Effect of crystallographic orientations of grains on the global mechanical properties of steel sheets by depth sensing indentation

NASA Astrophysics Data System (ADS)

Burik, P.; Pesek, L.; Kejzlar, P.; Andrsova, Z.; Zubko, P.

2017-01-01

The main idea of this work is using a physical model to prepare a virtual material with required properties. The model is based on the relationship between the microstructure and mechanical properties. The macroscopic (global) mechanical properties of steel are highly dependent upon microstructure, crystallographic orientation of grains, distribution of each phase present, etc... We need to know the local mechanical properties of each phase separately in multiphase materials. The grain size is a scale, where local mechanical properties are responsible for the behavior. Nanomechanical testing using depth sensing indentation (DSI) provides a straightforward solution for quantitatively characterizing each of phases in microstructure because it is very powerful technique for characterization of materials in small volumes. The aim of this experimental investigation is: (i) to prove how the mixing rule works for local mechanical properties (indentation hardness HIT) in microstructure scale using the DSI technique on steel sheets with different microstructure; (ii) to compare measured global properties with properties achieved by mixing rule; (iii) to analyze the effect of crystallographic orientations of grains on the mixing rule.

Microstructure characterization of multi-phase composites and utilization of phase change materials and recycled rubbers in cementitious materials

NASA Astrophysics Data System (ADS)

Meshgin, Pania

2011-12-01

This research focuses on two important subjects: (1) Characterization of heterogeneous microstructure of multi-phase composites and the effect of microstructural features on effective properties of the material. (2) Utilizations of phase change materials and recycled rubber particles from waste tires to improve thermal properties of insulation materials used in building envelopes. Spatial pattern of multi-phase and multidimensional internal structures of most composite materials are highly random. Quantitative description of the spatial distribution should be developed based on proper statistical models, which characterize the morphological features. For a composite material with multi-phases, the volume fraction of the phases as well as the morphological parameters of the phases have very strong influences on the effective property of the composite. These morphological parameters depend on the microstructure of each phase. This study intends to include the effect of higher order morphological details of the microstructure in the composite models. The higher order statistics, called two-point correlation functions characterize various behaviors of the composite at any two points in a stochastic field. Specifically, correlation functions of mosaic patterns are used in the study for characterizing transport properties of composite materials. One of the most effective methods to improve energy efficiency of buildings is to enhance thermal properties of insulation materials. The idea of using phase change materials and recycled rubber particles such as scrap tires in insulation materials for building envelopes has been studied.

Nonlinear optical microscopy and ultrasound imaging of human cervical structure

PubMed Central

Reusch, Lisa M.; Feltovich, Helen; Carlson, Lindsey C.; Hall, Gunnsteinn; Campagnola, Paul J.; Eliceiri, Kevin W.

2013-01-01

Abstract. The cervix softens and shortens as its collagen microstructure rearranges in preparation for birth, but premature change may lead to premature birth. The global preterm birth rate has not decreased despite decades of research, likely because cervical microstructure is poorly understood. Our group has developed a multilevel approach to evaluating the human cervix. We are developing quantitative ultrasound (QUS) techniques for noninvasive interrogation of cervical microstructure and corroborating those results with high-resolution images of microstructure from second harmonic generation imaging (SHG) microscopy. We obtain ultrasound measurements from hysterectomy specimens, prepare the tissue for SHG, and stitch together several hundred images to create a comprehensive view of large areas of cervix. The images are analyzed for collagen orientation and alignment with curvelet transform, and registered with QUS data, facilitating multiscale analysis in which the micron-scale SHG images and millimeter-scale ultrasound data interpretation inform each other. This novel combination of modalities allows comprehensive characterization of cervical microstructure in high resolution. Through a detailed comparative study, we demonstrate that SHG imaging both corroborates the quantitative ultrasound measurements and provides further insight. Ultimately, a comprehensive understanding of specific microstructural cervical change in pregnancy should lead to novel approaches to the prevention of preterm birth. PMID:23412434

Microstructure characterization of the non-modulated martensite in Ni-Mn-Ga alloy

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

Han, M.; Bennett, J.C.; Gharghouri, M.A.

2008-06-15

The microstructure of the non-modulated martensite in a Ni-Mn-Ga alloy has been characterized in detail by conventional transmission electron microscopy. Bright field images show that the martensite exhibits an internal substructure consisting of a high density of narrow twins. Using electron diffraction, it is found that the martensite has a tetragonal crystal structure. The lattice correspondence between the parent phase and the non-modulated martensite is investigated. Furthermore, the four twinning elements describing the microtwinning have been graphically and quantitatively determined. The results indicate that the microtwinning within the non-modulated martensite belongs to the compound type.

Application of ASTAR(TM)/Precession Electron Diffraction Technique to Quantitatively Study Defects in Nanocrystalline Metallic Materials

NASA Astrophysics Data System (ADS)

Ghamarian, Iman

Nanocrystalline metallic materials have the potential to exhibit outstanding performance which leads to their usage in challenging applications such as coatings and biomedical implant devices. To optimize the performance of nanocrystalline metallic materials according to the desired applications, it is important to have a decent understanding of the structure, processing and properties of these materials. Various efforts have been made to correlate microstructure and properties of nanocrystalline metallic materials. Based on these research activities, it is noticed that microstructure and defects (e.g., dislocations and grain boundaries) play a key role in the behavior of these materials. Therefore, it is of great importance to establish methods to quantitatively study microstructures, defects and their interactions in nanocrystalline metallic materials. Since the mechanisms controlling the properties of nanocrystalline metallic materials occur at a very small length scale, it is fairly difficult to study them. Unfortunately, most of the characterization techniques used to explore these materials do not have the high enough spatial resolution required for the characterization of these materials. For instance, by applying complex profile-fitting algorithms to X-ray diffraction patterns, it is possible to get an estimation of the average grain size and the average dislocation density within a relatively large area. However, these average values are not enough for developing meticulous phenomenological models which are able to correlate microstructure and properties of nanocrystalline metallic materials. As another example, electron backscatter diffraction technique also cannot be used widely in the characterization of these materials due to problems such as relative poor spatial resolution (which is 90 nm) and the degradation of Kikuchi diffraction patterns in severely deformed nano-size grain metallic materials. In this study, ASTAR(TM)/precession electron diffraction is introduced as a relatively new orientation microscopy technique to characterize defects (e.g., geometrically necessary dislocations and grain boundaries) in challenging nanocrystalline metallic materials. The capability of this characterization technique to quantitatively determine the dislocation density distributions of geometrically necessary dislocations in severely deformed metallic materials is assessed. Based on the developed method, it is possible to determine the distributions and accumulations of dislocations with respect to the nearest grain boundaries and triple junctions. Also, the competency of this technique to study the grain boundary character distributions of nanocrystalline metallic materials is presented.

Nanostructured Drugs Embedded into a Polymeric Matrix: Vinpocetine/PVP Hybrids Investigated by Debye Function Analysis.

PubMed

Hasa, Dritan; Giacobbe, Carlotta; Perissutti, Beatrice; Voinovich, Dario; Grassi, Mario; Cervellino, Antonio; Masciocchi, Norberto; Guagliardi, Antonietta

2016-09-06

Microcrystalline vinpocetine, coground with cross-linked polyvinylpyrrolidone, affords hybrids containing nanosized drug nanocrystals, the size and size distributions of which depend on milling times and drug-to-polymer weight ratios. Using an innovative approach to microstructural characterization, we analyzed wide-angle X-ray total scattering data by the Debye function analysis and demonstrated the possibility to characterize pharmaceutical solid dispersions obtaining a reliable quantitative view of the physicochemical status of the drug dispersed in an amorphous carrier. The microstructural properties derived therefrom have been successfully employed in reconciling the enigmatic difference in behavior between in vitro and in vivo solubility tests performed on nanosized vinpocetine embedded in a polymeric matrix.

Spatial variations in a.c. susceptibility and microstructure for the YBa2Cu3O(7-x) superconductor and their correlation with room-temperature ultrasonic measurements

NASA Technical Reports Server (NTRS)

Roth, Don J.; Hepp, Aloysius F.; Deguire, Mark R.; Dolhert, Leonard E.

1991-01-01

The spatial (within-sample) uniformity of superconducting behavior and microstructure in YBa2Cu30(7-x) specimens over the pore fraction range of 0.10 to 0.25 was examined. The viability of using a room-temperature, nondestructive characterization method (ultrasonic velocity imaging) to predict spatial variability was determined. Spatial variations in superconductor properties were observed for specimens containing 0.10 pore fraction. An ultrasonic velocity image constructed from measurements at 1 mm increments across one such specimen revealed microstructural variation between edge and center locations that correlated with variations in alternating-current shielding and loss behavior. Optical quantitative image analysis on sample cross-sections revealed pore fraction to be the varying microstructural feature.

Spatial variations in ac susceptibility and microstructure for the YBa2Cu3O(7-x) superconductor and their correlation with room-temperature ultrasonic measurements

NASA Technical Reports Server (NTRS)

Roth, Don J.; Deguire, Mark R.; Dolhert, Leonard E.; Hepp, Aloysius F.

1991-01-01

The spatial (within-sample) uniformity of superconducting behavior and microstructure in YBa2Cu3O(7-x) specimens over the pore fraction range of 0.10 to 0.25 was examined. The viability of using a room-temperature, nondestructive characterization method (ultrasonic velocity imaging) to predict spatial variability was determined. Spatial variations in superconductor properties were observed for specimens containing 0.10 pore fraction. An ultrasonic velocity image constructed from measurements at 1 mm increments across one such specimen revealed microstructural variation between edge and center locations that correlated with variations in alternating-current shielding and loss behavior. Optical quantitative image analysis on sample cross-sections revealed pore fraction to be the varying microstructural feature.

Characterizing microstructural features of biomedical samples by statistical analysis of Mueller matrix images

NASA Astrophysics Data System (ADS)

He, Honghui; Dong, Yang; Zhou, Jialing; Ma, Hui

2017-03-01

As one of the salient features of light, polarization contains abundant structural and optical information of media. Recently, as a comprehensive description of polarization property, the Mueller matrix polarimetry has been applied to various biomedical studies such as cancerous tissues detections. In previous works, it has been found that the structural information encoded in the 2D Mueller matrix images can be presented by other transformed parameters with more explicit relationship to certain microstructural features. In this paper, we present a statistical analyzing method to transform the 2D Mueller matrix images into frequency distribution histograms (FDHs) and their central moments to reveal the dominant structural features of samples quantitatively. The experimental results of porcine heart, intestine, stomach, and liver tissues demonstrate that the transformation parameters and central moments based on the statistical analysis of Mueller matrix elements have simple relationships to the dominant microstructural properties of biomedical samples, including the density and orientation of fibrous structures, the depolarization power, diattenuation and absorption abilities. It is shown in this paper that the statistical analysis of 2D images of Mueller matrix elements may provide quantitative or semi-quantitative criteria for biomedical diagnosis.

