of Al{sub 50}Ti{sub 50} amorphous powders is studied. The phase transformations during the consolidation process were determined by X-ray diffraction. The porosity distribution was observed by optical and scanning electron microscopy. The amorphous phase is partially transformed to the crystalline phase during the sintering process, and formation of AlTi and AlTi{sub 3} intermetallic compounds occurs for temperatures higher than 300 °C. Finally, it is observed that the compacts core have lower porosity and a higher tendency to the amorphous-crystallinemore » phase transformation than the periphery.« less

Microstructure and Mechanical Properties of C/C Composite/TC17 Joints with Ag-Cu-Ti Brazing Alloy

NASA Astrophysics Data System (ADS)

Cao, Xiujie; Zhu, Ying; Guo, Wei; Peng, Peng; Ma, Kaituo

2017-12-01

Carbon/Carbon composite(C/C) was vacuum brazed to titanium alloy (TC17) using Ag-Cu-Ti brazing alloy. The effects of brazing temperature on the interfacial microstructure and joint properties were investigated by energy dispersive spectrometer (EDS), a scanning electron microscope (SEM), X-ray diffraction (XRD) and Gleeble1500D testing machine. Results show that C/C composite and TC17 were successfully brazed using AgCuTi brazing alloy. Various phases including TiC, Ag(s, s), Cu(s, s), Ti3Cu4, TiCu, and Ti2Cu were formed in the brazed joint. The maximum shear strength of the brazed joints with AgCuTi brazing alloy was 24±1 MPa when brazed at 860°C for 15 min.

The effect of reaction conditions on formation of wet precipitated calcium phosphates

NASA Astrophysics Data System (ADS)

Huang, Chen; Cao, Peng

2015-03-01

The precipitation process discussed in the present study involves the addition of alkaline solutions to an acidic calcium phosphate suspension. Several parameters (pH, pH buffer reagent, ageing and stirring) were investigated. The synthesized powders were calcined at 1000°C for 1 h in air, in order to study the thermal stability and crystalline phase compositions. X-ray diffraction (XRD) and ESEM analysis were used for sample characterization. It is found that all these processing parameters affect the crystalline phases evolved and resultant microstructures. Phase evolution occurred at an elevated pH level. The pH buffer reagent would affect both the phase composition and microstructure. Ageing was essential for the phase maturation. Stirring accelerated the reaction process by providing a homogeneous medium for precipitation.

Partial-Isothermally-Treated Low Alloy Ultrahigh Strength Steel with Martensitic/Bainitic Microstructure

NASA Astrophysics Data System (ADS)

Luo, Quanshun; Kitchen, Matthew; Patel, Vinay; Filleul, Martin; Owens, Dave

We introduce a new strengthening heat treatment of a Ni-Cr-Mo-V alloyed spring steel by partial isothermal salt-bath and subsequent air-cooling and tempering. Detailed isothermal treatments were made at temperatures below or above the Ms point (230°C). The salt bath time was controlled between 10 and 80 minutes. Through the new treatment, the candidate steel developed ultrahigh tensile strength 2,100 MPa, yield strength 1,800 MPa, elongation 8-10 %, hardness 580-710 HV, and V-notch Charpy toughness 10-12 J. Optical and electron microscopic observations and X-ray diffraction revealed multi-phase microstructures of bainitic/martensitic ferrites, fine carbide precipitates and retained austenite. Carbon partitioning during the bainitic/martensitic transformation was investigated for its remarkable influence on the strengthening mechanism.

Densification of LSGM electrolytes using activated microwave sintering

NASA Astrophysics Data System (ADS)

Kesapragada, S. V.; Bhaduri, S. B.; Bhaduri, S.; Singh, P.

Lanthanum gallate doped with alkaline rare earths (LSGM) powders were densified using an activated microwave sintering process for developing a dense stable electrolyte layer for applications in intermediate temperature-solid oxide fuel cells (IT-SOFCs). Due to heat generation in situ, the process of sintering gets activated with faster kinetics compared to a conventional sintering process. The effect of various microwave process parameters on the microstructure and phase formation was studied. The sintered pellets were characterized using scanning electron microscopy-energy dispersive analysis (SEM-EDAX), and X-ray diffraction (XRD). The density of LSGM pellets microwave sintered at 1350 °C for 20 min is greater than 95% theoretical density with a fine grained microstructure (˜2-3 μm) and without the presence of other phase(s).

The Influence of Duration of Mechanical Activation of Titanium Powder on its Morphology, Microstructure, and Microhardness

NASA Astrophysics Data System (ADS)

Ditenberg, I. A.; Korchagin, M. A.; Pinzhin, Yu. P.; Melnikov, V. V.; Tyumentsev, A. N.; Grinyaev, K. V.; Smirnov, I. V.; Radishevskii, V. L.; Tsverova, A. S.; Sukhanov, I. I.