Stochastic Analysis and Design of Heterogeneous Microstructural Materials System

NASA Astrophysics Data System (ADS)

Xu, Hongyi

Advanced materials system refers to new materials that are comprised of multiple traditional constituents but complex microstructure morphologies, which lead to superior properties over the conventional materials. To accelerate the development of new advanced materials system, the objective of this dissertation is to develop a computational design framework and the associated techniques for design automation of microstructure materials systems, with an emphasis on addressing the uncertainties associated with the heterogeneity of microstructural materials. Five key research tasks are identified: design representation, design evaluation, design synthesis, material informatics and uncertainty quantification. Design representation of microstructure includes statistical characterization and stochastic reconstruction. This dissertation develops a new descriptor-based methodology, which characterizes 2D microstructures using descriptors of composition, dispersion and geometry. Statistics of 3D descriptors are predicted based on 2D information to enable 2D-to-3D reconstruction. An efficient sequential reconstruction algorithm is developed to reconstruct statistically equivalent random 3D digital microstructures. In design evaluation, a stochastic decomposition and reassembly strategy is developed to deal with the high computational costs and uncertainties induced by material heterogeneity. The properties of Representative Volume Elements (RVE) are predicted by stochastically reassembling SVE elements with stochastic properties into a coarse representation of the RVE. In design synthesis, a new descriptor-based design framework is developed, which integrates computational methods of microstructure characterization and reconstruction, sensitivity analysis, Design of Experiments (DOE), metamodeling and optimization the enable parametric optimization of the microstructure for achieving the desired material properties. Material informatics is studied to efficiently reduce the dimension of microstructure design space. This dissertation develops a machine learning-based methodology to identify the key microstructure descriptors that highly impact properties of interest. In uncertainty quantification, a comparative study on data-driven random process models is conducted to provide guidance for choosing the most accurate model in statistical uncertainty quantification. Two new goodness-of-fit metrics are developed to provide quantitative measurements of random process models' accuracy. The benefits of the proposed methods are demonstrated by the example of designing the microstructure of polymer nanocomposites. This dissertation provides material-generic, intelligent modeling/design methodologies and techniques to accelerate the process of analyzing and designing new microstructural materials system.

Characterizing ceramics and the interfacial adhesion to resin: I - The relationship of microstructure, composition, properties and fractography.

PubMed

Della Bona, Alvaro

2005-03-01

The appeal of ceramics as structural dental materials is based on their light weight, high hardness values, chemical inertness, and anticipated unique tribological characteristics. A major goal of current ceramic research and development is to produce tough, strong ceramics that can provide reliable performance in dental applications. Quantifying microstructural parameters is important to develop structure/property relationships. Quantitative microstructural analysis provides an association among the constitution, physical properties, and structural characteristics of materials. Structural reliability of dental ceramics is a major factor in the clinical success of ceramic restorations. Complex stress distributions are present in most practical conditions and strength data alone cannot be directly extrapolated to predict structural performance.

Characterization of a polymer-infiltrated ceramic-network material

PubMed Central

Corazza, Pedro H.; Zhang, Yu

2015-01-01

Objectives To characterize the microstructure and determine some mechanical properties of a polymer-ingfiltrated ceramic-network (PICN) material (Vita Enamic, Vita Zahnfabrik) available for CAD–CAM systems. Methods Specimens were fabricated to perform quantitative and qualitative analyses of the material’s microstructure and to determine the fracture toughness (KIc), density (ρ), Poisson’s ratio (v) and Young’s modulus (E). KIc was determined using V-notched specimens and the short beam toughness method, where bar-shaped specimens were notched and 3-point loaded to fracture. ρ was calculated using Archimedes principle, and v and E were measured using an ultrasonic thickness gauge with a combination of a pulse generator and an oscilloscope. Results Microstructural analyses showed a ceramic- and a polymer-based interpenetrating network. Mean and standard deviation values for the properties evaluated were: KIc = 1.09 ± 0.05 MPa m1/2, ρ = 2.09 ± 0.01 g/cm3, v = 0.23 ± 0.002 and E = 37.95 ± 0.34 GPa. Significance The PICN material showed mechanical properties between porcelains and resin-based composites, reflecting its microstructural components. PMID:24656471

Characterization of a polymer-infiltrated ceramic-network material.

PubMed

Della Bona, Alvaro; Corazza, Pedro H; Zhang, Yu

2014-05-01

To characterize the microstructure and determine some mechanical properties of a polymer-infiltrated ceramic-network (PICN) material (Vita Enamic, Vita Zahnfabrik) available for CAD-CAM systems. Specimens were fabricated to perform quantitative and qualitative analyses of the material's microstructure and to determine the fracture toughness (KIc), density (ρ), Poisson's ratio (ν) and Young's modulus (E). KIc was determined using V-notched specimens and the short beam toughness method, where bar-shaped specimens were notched and 3-point loaded to fracture. ρ was calculated using Archimedes principle, and ν and E were measured using an ultrasonic thickness gauge with a combination of a pulse generator and an oscilloscope. Microstructural analyses showed a ceramic- and a polymer-based interpenetrating network. Mean and standard deviation values for the properties evaluated were: KIc=1.09±0.05MPam(1/2), ρ=2.09±0.01g/cm(3), ν=0.23±0.002 and E=37.95±0.34GPa. The PICN material showed mechanical properties between porcelains and resin-based composites, reflecting its microstructural components. Copyright © 2014 Academy of Dental Materials. Published by Elsevier Ltd. All rights reserved.

Quantitatively characterizing microstructural variations of skin tissues during ultraviolet radiation damaging process based on Mueller matrix polarimetry

NASA Astrophysics Data System (ADS)

Sheng, Wei; He, Honghui; Dong, Yang; Ma, Hui

2018-02-01

As one of the most fundamental features of light, polarization can be used to develop imaging techniques which can provide insight into the optical and structural properties of tissues. Especially, the Mueller matrix polarimetry is suitable to detect the changes in collagen and elastic fibres, which are the main compositions of skin tissue. Here we demonstrate a novel quantitative, non-contact and in situ technique to monitor the microstructural variations of skin tissue during ultraviolet radiation (UVR) induced photoaging based on Mueller matrix polarimetry. Specifically, we measure the twodimensional (2D) backscattering Mueller matrices of nude mouse skin samples, then calculate and analyze the Mueller matrix derived parameters during the skin photoaging and self-repairing processes. To induce three-day skin photoaging, the back skin of each mouse is irradiated with UVR (0.05J/cm2) for five minutes per day. After UVR, the microstructures of the nude mouse skin are damaged. During the process of UV damage, we measure the backscattering Mueller matrices of the mouse skin samples and examine the relationship between the Mueller matrix parameters and the microstructural variations of skin tissue quantitatively. The comparisons between the UVR damaged groups with and without sunscreens show that the Mueller matrix derived parameters are potential indicators for fibrous microstructure variation in skin tissue. The pathological examinations and Monte Carlo simulations confirm the relationship between the values of Mueller matrix parameters and the changes of fibrous structures. Combined with smart phones or wearable devices, this technique may have a good application prospect in the fields of cosmetics and dermatological health.

Monitoring temporal microstructural variations of skeletal muscle tissues by multispectral Mueller matrix polarimetry

NASA Astrophysics Data System (ADS)

Dong, Yang; He, Honghui; He, Chao; Ma, Hui

2017-02-01

Mueller matrix polarimetry is a powerful tool for detecting microscopic structures, therefore can be used to monitor physiological changes of tissue samples. Meanwhile, spectral features of scattered light can also provide abundant microstructural information of tissues. In this paper, we take the 2D multispectral backscattering Mueller matrix images of bovine skeletal muscle tissues, and analyze their temporal variation behavior using multispectral Mueller matrix parameters. The 2D images of the Mueller matrix elements are reduced to the multispectral frequency distribution histograms (mFDHs) to reveal the dominant structural features of the muscle samples more clearly. For quantitative analysis, the multispectral Mueller matrix transformation (MMT) parameters are calculated to characterize the microstructural variations during the rigor mortis and proteolysis processes of the skeletal muscle tissue samples. The experimental results indicate that the multispectral MMT parameters can be used to judge different physiological stages for bovine skeletal muscle tissues in 24 hours, and combining with the multispectral technique, the Mueller matrix polarimetry and FDH analysis can monitor the microstructural variation features of skeletal muscle samples. The techniques may be used for quick assessment and quantitative monitoring of meat qualities in food industry.

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

Microstructural Characterization of a Directionally-Solidified Ni-33 (at. %)Al-31Cr-3Mo Eutectic Alloy as a Function of Withdrawal Rate

NASA Technical Reports Server (NTRS)

Raj, S. V.; Locci, I. E.; Whittenberger, J. D.; Salem, J. A.

2000-01-01

The Ni-33 (at. %)Al-3lCr-3Mo eutectic alloy was directionally-solidified (DS) at different rates, V(sub I), varying between 2.5 to 508 mm/ h. Detailed qualitative and quantitative metallographic and chemical analyses were conducted on the directionally-solidified rods. The microstructures consisted of eutectic colonies with parallel lamellar NiAl/(Cr,Mo) plates for solidification rates at and below 12.7 mm/ h. Cellular eutectic microstructures were observed at higher solidification rates, where the plates exhibited a radial pattern. The microstructures were demonstrated to be fairly uniform throughout a 100 mm length of the DS zone by quantitative metallography. The average cell size, bar-d, decreased with increasing growth rate to a value of 125 microns at 508 mm/ h according to the relation bar-d (microns) approx. = 465 V(sup -0.22, sub I), where V(sub I) is in mm/ h. Both the average NiAl plate thickness, bar-Delta(sub NiAl), and the interlamellar spacing, bar-lambda, were observed to be constant for V(sub I) less than or = 50.8 mm/ h but decreased with increasing growth rate above this value as 0.93 bar-Delta(sub NiAl)(microns) = 61.2 V(sup -0.93, sub I) and bar-lambda (microns) = 47.7 V(sup -0.64, sub I), respectively. The present results are detailed on a microstructural map. Keywords Optical microscopy, microstructure, compounds intermetallic, directional solidification

Property and microstructural nonuniformity in the yttrium-barium-copper-oxide superconductor determined from electrical, magnetic, and ultrasonic measurements. Ph.D. Thesis - Case Western Reserve Univ.

NASA Technical Reports Server (NTRS)

Roth, Don J.

1991-01-01

The purpose of this dissertation was the following: (1) to characterize the effect of pore fraction on a comprehensive set of electrical and magnetic properties for the yttrium-barium-copper-oxide (YBCO) high temperature ceramic superconductor; and (2) to determine the viability of using a room-temperature, nondestructive characterization method to aid in the prediction of superconducting (cryogenic) properties. The latter involved correlating ultrasonic velocity measurements at room temperature with property-affecting pore fraction and oxygen content variations. The use of ultrasonic velocity for estimating pore fraction in YBCO is presented, and other polycrystalline materials are reviewed, modeled, and statistically analyzed. This provides the basis for using ultrasonic velocity to interrogate microstructure. The effect of pore fraction (0.10-0.25) on superconductor properties of YBCO samples was characterized. Spatial (within-sample) variations in microstructure and superconductor properties were investigated, and the effect of oxygen content on elastic behavior was examined. Experimental methods used included a.c. susceptibility, electrical, and ultrasonic velocity measurements. Superconductor properties measured included transition temperature, magnetic transition width, transport and magnetic critical current density, magnetic shielding, a.c. loss, and sharpness of the voltage-current characteristics. An ultrasonic velocity image constructed from measurements at 1mm increments across a YBCO sample revealed microstructural variations that correlated with variations in magnetic shielding and a.c. loss behavior. Destructive examination using quantitative image analysis revealed pore fraction to be the varying microstructural feature.

Effects of white matter microstructure on phase and susceptibility maps.

PubMed

Wharton, Samuel; Bowtell, Richard

2015-03-01

To investigate the effects on quantitative susceptibility mapping (QSM) and susceptibility tensor imaging (STI) of the frequency variation produced by the microstructure of white matter (WM). The frequency offsets in a WM tissue sample that are not explained by the effect of bulk isotropic or anisotropic magnetic susceptibility, but rather result from the local microstructure, were characterized for the first time. QSM and STI were then applied to simulated frequency maps that were calculated using a digitized whole-brain, WM model formed from anatomical and diffusion tensor imaging data acquired from a volunteer. In this model, the magnitudes of the frequency contributions due to anisotropy and microstructure were derived from the results of the tissue experiments. The simulations suggest that the frequency contribution of microstructure is much larger than that due to bulk effects of anisotropic magnetic susceptibility. In QSM, the microstructure contribution introduced artificial WM heterogeneity. For the STI processing, the microstructure contribution caused the susceptibility anisotropy to be significantly overestimated. Microstructure-related phase offsets in WM yield artifacts in the calculated susceptibility maps. If susceptibility mapping is to become a robust MRI technique, further research should be carried out to reduce the confounding effects of microstructure-related frequency contributions. © 2014 Wiley Periodicals, Inc.

Effects of White Matter Microstructure on Phase and Susceptibility Maps

PubMed Central

Wharton, Samuel; Bowtell, Richard

2015-01-01

Purpose To investigate the effects on quantitative susceptibility mapping (QSM) and susceptibility tensor imaging (STI) of the frequency variation produced by the microstructure of white matter (WM). Methods The frequency offsets in a WM tissue sample that are not explained by the effect of bulk isotropic or anisotropic magnetic susceptibility, but rather result from the local microstructure, were characterized for the first time. QSM and STI were then applied to simulated frequency maps that were calculated using a digitized whole-brain, WM model formed from anatomical and diffusion tensor imaging data acquired from a volunteer. In this model, the magnitudes of the frequency contributions due to anisotropy and microstructure were derived from the results of the tissue experiments. Results The simulations suggest that the frequency contribution of microstructure is much larger than that due to bulk effects of anisotropic magnetic susceptibility. In QSM, the microstructure contribution introduced artificial WM heterogeneity. For the STI processing, the microstructure contribution caused the susceptibility anisotropy to be significantly overestimated. Conclusion Microstructure-related phase offsets in WM yield artifacts in the calculated susceptibility maps. If susceptibility mapping is to become a robust MRI technique, further research should be carried out to reduce the confounding effects of microstructure-related frequency contributions. Magn Reson Med 73:1258–1269, 2015. © 2014 Wiley Periodicals, Inc. PMID:24619643

Three dimensional microstructural characterization of nanoscale precipitates in AA7075-T651 by focused ion beam (FIB) tomography

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

Singh, Sudhanshu S.; Loza, Jose J.

2016-08-15

The size and distribution of precipitates in Al 7075 alloys affects both the mechanical and corrosion behavior (including stress corrosion cracking and fatigue corrosion) of the alloy. Three dimensional (3D) quantitative microstructural analysis of Al 7075 in the peak aged condition (T651) allows for a better understanding of these behaviors. In this study, Focused ion beam (FIB) tomography was used to characterize the microstructure in three dimensions. Analysis of grains and precipitates was performed in terms of volume, size, and morphology. It was found that the precipitates at the grain boundaries are larger in size, higher in aspect ratios andmore » maximum Feret diameter compared to the precipitates inside the grains, due to earlier nucleation of the precipitates at the grain boundaries. Our data on the precipitates at the interface between grains and Mg{sub 2}Si inclusion show that the surfaces of inclusion (impurity) particles can serve as a location for heterogeneous nucleation of precipitates. - Highlights: •Focused ion beam (FIB) tomography was used to characterize the microstructure of Al 7075 in three dimensions. •Analysis of grains and precipitates was performed in terms of volume, size, and morphology. •Precipitates at the grain boundaries have larger size and aspect ratio compared to the precipitates inside the grains.« less

Quantitative phase analysis and microstructure characterization of magnetite nanocrystals obtained by microwave assisted non-hydrolytic sol–gel synthesis

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

Sciancalepore, Corrado, E-mail: corrado.sciancalepore@unimore.it; Bondioli, Federica; INSTM Consortium, Via G. Giusti 9, 51121 Firenze

2015-02-15

An innovative preparation procedure, based on microwave assisted non-hydrolytic sol–gel synthesis, to obtain spherical magnetite nanoparticles was reported together with a detailed quantitative phase analysis and microstructure characterization of the synthetic products. The nanoparticle growth was analyzed as a function of the synthesis time and was described in terms of crystallization degree employing the Rietveld method on the magnetic nanostructured system for the determination of the amorphous content using hematite as internal standard. Product crystallinity increases as the microwave thermal treatment is increased and reaches very high percentages for synthesis times longer than 1 h. Microstructural evolution of nanocrystals wasmore » followed by the integral breadth methods to obtain information on the crystallite size-strain distribution. The results of diffraction line profile analysis were compared with nanoparticle grain distribution estimated by dimensional analysis of the transmission electron microscopy (TEM) images. A variation both in the average grain size and in the distribution of the coherently diffraction domains is evidenced, allowing to suppose a relationship between the two quantities. The traditional integral breadth methods have proven to be valid for a rapid assessment of the diffraction line broadening effects in the above-mentioned nanostructured systems and the basic assumption for the correct use of these methods are discussed as well. - Highlights: • Fe{sub 3}O{sub 4} nanocrystals were obtained by MW-assisted non-hydrolytic sol–gel synthesis. • Quantitative phase analysis revealed that crystallinity up to 95% was reached. • The strategy of Rietveld refinements was discussed in details. • Dimensional analysis showed nanoparticles ranging from 4 to 8 nm. • Results of integral breadth methods were compared with microscopic analysis.« less

Microstructural study of the nickel-base alloy WAZ-20 using qualitative and quantitative electron optical techniques

NASA Technical Reports Server (NTRS)

Young, S. G.

1973-01-01

The NASA nickel-base alloy WAZ-20 was analyzed by advanced metallographic techniques to qualitatively and quantitatively characterize its phases and stability. The as-cast alloy contained primary gamma-prime, a coarse gamma-gamma prime eutectic, a gamma-fine gamma prime matrix, and MC carbides. A specimen aged at 870 C for 1000 hours contained these same constituents and a few widely scattered high W particles. No detrimental phases (such as sigma or mu) were observed. Scanning electron microscope, light metallography, and replica electron microscope methods are compared. The value of quantitative electron microprobe techniques such as spot and area analysis is demonstrated.

Cement-based materials' characterization using ultrasonic attenuation

NASA Astrophysics Data System (ADS)

Punurai, Wonsiri

The quantitative nondestructive evaluation (NDE) of cement-based materials is a critical area of research that is leading to advances in the health monitoring and condition assessment of the civil infrastructure. Ultrasonic NDE has been implemented with varying levels of success to characterize cement-based materials with complex microstructure and damage. A major issue with the application of ultrasonic techniques to characterize cement-based materials is their inherent inhomogeneity at multiple length scales. Ultrasonic waves propagating in these materials exhibit a high degree of attenuation losses, making quantitative interpretations difficult. Physically, these attenuation losses are a combination of internal friction in a viscoelastic material (ultrasonic absorption), and the scattering losses due to the material heterogeneity. The objective of this research is to use ultrasonic attenuation to characterize the microstructure of heterogeneous cement-based materials. The study considers a real, but simplified cement-based material, cement paste---a common bonding matrix of all cement-based composites. Cement paste consists of Portland cement and water but does not include aggregates. First, this research presents the findings of a theoretical study that uses a set of existing acoustics models to quantify the scattered ultrasonic wavefield from a known distribution of entrained air voids. These attenuation results are then coupled with experimental measurements to develop an inversion procedure that directly predicts the size and volume fraction of entrained air voids in a cement paste specimen. Optical studies verify the accuracy of the proposed inversion scheme. These results demonstrate the effectiveness of using attenuation to measure the average size, volume fraction of entrained air voids and the existence of additional larger entrapped air voids in hardened cement paste. Finally, coherent and diffuse ultrasonic waves are used to develop a direct relationship between attenuation and water to cement (w/c) ratio. A phenomenological model based on the existence of fluid-filled capillary voids is used to help explain the experimentally observed behavior. Overall this research shows the potential of using ultrasonic attenuation to quantitatively characterize cement paste. The absorption and scattering losses can be related to the individual microstructural elements of hardened cement paste. By taking a fundamental, mechanics-based approach, it should be possible to add additional components such as scattering by aggregates or even microcracks in a systematic fashion and eventually build a realistic model for ultrasonic wave propagation study for concrete.

Symposium II: Mechanochemistry in Materials Science, MRS Fall Meeting, Nov 30-Dec 4, 2009, Boston, MA

DTIC Science & Technology

2010-09-02

Dynamic Mechanical Analysis (DMA). The fracture behavior of the mechanophore-linked polymer is also examined through the Double Cleavage Drilled ...multinary complex structures. Structural, microstructural, and chemical characterizations were explored by metrological tools to support this...simple hydrocarbons in order to quantitatively define structure-property relationships for reacting materials under shock compression. Embedded gauge

Investigation of Effects of Material Architecture on the Elastic Response of a Woven Ceramic Matrix Composite

NASA Technical Reports Server (NTRS)

Goldberg, Robert K.; Bonacuse, Peter J.; Mital, Subodh K.