2017-10-01

Using the methods of X-ray diffraction analysis and scanning and transmission electron microscopy, an investigation of the influence of duration of mechanical activation on morphology and structure of titanium powder is performed. In the course of processing the following stages of material transformation are revealed: fragmentation of the initial powder, conglomeration, and ovalization of the conglomerates. It is found that when the duration of mechanical activation increases, the characteristic size of coherent scattering regions is significantly decreased, which is accompanied by an increase in the value of microdistortions and intensive fragmentation of the crystal lattice inside powder particles followed by the formation of highly defective nanostructured states. The transformation of microstructure is accompanied by a considerable increase in microhardness.

Magnetic characteristics of ultrafine Fe particles reduced from uniform iron oxide particles

NASA Astrophysics Data System (ADS)

Bridger, K.; Watts, J.; Tadros, M.; Xiao, Gang; Liou, S. H.; Chien, C. L.

1987-04-01

Uniform, cubic 0.05-μm iron oxide particles were formed by forced hydrolysis of ferric perchlorate. These particles were reduced to α-Fe by heating in hydrogen at temperatures between 300 and 500 °C. The effect of reduction temperature and various prereduction treatments on the microstructure of the iron particles will be discussed. Complete reduction to α-Fe was established by 57Fe Mössbauer spectroscopy and x-ray diffraction. Magnetic measurements on epoxy and polyurethane films containing these particles with various mass fractions gave coercivities as high as 1000 Oe. The relationship between the magnetic measurements and the microstructure will be discussed. Na2SiO3 is found to be the best coating material for the process of reducing iron oxide particles to iron.

Grain refinement and Lattice Imperfections in Commercial Aluminum Alloy Processed by Severe Plastic Deformation

NASA Astrophysics Data System (ADS)

Charfeddine, Saifeddine; Zehani, Karim; Besais, Lotfi; Korchef, Atef

2014-08-01

In the present work, investigations on the microstructure of an aluminum alloy that had been subjected to severe plastic deformation (SPD) by equal channel angular pressing (ECAP), filing and ball milling, were carried out using X-ray diffraction and scanning electron microscopy. SPD leads to lattice distortions, increased dislocation density and an intensive refinement of the microstructure. The refinement and lattice imperfections of the material are greatly affected by the deformation modes and loading performance occurring during SPD. During the milling, the dislocation annihilation increases at higher strains thereby resulting in a smaller crystallite size. After ECAP, the material manifests a strong shear texture and anisotropy of the deformation behavior. Strain anisotropy is less pronounced in filed and ball milled powder particles.

The role of microstructure and phase distribution in the failure mechanisms and life prediction model for PSZ coatings

NASA Technical Reports Server (NTRS)

Sisson, R. D., Jr.; Sone, Ichiro; Biederman, R. R.

1985-01-01

Partially Stabilized Zirconia (PSZ) may become widely used for Thermal Barrier Coatings (TBC). Failure of these coatings can occur due to thermal fatigue in oxidizing atmospheres. The failure is due to the strains that develop due to thermal gradients, differences in thermal expansion coefficients, and oxidation of the bond coating. The role of microstructure and the cubic, tetragonal, and monoclinic phase distribution in the strain development and subsequent failure will be discussed. An X-ray diffraction technique for accurate determination of the fraction of each phase in PSZ will be applied to understanding the phase transformations and strain development. These results will be discussed in terms of developing a model for life prediction in PSZ coatings during thermal cycling.

High-resolution X-ray diffraction with no sample preparation

PubMed Central

Turner, S. M. R.; Degryse, P.; Shortland, A. J.

2017-01-01

It is shown that energy-dispersive X-ray diffraction (EDXRD) implemented in a back-reflection geometry is extremely insensitive to sample morphology and positioning even in a high-resolution configuration. This technique allows high-quality X-ray diffraction analysis of samples that have not been prepared and is therefore completely non-destructive. The experimental technique was implemented on beamline B18 at the Diamond Light Source synchrotron in Oxfordshire, UK. The majority of the experiments in this study were performed with pre-characterized geological materials in order to elucidate the characteristics of this novel technique and to develop the analysis methods. Results are presented that demonstrate phase identification, the derivation of precise unit-cell parameters and extraction of microstructural information on unprepared rock samples and other sample types. A particular highlight was the identification of a specific polytype of a muscovite in an unprepared mica schist sample, avoiding the time-consuming and difficult preparation steps normally required to make this type of identification. The technique was also demonstrated in application to a small number of fossil and archaeological samples. Back-reflection EDXRD implemented in a high-resolution configuration shows great potential in the crystallographic analysis of cultural heritage artefacts for the purposes of scientific research such as provenancing, as well as contributing to the formulation of conservation strategies. Possibilities for moving the technique from the synchrotron into museums are discussed. The avoidance of the need to extract samples from high-value and rare objects is a highly significant advantage, applicable also in other potential research areas such as palaeontology, and the study of meteorites and planetary materials brought to Earth by sample-return missions. PMID:28660862