2012-01-01

To develop methods for quantifying the effects of the microstructural variations of woven ceramic matrix composites on the effective properties and response of the material, a research program has been undertaken which is described in this paper. In order to characterize and quantify the variations in the microstructure of a five harness satin weave, CVI SiC/SiC, composite material, specimens were serially sectioned and polished to capture images that detailed the fiber tows, matrix, and porosity. Open source quantitative image analysis tools were then used to isolate the constituents and collect relevant statistics such as within ply tow spacing. This information was then used to build two dimensional finite element models that approximated the observed section geometry. With the aid of geometrical models generated by the microstructural characterization process, finite element models were generated and analyses were performed to quantify the effects of the microstructure and its variation on the effective stiffness and areas of stress concentration of the material. The results indicated that the geometry and distribution of the porosity appear to have significant effects on the through-thickness modulus. Similarly, stress concentrations on the outer surface of the composite appear to correlate to regions where the transverse tows are separated by a critical amount.

Additive Manufacturing of IN100 Superalloy Through Scanning Laser Epitaxy for Turbine Engine Hot-Section Component Repair: Process Development, Modeling, Microstructural Characterization, and Process Control

NASA Astrophysics Data System (ADS)

Acharya, Ranadip; Das, Suman

2015-09-01

This article describes additive manufacturing (AM) of IN100, a high gamma-prime nickel-based superalloy, through scanning laser epitaxy (SLE), aimed at the creation of thick deposits onto like-chemistry substrates for enabling repair of turbine engine hot-section components. SLE is a metal powder bed-based laser AM technology developed for nickel-base superalloys with equiaxed, directionally solidified, and single-crystal microstructural morphologies. Here, we combine process modeling, statistical design-of-experiments (DoE), and microstructural characterization to demonstrate fully metallurgically bonded, crack-free and dense deposits exceeding 1000 μm of SLE-processed IN100 powder onto IN100 cast substrates produced in a single pass. A combined thermal-fluid flow-solidification model of the SLE process compliments DoE-based process development. A customized quantitative metallography technique analyzes digital cross-sectional micrographs and extracts various microstructural parameters, enabling process model validation and process parameter optimization. Microindentation measurements show an increase in the hardness by 10 pct in the deposit region compared to the cast substrate due to microstructural refinement. The results illustrate one of the very few successes reported for the crack-free deposition of IN100, a notoriously "non-weldable" hot-section alloy, thus establishing the potential of SLE as an AM method suitable for hot-section component repair and for future new-make components in high gamma-prime containing crack-prone nickel-based superalloys.

Microstructural characterization, petrophysics and upscaling - from porous media to fractural media

NASA Astrophysics Data System (ADS)

Liu, J.; Liu, K.; Regenauer-Lieb, K.

2017-12-01

We present an integrated study for the characterization of complex geometry, fluid transport features and mechanical deformation at micro-scale and the upscaling of properties using microtomographic data: We show how to integrate microstructural characterization by the volume fraction, specific surface area, connectivity (percolation), shape and orientation of microstructures with identification of individual fractures from a 3D fractural network. In a first step we use stochastic analyses of microstructures to determine the geometric RVE (representative volume element) of samples. We proceed by determining the size of a thermodynamic RVE by computing upper/lower bounds of entropy production through Finite Element (FE) analyses on a series of models with increasing sizes. The minimum size for thermodynamic RVE's is identified on the basis of the convergence criteria of the FE simulations. Petrophysical properties (permeability and mechanical parameters, including plastic strength) are then computed numerically if thermodynamic convergence criteria are fulfilled. Upscaling of properties is performed by means of percolation theory. The percolation threshold is detected by using a shrinking/expanding algorithm on static micro-CT images of rocks. Parameters of the scaling laws can be extracted from quantitative analyses and/or numerical simulations on a series of models with similar structures but different porosities close to the percolation threshold. Different rock samples are analyzed. Characterizing parameters of porous/fractural rocks are obtained. Synthetic derivative models of the microstructure are used to estimate the relationships between porosity and mechanical properties. Results obtained from synthetic sandstones show that yield stress, cohesion and the angle of friction are linearly proportional to porosity. Our integrated study shows that digital rock technology can provide meaningful parameters for effective upscaling if thermodynamic volume averaging satisfies the convergence criteria. For strongly heterogeneous rocks, however, thermodynamic convergence criteria may not meet; a continuum approach cannot be justified in this case.

Chemical and Physical Characterization of Comp A-3 Type II Prills

DTIC Science & Technology

2013-06-01

the composition and properties of the explosive for implementation into modeling and simulation tools as part of the Multi-scale Response of...emulsion were identified using desorption-gas chromatography/mass spectroscopy (D-GC- MS) and Fourier transform infrared ( FTIR ) spectroscopy. Quantitative...understanding the microstructure of the pressed explosive and provides critical information for the development of a high fidelity particle-based course-grain

Microstructural Organization of Elastomeric Polyurethanes with Siloxane-Containing Soft Segments

NASA Astrophysics Data System (ADS)

Choi, Taeyi; Weklser, Jadwiga; Padsalgikar, Ajay; Runt, James

2011-03-01

In the present study, we investigate the microstructure of two series of segmented polyurethanes (PUs) containing siloxane-based soft segments and the same hard segments, the latter synthesized from diphenylmethane diisocyanate and butanediol. The first series is synthesized using a hydroxy-terminated polydimethylsiloxane macrodiol and varying hard segment contents. The second series are derived from an oligomeric diol containing both siloxane and aliphatic carbonate species. Hard domain morphologies were characterized using tapping mode atomic force microscopy and quantitative analysis of hard/soft segment demixing was conducted using small-angle X-ray scattering. The phase transitions of all materials were investigated using DSC and dynamic mechanical analysis, and hydrogen bonding by FTIR spectroscopy.

Quantitative Microstructure Characterization of a NMC Electrode

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

Usseglio Viretta, Francois L; Smith, Kandler A

Performance of lithium-ion batteries (LIBs) is strongly influenced by the porous microstructure of their electrodes. In this work, 3D microstructures of calendared and un-calendared positive electrode LiNi1/3Mn1/3Co1/3O2 (NMC) have been investigated in order to extract relevant properties useful for battery modeling. Transport (volume fraction, connectivity, particle size and tortuosity) and electrochemical (specific surface area) properties have been calculated for the pore and the active material. Special attention has been paid to determine the size of the so-called representative volume element (RVE) required to be statistically representative of the heterogeneous medium. Several parameters have been calculated using a panel of differentmore » numerical methods in order to compare their results. Besides, the image level of detail has been evaluated (using original criteria based upon edge detection) to assess the overall data quality available for the study.« less

Initial Assessment of X-Ray Computer Tomography image analysis for material defect microstructure

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

Kane, Joshua James; Windes, William Enoch

2016-06-01

The original development work leading to this report was focused on the non destructive three-dimensional (3-D) characterization of nuclear graphite as a means to better understand the nature of the inherent pore structure. The pore structure of graphite and its evolution under various environmental factors such as irradiation, mechanical stress, and oxidation plays an important role in their observed properties and characteristics. If we are to transition from an empirical understanding of graphite behavior to a truly predictive mechanistic understanding the pore structure must be well characterized and understood. As the pore structure within nuclear graphite is highly interconnected andmore » truly 3-D in nature, 3-D characterization techniques are critical. While 3-D characterization has been an excellent tool for graphite pore characterization, it is applicable to a broad number of materials systems over many length scales. Given the wide range of applications and the highly quantitative nature of the tool, it is quite surprising to discover how few materials researchers understand and how valuable of a tool 3-D image processing and analysis can be. Ultimately, this report is intended to encourage broader use of 3 D image processing and analysis in materials science and engineering applications, more specifically nuclear-related materials applications, by providing interested readers with enough familiarity to explore its vast potential in identifying microstructure changes. To encourage this broader use, the report is divided into two main sections. Section 2 provides an overview of some of the key principals and concepts needed to extract a wide variety of quantitative metrics from a 3-D representation of a material microstructure. The discussion includes a brief overview of segmentation methods, connective components, morphological operations, distance transforms, and skeletonization. Section 3 focuses on the application of concepts from Section 2 to relevant materials at Idaho National Laboratory. In this section, image analysis examples featuring nuclear graphite will be discussed in detail. Additionally, example analyses from Transient Reactor Test Facility low-enriched uranium conversion, Advanced Gas Reactor like compacts, and tristructural isotopic particles are shown to give a broader perspective of the applicability to relevant materials of interest.« less

Importance of Multimodal MRI in Characterizing Brain Tissue and Its Potential Application for Individual Age Prediction.

PubMed

Cherubini, Andrea; Caligiuri, Maria Eugenia; Peran, Patrice; Sabatini, Umberto; Cosentino, Carlo; Amato, Francesco

2016-09-01

This study presents a voxel-based multiple regression analysis of different magnetic resonance image modalities, including anatomical T1-weighted, T2(*) relaxometry, and diffusion tensor imaging. Quantitative parameters sensitive to complementary brain tissue alterations, including morphometric atrophy, mineralization, microstructural damage, and anisotropy loss, were compared in a linear physiological aging model in 140 healthy subjects (range 20-74 years). The performance of different predictors and the identification of the best biomarker of age-induced structural variation were compared without a priori anatomical knowledge. The best quantitative predictors in several brain regions were iron deposition and microstructural damage, rather than macroscopic tissue atrophy. Age variations were best resolved with a combination of markers, suggesting that multiple predictors better capture age-induced tissue alterations. The results of the linear model were used to predict apparent age in different regions of individual brain. This approach pointed to a number of novel applications that could potentially help highlighting areas particularly vulnerable to disease.

Two-Dimensional Nonlinear Finite Element Analysis of CMC Microstructures

NASA Technical Reports Server (NTRS)

Mital, Subodh K.; Goldberg, Robert K.; Bonacuse, Peter J.

2012-01-01

A research program has been developed to quantify the effects of the microstructure of a woven ceramic matrix composite and its variability on the effective properties and response of the material. In order to characterize and quantify the variations in the microstructure of a five harness satin weave, chemical vapor infiltrated (CVI) SiC/SiC composite material, specimens were serially sectioned and polished to capture images that detailed the fiber tows, matrix, and porosity. Open source quantitative image analysis tools were then used to isolate the constituents, from which two dimensional finite element models were generated which approximated the actual specimen section geometry. A simplified elastic-plastic model, wherein all stress above yield is redistributed to lower stress regions, is used to approximate the progressive damage behavior for each of the composite constituents. Finite element analyses under in-plane tensile loading were performed to examine how the variability in the local microstructure affected the macroscopic stress-strain response of the material as well as the local initiation and progression of damage. The macroscopic stress-strain response appeared to be minimally affected by the variation in local microstructure, but the locations where damage initiated and propagated appeared to be linked to specific aspects of the local microstructure.

Evaluation of agave fiber delignification by means of microscopy techniques and image analysis.

PubMed

Hernández-Hernández, Hilda M; Chanona-Pérez, Jorge J; Calderón-Domínguez, Georgina; Perea-Flores, María J; Mendoza-Pérez, Jorge A; Vega, Alberto; Ligero, Pablo; Palacios-González, Eduardo; Farrera-Rebollo, Reynold R

2014-10-01

Recently, the use of different types of natural fibers to produce paper and textiles from agave plants has been proposed. Agave atrovirens can be a good source of cellulose and lignin; nevertheless, the microstructural changes that happen during delignification have scarcely been studied. The aim of this work was to study the microstructural changes that occur during the delignification of agave fibers by means of microscopy techniques and image analysis. The fibers of A. atrovirens were obtained from leaves using convective drying, milling, and sieving. Fibers were processed using the Acetosolv pulping method at different concentrations of acetic acid; increasing acid concentration promoted higher levels of delignification, structural damage, and the breakdown of fiber clumps. Delignification followed by spectrometric analysis and microstructural studies were carried out by light, confocal laser scanning and scanning electron microscopy and showed that the delignification process follows three stages: initial, bulk, and residual. Microscopy techniques and image analysis were efficient tools for microstructural characterization during delignification of agave fibers, allowing quantitative evaluation of the process and the development of linear prediction models. The data obtained integrated numerical and microstructural information that could be valuable for the study of pulping of lignocellulosic materials.

Characterization of transition carbides in quench and partitioned steel microstructures by Mössbauer spectroscopy and complementary techniques

DOE PAGES

Pierce, D. T.; Coughlin, D. R.; Williamson, D. L.; ...

2015-05-01

Quenching and partitioning (Q&P) produces steel microstructures with martensite and austenite that exhibit promising property combinations for third generation advanced high strength steels. Understanding the kinetics of reactions that compete for available carbon, such as carbide formation, is critical for alloying and processing design and achieving austenite enrichment and retention during Q&P. Mössbauer effect spectroscopy (MES) was used to characterize Q&P microstructures in a 0.38C-1.54Mn-1.48Si wt.% steel after quenching to 225 °C and partitioning at 400 °C for 10 or 300 s, with an emphasis on transition carbides. The recoilless fraction for η-carbide was calculated and a correction for saturationmore » of the MES absorption spectrum was applied, making quantitative measurements of small amounts of η-carbide, including non-stoichiometric η-carbide, possible in Q&P microstructures. Complementary transmission electron microscopy confirmed the presence of η-carbides, and MES and X-ray diffraction were used to characterize the austenite. The amount of η-carbide formed during Q&P ranged from 1.4 to 2.4 at.%, accounting for a substantial portion (~24% to 41%) of the bulk carbon content of the steel. The amount (5.0 at.%) of η-carbide that formed after quenching and tempering (Q&T) at 400 °C for 300 s was significantly greater than after partitioning at 400 °C for 300 s (2.4 at.%), suggesting that carbon partitioning from martensite to austenite occurs in conjunction with η-carbide formation during Q&P in these specimens.« less

Scaling up the Single Transducer Thickness-Independent Ultrasonic Imaging Method for Accurate Characterization of Microstructural Gradients in Monolithic and Composite Tubular Structures

NASA Technical Reports Server (NTRS)

Roth, Don J.; Carney, Dorothy V.; Baaklini, George Y.; Bodis, James R.; Rauser, Richard W.

1998-01-01

Ultrasonic velocity/time-of-flight imaging that uses back surface reflections to gauge volumetric material quality is highly suited for quantitative characterization of microstructural gradients including those due to pore fraction, density, fiber fraction, and chemical composition variations. However, a weakness of conventional pulse-echo ultrasonic velocity/time-of-flight imaging is that the image shows the effects of thickness as well as microstructural variations unless the part is uniformly thick. This limits this imaging method's usefulness in practical applications. Prior studies have described a pulse-echo time-of-flight-based ultrasonic imaging method that requires using a single transducer in combination with a reflector plate placed behind samples that eliminates the effect of thickness variation in the image. In those studies, this method was successful at isolating ultrasonic variations due to material microstructure in plate-like samples of silicon nitride, metal matrix composite, and polymer matrix composite. In this study, the method is engineered for inspection of more complex-shaped structures-those having (hollow) tubular/curved geometry. The experimental inspection technique and results are described as applied to (1) monolithic mullite ceramic and polymer matrix composite 'proof-of-concept' tubular structures that contain machined patches of various depths and (2) as-manufactured monolithic silicon nitride ceramic and silicon carbide/silicon carbide composite tubular structures that might be used in 'real world' applications.

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.

On the feasibility of quantitative ultrasonic determination of fracture toughness: A literature review

NASA Technical Reports Server (NTRS)

Fu, L. S.

1980-01-01

The three main topics covered are: (1) fracture toughness and microstructure, (2) quantitative ultrasonic and microstructure; and (3) scattering and related mathematical methods. Literature in these areas is reviewed to give insight to the search of a theoretical foundation for quantitative ultrasonic measurement of fracture toughness. The literature review shows that fracture toughness is inherently related to the microstructure and in particular, it depends upon the spacing of inclusions or second particles and the aspect ratio of second phase particles. There are indications that ultrasonic velocity attenuation measurements can be used to determine fracture toughness. The leads to a review of the mathematical models available in solving boundary value problems related to microstructural factors that govern facture toughness and wave motion. A framework towards the theoretical study for the quantitative determination of fracture toughness is described and suggestions for future research are proposed.

Developing High-Frequency Quantitative Ultrasound Techniques to Characterize Three-Dimensional Engineered Tissues

NASA Astrophysics Data System (ADS)

Mercado, Karla Patricia E.

Tissue engineering holds great promise for the repair or replacement of native tissues and organs. Further advancements in the fabrication of functional engineered tissues are partly dependent on developing new and improved technologies to monitor the properties of engineered tissues volumetrically, quantitatively, noninvasively, and nondestructively over time. Currently, engineered tissues are evaluated during fabrication using histology, biochemical assays, and direct mechanical tests. However, these techniques destroy tissue samples and, therefore, lack the capability for real-time, longitudinal monitoring. The research reported in this thesis developed nondestructive, noninvasive approaches to characterize the structural, biological, and mechanical properties of 3-D engineered tissues using high-frequency quantitative ultrasound and elastography technologies. A quantitative ultrasound technique, using a system-independent parameter known as the integrated backscatter coefficient (IBC), was employed to visualize and quantify structural properties of engineered tissues. Specifically, the IBC was demonstrated to estimate cell concentration and quantitatively detect differences in the microstructure of 3-D collagen hydrogels. Additionally, the feasibility of an ultrasound elastography technique called Single Tracking Location Acoustic Radiation Force Impulse (STL-ARFI) imaging was demonstrated for estimating the shear moduli of 3-D engineered tissues. High-frequency ultrasound techniques can be easily integrated into sterile environments necessary for tissue engineering. Furthermore, these high-frequency quantitative ultrasound techniques can enable noninvasive, volumetric characterization of the structural, biological, and mechanical properties of engineered tissues during fabrication and post-implantation.

Quantitative characterization of the carbon/carbon composites components based on video of polarized light microscope.

PubMed

Li, Yixian; Qi, Lehua; Song, Yongshan; Chao, Xujiang

2017-06-01

The components of carbon/carbon (C/C) composites have significant influence on the thermal and mechanical properties, so a quantitative characterization of component is necessary to study the microstructure of C/C composites, and further to improve the macroscopic properties of C/C composites. Considering the extinction crosses of the pyrocarbon matrix have significant moving features, the polarized light microscope (PLM) video is used to characterize C/C composites quantitatively because it contains sufficiently dynamic and structure information. Then the optical flow method is introduced to compute the optical flow field between the adjacent frames, and segment the components of C/C composites from PLM image by image processing. Meanwhile the matrix with different textures is re-segmented by the length difference of motion vectors, and then the component fraction of each component and extinction angle of pyrocarbon matrix are calculated directly. Finally, the C/C composites are successfully characterized from three aspects of carbon fiber, pyrocarbon, and pores by a series of image processing operators based on PLM video, and the errors of component fractions are less than 15%. © 2017 Wiley Periodicals, Inc.

Widespread age-related differences in the human brain microstructure revealed by quantitative magnetic resonance imaging.

PubMed

Callaghan, Martina F; Freund, Patrick; Draganski, Bogdan; Anderson, Elaine; Cappelletti, Marinella; Chowdhury, Rumana; Diedrichsen, Joern; Fitzgerald, Thomas H B; Smittenaar, Peter; Helms, Gunther; Lutti, Antoine; Weiskopf, Nikolaus

2014-08-01

A pressing need exists to disentangle age-related changes from pathologic neurodegeneration. This study aims to characterize the spatial pattern and age-related differences of biologically relevant measures in vivo over the course of normal aging. Quantitative multiparameter maps that provide neuroimaging biomarkers for myelination and iron levels, parameters sensitive to aging, were acquired from 138 healthy volunteers (age range: 19-75 years). Whole-brain voxel-wise analysis revealed a global pattern of age-related degeneration. Significant demyelination occurred principally in the white matter. The observed age-related differences in myelination were anatomically specific. In line with invasive histologic reports, higher age-related differences were seen in the genu of the corpus callosum than the splenium. Iron levels were significantly increased in the basal ganglia, red nucleus, and extensive cortical regions but decreased along the superior occipitofrontal fascicle and optic radiation. This whole-brain pattern of age-associated microstructural differences in the asymptomatic population provides insight into the neurobiology of aging. The results help build a quantitative baseline from which to examine and draw a dividing line between healthy aging and pathologic neurodegeneration. Copyright © 2014 The Authors. Published by Elsevier Inc. All rights reserved.

Widespread age-related differences in the human brain microstructure revealed by quantitative magnetic resonance imaging☆

PubMed Central

Callaghan, Martina F.; Freund, Patrick; Draganski, Bogdan; Anderson, Elaine; Cappelletti, Marinella; Chowdhury, Rumana; Diedrichsen, Joern; FitzGerald, Thomas H.B.; Smittenaar, Peter; Helms, Gunther; Lutti, Antoine; Weiskopf, Nikolaus

2014-01-01

A pressing need exists to disentangle age-related changes from pathologic neurodegeneration. This study aims to characterize the spatial pattern and age-related differences of biologically relevant measures in vivo over the course of normal aging. Quantitative multiparameter maps that provide neuroimaging biomarkers for myelination and iron levels, parameters sensitive to aging, were acquired from 138 healthy volunteers (age range: 19–75 years). Whole-brain voxel-wise analysis revealed a global pattern of age-related degeneration. Significant demyelination occurred principally in the white matter. The observed age-related differences in myelination were anatomically specific. In line with invasive histologic reports, higher age-related differences were seen in the genu of the corpus callosum than the splenium. Iron levels were significantly increased in the basal ganglia, red nucleus, and extensive cortical regions but decreased along the superior occipitofrontal fascicle and optic radiation. This whole-brain pattern of age-associated microstructural differences in the asymptomatic population provides insight into the neurobiology of aging. The results help build a quantitative baseline from which to examine and draw a dividing line between healthy aging and pathologic neurodegeneration. PMID:24656835

Assessing White Matter Microstructure in Brain Regions with Different Myelin Architecture Using MRI.

PubMed

Groeschel, Samuel; Hagberg, Gisela E; Schultz, Thomas; Balla, Dávid Z; Klose, Uwe; Hauser, Till-Karsten; Nägele, Thomas; Bieri, Oliver; Prasloski, Thomas; MacKay, Alex L; Krägeloh-Mann, Ingeborg; Scheffler, Klaus

2016-01-01

We investigate how known differences in myelin architecture between regions along the cortico-spinal tract and frontal white matter (WM) in 19 healthy adolescents are reflected in several quantitative MRI parameters that have been proposed to non-invasively probe WM microstructure. In a clinically feasible scan time, both conventional imaging sequences as well as microstructural MRI parameters were assessed in order to quantitatively characterise WM regions that are known to differ in the thickness of their myelin sheaths, and in the presence of crossing or parallel fibre organisation. We found that diffusion imaging, MR spectroscopy (MRS), myelin water fraction (MWF), Magnetization Transfer Imaging, and Quantitative Susceptibility Mapping were myelin-sensitive in different ways, giving complementary information for characterising WM microstructure with different underlying fibre architecture. From the diffusion parameters, neurite density (NODDI) was found to be more sensitive than fractional anisotropy (FA), underlining the limitation of FA in WM crossing fibre regions. In terms of sensitivity to different myelin content, we found that MWF, the mean diffusivity and chemical-shift imaging based MRS yielded the best discrimination between areas. Multimodal assessment of WM microstructure was possible within clinically feasible scan times using a broad combination of quantitative microstructural MRI sequences. By assessing new microstructural WM parameters we were able to provide normative data and discuss their interpretation in regions with different myelin architecture, as well as their possible application as biomarker for WM disorders.

Analyzing Remodeling of Cardiac Tissue: A Comprehensive Approach Based on Confocal Microscopy and 3D Reconstructions

PubMed Central

Sachse, F. B.

2015-01-01

Microstructural characterization of cardiac tissue and its remodeling in disease is a crucial step in many basic research projects. We present a comprehensive approach for three-dimensional characterization of cardiac tissue at the submicrometer scale. We developed a compression-free mounting method as well as labeling and imaging protocols that facilitate acquisition of three-dimensional image stacks with scanning confocal microscopy. We evaluated the approach with normal and infarcted ventricular tissue. We used the acquired image stacks for segmentation, quantitative analysis and visualization of important tissue components. In contrast to conventional mounting, compression-free mounting preserved cell shapes, capillary lumens and extracellular laminas. Furthermore, the new approach and imaging protocols resulted in high signal-to-noise ratios at depths up to 60 μm. This allowed extensive analyses revealing major differences in volume fractions and distribution of cardiomyocytes, blood vessels, fibroblasts, myofibroblasts and extracellular space in control versus infarct border zone. Our results show that the developed approach yields comprehensive data on microstructure of cardiac tissue and its remodeling in disease. In contrast to other approaches, it allows quantitative assessment of all major tissue components. Furthermore, we suggest that the approach will provide important data for physiological models of cardiac tissue at the submicrometer scale. PMID:26399990

WHAT MAKES A GOOD PEDIATRIC TRANSPLANT LUNG: INSIGHTS FROM IN VIVO LUNG MORPHOMETRY WITH HYPERPOLARIZED 3HE MRI (WHAT MAKES A GOOD PEDIATRIC TRANSPLANT LUNG)

PubMed Central

Fishman, Emily F.; Quirk, James D.; Sweet, Stuart C.; Woods, Jason C.; Gierada, David S.; Conradi, Mark S.; Siegel, Marilyn J.; Yablonskiy, Dmitriy A.

2016-01-01

Background Obtaining information on transplanted lung microstructure is an important part of the current care for monitoring transplant recipients. However, until now this information was only available from invasive lung biopsy. The objective of this study was to evaluate the use of an innovative non-invasive technique in vivo lung morphometry with hyperpolarized 3He MRI - to characterize lung microstructure in the pediatric lung transplant population. This technique yields quantitative measurements of acinar airways’ (alveolar ducts and sacs) parameters, such as acinar airways radii and alveolar depth. Methods Six pediatric lung transplant recipients with cystic fibrosis underwent in vivo lung morphometry MRI, pulmonary function testing, and quantitative CT. Results We found a strong correlation between lung lifespan and alveolar depth - patients with more shallow alveoli were likely to have a negative outcome sooner than those with larger alveolar depth. Combining morphometric results with CT we also determined mean alveolar wall thickness and found substantial increases in this parameter in some patients that negatively correlated with DLCO. Conclusion In vivo lung morphometry uniquely provides previously unavailable information on lung microstructure that may be predictive of a negative outcome and has a potential to aid in lung selection for transplantation. PMID:28120553

Monitoring microstructural evolution of alloy 617 with non-linear acoustics for remaining useful life prediction; multiaxial creep-fatigue and creep-ratcheting

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

Lissenden, Cliff; Hassan, Tasnin; Rangari, Vijaya

The research built upon a prior investigation to develop a unified constitutive model for design-­by-­analysis of the intermediate heat exchanger (IHX) for a very high temperature reactor (VHTR) design of next generation nuclear plants (NGNPs). Model development requires a set of failure data from complex mechanical experiments to characterize the material behavior. Therefore uniaxial and multiaxial creep-­fatigue and creep-­ratcheting tests were conducted on the nickel-­base Alloy 617 at 850 and 950°C. The time dependence of material behavior, and the interaction of time dependent behavior (e.g., creep) with ratcheting, which is an increase in the cyclic mean strain under load-­controlled cycling,more » are major concerns for NGNP design. This research project aimed at characterizing the microstructure evolution mechanisms activated in Alloy 617 by mechanical loading and dwell times at elevated temperature. The acoustic harmonic generation method was researched for microstructural characterization. It is a nonlinear acoustics method with excellent potential for nondestructive evaluation, and even online continuous monitoring once high temperature sensors become available. It is unique because it has the ability to quantitatively characterize microstructural features well before macroscale defects (e.g., cracks) form. The nonlinear acoustics beta parameter was shown to correlate with microstructural evolution using a systematic approach to handle the complexity of multiaxial creep-­fatigue and creep-­ratcheting deformation. Mechanical testing was conducted to provide a full spectrum of data for: thermal aging, tensile creep, uniaxial fatigue, uniaxial creep-­fatigue, uniaxial creep-ratcheting, multiaxial creep-fatigue, and multiaxial creep-­ratcheting. Transmission Electron Microscopy (TEM), Scanning Electron Microscopy (SEM), and Optical Microscopy were conducted to correlate the beta parameter with individual microstructure mechanisms. We researched application of the harmonic generation method to tubular mechanical test specimens and pipes for nondestructive evaluation. Tubular specimens and pipes act as waveguides, thus we applied the acoustic harmonic generation method to guided waves in both plates and shells. Magnetostrictive transducers were used to generate and receive guided wave modes in the shell sample and the received signals were processed to show the sensitivity of higher harmonic generation to microstructure evolution. Modeling was initiated to correlate higher harmonic generation with the microstructure that will lead to development of a life prediction model that is informed by the nonlinear acoustics measurements.« less

Pressure-temperature dependence of nanowire formation in the arsenic-sulfur system

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

Riley, Brian J.; Johnson, Bradley R.; Sundaram, S. K.

2006-12-01

Nanowire Formation in Arsenic Trisulfide Brian J. Riley, S.K. Sundaram*, Bradley R. Johnson, Mark Engelhard Pacific Northwest National Laboratory, PO Box 999, Richland, WA 99352 * Corresponding author: Phone: 509-373-6665; Fax: 509-376-3108, E-mail: sk.Sundaram@pnl.gov Abstract: Arsenic trisulfide (As2S3) nanowires, nano-droplets, and micro-islands were synthesized on fused silica substrates, using a sublimation-condensation process at reduced pressures (70 mtorr – 70 torr) in a sealed ampoule. Microstructural control of the deposited thin film was achieved by controlling initial pressure, substrate temperature and substrate surface treatment. Microstructures were characterized using scanning electron microscopy (SEM), and energy dispersive spectrometry (EDS). Surface topography and chemistrymore » of the substrates were characterized using x-ray photoelectron spectroscopy (XPS) and atomic force microscopy (AFM). Semi-quantitative image analysis and basic curve-fitting were used to develop empirical models to mathematically describe the variation of microstructure as a function of initial pressure and substrate temperature and map out the regions of different microstructures in P-T space. Thermodyamic properties (available from literature) of this system are also incorporated in this map. Nanowires of an amorphous, transparent in visible-LWIR region, semi-conducting material, like As2S3, provide new opportunities for the development of novel nano-photonic and electronic devices. Additionally, this system provides an excellent opportunity to model (and control) microstructure development from nanometer to micron scales in a physical vapor deposition process, which is of great value to nanoscience and nanotechnology in general.« less

Atomic scale characterization of white etching area and its adjacent matrix in a martensitic 100Cr6 bearing steel

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

Li, Y.J., E-mail: y.li@mpie.de

Atom probe tomography was employed to characterize the microstructure and C distribution in the white etching area (WEA) of a martensitic 100Cr6 bearing steel subjected to rolling contact fatigue. Different from its surrounding matrix where a plate-like martensitic structure prevails, the WEA exhibits equiaxed grains with a uniform grain size of about 10 nm. Significant C grain boundary enrichment (>7.5at.%) and an overall higher C concentration than the nominal value are observed in the WEA. These results suggest that the formation of WEA results from severe local plastic deformation that causes dissolution of carbides and the redistribution of C. -more » Highlights: •APT has been applied to characterize the microstructure of white etching area (WEA). •Quantitative analyses of C distribution indicate that carbides are dissolved on the WEA. •WEA contains equiaxed grains with a uniform grain size of 10 nm. •C segregation at grain boundaries stabilizes the nanosized grain structure. •Formation of WEA is explained by severe local plastic deformation introduced by cyclic contact loading.« less

Direct comparison of Fe-Cr unmixing characterization by atom probe tomography and small angle scattering

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

Couturier, Laurent, E-mail: laurent.couturier55@ho

The fine microstructure obtained by unmixing of a solid solution either by classical precipitation or spinodal decomposition is often characterized either by small angle scattering or atom probe tomography. This article shows that a common data analysis framework can be used to analyze data obtained from these two techniques. An example of the application of this common analysis is given for characterization of the unmixing of the Fe-Cr matrix of a 15-5 PH stainless steel during long-term ageing at 350 °C and 400 °C. A direct comparison of the Cr composition fluctuations amplitudes and characteristic lengths obtained with both techniquesmore » is made showing a quantitative agreement for the fluctuation amplitudes. The origin of the discrepancy remaining for the characteristic lengths is discussed. - Highlights: •Common analysis framework for atom probe tomography and small angle scattering •Comparison of same microstructural characteristics obtained using both techniques •Good correlation of Cr composition fluctuations amplitudes from both techniques •Good correlation of Cr composition fluctuations amplitudes with classic V parameter.« less

Quantitative Evaluation of Aged AISI 316L Stainless Steel Sensitization to Intergranular Corrosion: Comparison Between Microstructural Electrochemical and Analytical Methods

NASA Astrophysics Data System (ADS)

Sidhom, H.; Amadou, T.; Sahlaoui, H.; Braham, C.

2007-06-01

The evaluation of the degree of sensitization (DOS) to intergranular corrosion (IGC) of a commercial AISI 316L austenitic stainless steel aged at temperatures ranging from 550 °C to 800 °C during 100 to 80,000 hours was carried out using three different assessment methods. (1) The microstructural method coupled with the Strauss standard test (ASTM A262). This method establishes the kinetics of the precipitation phenomenon under different aging conditions, by transmission electronic microscope (TEM) examination of thin foils and electron diffraction. The subsequent chromium-depleted zones are characterized by X-ray microanalysis using scanning transmission electronic microscope (STEM). The superimposition of microstructural time-temperature-precipitation (TTP) and ASTM A262 time-temperature-sensitization (TTS) diagrams provides the relationship between aged microstructure and IGC. Moreover, by considering the chromium-depleted zone characteristics, sensitization and desensitization criteria could be established. (2) The electrochemical method involving the double loop-electrochemical potentiokinetic reactivation (DL-EPR) test. The operating conditions of this test were initially optimized using the experimental design method on the bases of the reliability, the selectivity, and the reproducibility of test responses for both annealed and sensitized steels. The TTS diagram of the AISI 316L stainless steel was established using this method. This diagram offers a quantitative assessment of the DOS and a possibility to appreciate the time-temperature equivalence of the IGC sensitization and desensitization. (3) The analytical method based on the chromium diffusion models. Using the IGC sensitization and desensitization criteria established by the microstructural method, numerical solving of the chromium diffusion equations leads to a calculated AISI 316L TTS diagram. Comparison of these three methods gives a clear advantage to the nondestructive DL-EPR test when it is used with its optimized operating conditions. This quantitative method is simple to perform; it is fast, reliable, economical, and presents the best ability to detect the lowest DOS to IGC. For these reasons, this method can be considered as a serious candidate for IGC checking of stainless steel components of industrial plants.

Clinical Imaging of Bone Microarchitecture with HR-pQCT

PubMed Central

Nishiyama, Kyle K.; Shane, Elizabeth

2014-01-01

Osteoporosis, a disease characterized by loss of bone mass and structural deterioration, is currently diagnosed by dual-energy x-ray absorptiometry (DXA). However, DXA does not provide information about bone microstructure, which is a key determinant of bone strength. Recent advances in imaging permit the assessment of bone microstructure in vivo using high-resolution peripheral quantitative computed tomography (HR-pQCT). From these data, novel image processing techniques can be applied to characterize bone quality and strength. To date, most HR-pQCT studies are cross-sectional comparing subjects with and without fracture. These studies have shown that HR-pQCT is capable of discriminating fracture status independent of DXA. Recent longitudinal studies present new challenges in terms of analyzing the same region of interest and multisite calibrations. Careful application of analysis techniques and educated clinical interpretation of HR-pQCT results have improved our understanding of various bone-related diseases and will no doubt continue to do so in the future. PMID:23504496

Quantitative analysis and feature recognition in 3-D microstructural data sets

NASA Astrophysics Data System (ADS)

Lewis, A. C.; Suh, C.; Stukowski, M.; Geltmacher, A. B.; Spanos, G.; Rajan, K.

2006-12-01

A three-dimensional (3-D) reconstruction of an austenitic stainless-steel microstructure was used as input for an image-based finite-element model to simulate the anisotropic elastic mechanical response of the microstructure. The quantitative data-mining and data-warehousing techniques used to correlate regions of high stress with critical microstructural features are discussed. Initial analysis of elastic stresses near grain boundaries due to mechanical loading revealed low overall correlation with their location in the microstructure. However, the use of data-mining and feature-tracking techniques to identify high-stress outliers revealed that many of these high-stress points are generated near grain boundaries and grain edges (triple junctions). These techniques also allowed for the differentiation between high stresses due to boundary conditions of the finite volume reconstructed, and those due to 3-D microstructural features.

Towards modeling of cardiac micro-structure with catheter-based confocal microscopy: a novel approach for dye delivery and tissue characterization.

PubMed

Lasher, Richard A; Hitchcock, Robert W; Sachse, Frank B

2009-08-01

This work presents a methodology for modeling of cardiac tissue micro-structure. The approach is based on catheter-based confocal imaging systems, which are emerging as tools for diagnosis in various clinical disciplines. A limitation of these systems is that a fluorescent marker must be available in sufficient concentration in the imaged region. We introduce a novel method for the local delivery of fluorescent markers to cardiac tissue based on a hydro-gel carrier brought into contact with the tissue surface. The method was tested with living rabbit cardiac tissue and applied to acquire three-dimensional image stacks with a standard inverted confocal microscope and two-dimensional images with a catheter-based confocal microscope. We processed these image stacks to obtain spatial models and quantitative data on tissue microstructure. Volumes of atrial and ventricular myocytes were 4901 +/- 1713 and 10 299 +/-3598 mum (3) (mean+/-sd), respectively. Atrial and ventricular myocyte volume fractions were 72.4 +/-4.7% and 79.7 +/- 2.9% (mean +/-sd), respectively. Atrial and ventricular myocyte density was 165 571 +/- 55 836 and 86 957 +/- 32 280 cells/mm (3) (mean+/-sd), respectively. These statistical data and spatial descriptions of tissue microstructure provide important input for modeling studies of cardiac tissue function. We propose that the described methodology can also be used to characterize diseased tissue and allows for personalized modeling of cardiac tissue.

X-ray nanotomography analysis of the microstructural evolution of LiMn 2O 4 electrodes

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

Liu, Zhao; Han, Kai; Chen-Wiegart, Yu-chen Karen

One of the greatest challenges for advancing lithium-ion battery (LIB) technology is to minimize cell degradation during operation for long-term stability. To this end, it is important to understand how cell performance during operation relates to complex LIB microstructures. In this report, transmission X-ray microscopy (TXM) nanotomography is used to gain quantitative three-dimensional (3D) microstructure-performance correlations of LIB cathodes during cycling. The 3D microstructures of LiMn 2O 4 (LMO) electrodes, cycled under different conditions, including cycle number, operating voltage, and temperature, are characterized via TXM and statistically analyzed to investigate the impact of cycling conditions on the electrode microstructural evolutionmore » and cell performance. It is found that the number of cracks formed within LMO particles correlated with capacity fade. For the cell cycled at elevated temperatures, which exhibits the most severe capacity fade among all cells tested, mechanical cracking observed in TXM is not the only dominant contributor to the observed degradation. Mn 2+ dissolution, as verified by detection of Mn on the counter electrode by energy dispersive spectrometry, also contributed. The current work demonstrate 3D TXM nanotomography as a powerful tool to help probe in-depth.« less

X-ray nanotomography analysis of the microstructural evolution of LiMn 2O 4 electrodes

DOE PAGES

Liu, Zhao; Han, Kai; Chen-Wiegart, Yu-chen Karen; ...

2017-06-17

One of the greatest challenges for advancing lithium-ion battery (LIB) technology is to minimize cell degradation during operation for long-term stability. To this end, it is important to understand how cell performance during operation relates to complex LIB microstructures. In this report, transmission X-ray microscopy (TXM) nanotomography is used to gain quantitative three-dimensional (3D) microstructure-performance correlations of LIB cathodes during cycling. The 3D microstructures of LiMn 2O 4 (LMO) electrodes, cycled under different conditions, including cycle number, operating voltage, and temperature, are characterized via TXM and statistically analyzed to investigate the impact of cycling conditions on the electrode microstructural evolutionmore » and cell performance. It is found that the number of cracks formed within LMO particles correlated with capacity fade. For the cell cycled at elevated temperatures, which exhibits the most severe capacity fade among all cells tested, mechanical cracking observed in TXM is not the only dominant contributor to the observed degradation. Mn 2+ dissolution, as verified by detection of Mn on the counter electrode by energy dispersive spectrometry, also contributed. The current work demonstrate 3D TXM nanotomography as a powerful tool to help probe in-depth.« less

Early Stages of Microstructure and Texture Evolution during Beta Annealing of Ti-6Al-4V

NASA Astrophysics Data System (ADS)

Pilchak, A. L.; Sargent, G. A.; Semiatin, S. L.

2018-03-01

The early stages of microstructure evolution during annealing of Ti-6Al-4V in the beta phase field were established. For this purpose, a series of short-time heat treatments was performed using sheet samples that had a noticeable degree of alpha-phase microtexture in the as-received condition. Reconstruction of the beta-grain structure from electron-backscatter-diffraction measurements of the room-temperature alpha-phase texture revealed that microstructure evolution at short times was controlled not by general grain growth, but rather by nucleation-and-growth events analogous to discontinuous recrystallization. The nuclei comprised a small subset of beta grains that were highly misoriented relative to those comprising the principal texture component of the beta matrix. From a quantitative standpoint, the transformation kinetics were characterized by an Avrami exponent of approximately unity, thus suggestive of metadynamic recrystallization. The recrystallization process led to the weakening and eventual elimination of the initial beta texture through the growth of a population of highly misoriented grains.

Precipitation and Phase Transformations in 2101 Lean Duplex Stainless Steel During Isothermal Aging

NASA Astrophysics Data System (ADS)

Maetz, Jean-Yves; Cazottes, Sophie; Verdu, Catherine; Kleber, Xavier

2016-01-01

The effect of isothermal aging at 963 K (690 °C) on the microstructure of a 2101 lean duplex stainless steel, with the composition Fe-21.5Cr-5Mn-1.6Ni-0.22N-0.3Mo, was investigated using a multi-technique and multi-scale approach. The kinetics of phase transformation and precipitation was followed from a few minutes to thousands of hours using thermoelectric power measurements; based on these results, certain aging states were selected for electron microscopy characterization. Scanning electron microscopy, electron back-scattered diffraction, and transmission electron microscopy were used to quantitatively describe the microstructural evolution through crystallographic analysis, chemical analysis, and volume fraction measurements from the macroscopic scale down to the nanometric scale. During aging, the precipitation of M23C6 carbides, Cr2N nitrides, and σ phase as well as the transformation of ferrite into austenite and austenite into martensite was observed. These complex microstructural changes are controlled by Cr volume diffusion. The precipitation and phase transformation mechanisms are described.

The effect of solidification rate on the formability of nickel aluminide containing iron and boron

NASA Technical Reports Server (NTRS)

Carro, G.; Flanagan, W. F.

1987-01-01

Following reports that rapid solidification improves the ductility of some nickel aluminides, an investigation has been conducted of the possibility of additional improvement in a nickel aluminide containing both Fe and B. Free fall-solidified and free fall/splat-quenched samples similar to those producible under microgravity conditions in space were prepared, and their microstructure was characterized. Attention is given to the preliminary results of tests quantitatively measuring mechanical properties.

The Quantitative Microstructural Characterization of Multipass TIG Ultra Low Carbon Bainitic Steel Weldments and Correlation with Mechanical Properties

DTIC Science & Technology

1993-09-01

in TIG weldments. The alloying elements used in ULCB steels are; Carbon (C), Manganese (Mn), Molybdenum (Mo), Nickel (Ni), Niobium (Nb), Chromium (Cr...process. 7 C. WELDING PROCESSES 1. Tungsten Inert Gas (TIG) Welding Tungsten Inert Gas (TIG) Welding (or Gas Tungsten Arc Welding ( GTAW )), produces... chromium (Cr), molybdenum (Mo), and sometimes vanadium (V). Reheat cracking occurs in the HAZ during postweld stress relieving, especially in thick

Quantitative Analysis of Three-dimensional Microstructure of Li-ion Battery Electrodes

NASA Astrophysics Data System (ADS)

Liu, Zhao

Li-ion batteries (LIBs) have attracted considerable attention in the past two decades due to their widespread applications in portable electronics, and their growing use in electric vehicles and large-scale grid storage. Increasing battery energy density and powder density while maintaining long life, along with battery safety, are the biggest challenges that limit their further development. Various approaches with materials and chemistry have been employed to improve performance. However, one less-studied aspect that also impacts performance is the electrode microstructure. In particular, three-dimensional (3D) electrode microstructural data for LIB electrodes, which were not widely available prior to this thesis, can provide important input for understanding and improving LIB performance. The focus of this thesis is to apply 3D tomographic techniques, together with electrochemical performance data, to obtain LIB microstructure-performance correlations. Two advanced 3D structural analysis techniques, focused ion beam-scanning electron microscopy (FIB-SEM) and transmission X-ray microscopy (TXM) nanotomography, are used to quantify LIB electrode microstructure. 3D characterization of LIB electrode microstructure is used to obtain a deeper understanding of mechanisms that limit LIB performance. Microstructural characterization before and after cycling is used to explore capacity loss mechanisms. It is hoped that the results can guide electrode microstructures design to improve performance and stability. Two types of commercial electrodes, LiCoO2 and LiCoO 2/Li(Ni1/3Mn1/3Co1/3)O2, are studied using FIB-SEM and TXM. Both methods were found to be applicable to quantifying the oxide particle microstructure, including volume fraction, surface area, and particle size distribution, and results agreed well. However, structural inhomogeneity found in these commercial samples, limited the capability to resolve microstructural changes during cycling. In order to also quantify carbonaceous phases in the electrodes, which strongly correlate with LIB transport properties, a three-phase FIB-SEM method was developed where silicone resin was infiltrated into electrode pores, providing good image contrast with the carbon particles. Structural parameters including phase connectivity and tortuosity are quantified for commercial LiCoO 2 and laboratory-made LiFePO4 electrodes to help understand the transport process in these electrodes. For LiCoO2 electrodes, a heterogeneous tortuosity distribution observed in the electrolyte phase may result in inhomogeneous charge/discharge states, and consequently cause battery degradation. For LiFePO4 electrodes, highly percolated and less tortuous carbon found in a templated electrode explain its better high-C-rate performance. Finally, laboratory-made LiMn2O4 electrodes were electrochemically cycled with different operation parameters, including cycle number, temperature, and operating voltage. Quantitative analyses on 3D TXM data sets indicate particle fracture, mainly due to tetragonal to cubic phase transformations induced by the Jahn-Teller effect, resulting in electrode degradation. Moreover, high temperature operation is found to enhance active material dissolution and can also accelerate cell degradation. This ex-situ method, which combines electrochemical cycling and statistical analysis, proved to be an effective approach to provide insight for the interpretation of complex mechanical and electrochemical interactions within the electrodes.

Relationships between microstructure and mechanical properties of Ti-5Al-5Mo-5V-3Cr-1Zr alloy

NASA Astrophysics Data System (ADS)

Li, Z. Y.; Wu, G. Q.; Huang, Z.

2018-03-01

Through a statistical, quantitative analysis on microstructure of Ti-5Al-5Mo-5V-3Cr-1Zr (Ti55531) alloy, the relationships between microstructure and mechanical properties and heat treatment temperatures were investigated. The results show that in Widmanstätten structure, the size of β grain is greatly increased with increasing annealing temperature. Static toughness is related to grain boundary alpha phase discontinuity, the tensile strength is related to acicular alpha phase interface length and acicular alpha phase proportion. In duplex microstructure, the tensile strength is related to the equiaxed alpha proportion. Elongation, static toughness and crack forming work are related to the equiaxed alpha proportion and negatively related to secondary phase proportion. The microstructure can be described quantitatively and the mechanical properties can be predicted by analysis of microstructure.

The spatial-temporal characteristics of type I collagen-based extracellular matrix.

PubMed

Jones, Christopher Allen Rucksack; Liang, Long; Lin, Daniel; Jiao, Yang; Sun, Bo

2014-11-28

Type I collagen abounds in mammalian extracellular matrix (ECM) and is crucial to many biophysical processes. While previous studies have mostly focused on bulk averaged properties, here we provide a comprehensive and quantitative spatial-temporal characterization of the microstructure of type I collagen-based ECM as the gelation temperature varies. The structural characteristics including the density and nematic correlation functions are obtained by analyzing confocal images of collagen gels prepared at a wide range of gelation temperatures (from 16 °C to 36 °C). As temperature increases, the gel microstructure varies from a "bundled" network with strong orientational correlation between the fibers to an isotropic homogeneous network with no significant orientational correlation, as manifested by the decaying of length scales in the correlation functions. We develop a kinetic Monte-Carlo collagen growth model to better understand how ECM microstructure depends on various environmental or kinetic factors. We show that the nucleation rate, growth rate, and an effective hydrodynamic alignment of collagen fibers fully determines the spatiotemporal fluctuations of the density and orientational order of collagen gel microstructure. Also the temperature dependence of the growth rate and nucleation rate follow the prediction of classical nucleation theory.

The Effect of Post-heat Treatment on the Microstructures of Single Crystal DD6 Superalloy

NASA Astrophysics Data System (ADS)

Li, Dongfan; Gao, Hangshan; Wen, Zhixun; Li, Zhenwei; Yue, Zhufeng

2016-09-01

Various thermal cycles at the end of solution heat treatment and their influences on microstructure of single crystal superalloy DD6 were studied by experiments. During various thermal cycles, the qualitative and quantitative microstructure of samples quenched of the transformations is microscopically characterized. This completely includes the large changes in volume fraction, size distribution and morphology of gamma prime precipitate experienced in the upper temperature transformation. Noticeable deviation from the equilibrium volume fraction of γ' phase is detected in both the dissolution and precipitation processes above 1,120°C for both moderate cooling and heating rate; differences were mainly attributed to the unsteady nature of the turbulent flow. The growth and alignment of the γ' precipitates are deeply influenced by several factors, e.g. ageing time, cooling rate and quenching temperature. In addition, interesting findings such as "labyrinth" and "cluster" morphologies were observed by scanning electron microscope. During precipitation processes, the complicated microstructure evolution is illustrated by considering the consecutive equilibrium shapes of a coherent precipitate, which grows under the interaction with its neighbors and the coherency of the precipitates improves their potential to resist dissolution.

Use of EBSD Data in Numerical Analyses

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

Becker, R; Wiland, H

2000-01-14

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

A method for three-dimensional quantitative observation of the microstructure of biological samples

NASA Astrophysics Data System (ADS)

Wang, Pengfei; Chen, Dieyan; Ma, Wanyun; Wu, Hongxin; Ji, Liang; Sun, Jialin; Lv, Danyu; Zhang, Lu; Li, Ying; Tian, Ning; Zheng, Jinggao; Zhao, Fengying

2009-07-01

Contemporary biology has developed into the era of cell biology and molecular biology, and people try to study the mechanism of all kinds of biological phenomena at the microcosmic level now. Accurate description of the microstructure of biological samples is exigent need from many biomedical experiments. This paper introduces a method for 3-dimensional quantitative observation on the microstructure of vital biological samples based on two photon laser scanning microscopy (TPLSM). TPLSM is a novel kind of fluorescence microscopy, which has excellence in its low optical damage, high resolution, deep penetration depth and suitability for 3-dimensional (3D) imaging. Fluorescent stained samples were observed by TPLSM, and afterward the original shapes of them were obtained through 3D image reconstruction. The spatial distribution of all objects in samples as well as their volumes could be derived by image segmentation and mathematic calculation. Thus the 3-dimensionally and quantitatively depicted microstructure of the samples was finally derived. We applied this method to quantitative analysis of the spatial distribution of chromosomes in meiotic mouse oocytes at metaphase, and wonderful results came out last.

Experimental and model based investigation of the links between snow bidirectional reflectance and snow microstructure

NASA Astrophysics Data System (ADS)

Dumont, M.; Flin, F.; Malinka, A.; Brissaud, O.; Hagenmuller, P.; Dufour, A.; Lapalus, P.; Lesaffre, B.; Calonne, N.; Rolland du Roscoat, S.; Ando, E.

2017-12-01

Snow optical properties are unique among Earth surface and crucial for a wide range of applications. The bi-directional reflectance, hereafter BRDF, of snow is sensible to snow microstructure. However the complex interplays between different parameters of snow microstructure namely size parameters and shape parameters on reflectance are challenging to disentangle both theoretically and experimentally. An accurate understanding and modelling of snow BRDF is required to correctly process satellite data. BRDF measurements might also provide means of characterizing snow morphology. This study presents one of the very few dataset that combined bi-directional reflectance measurements over 500-2500 nm and X-ray tomography of the snow microstructure for three different snow samples and two snow types. The dataset is used to evaluate the approach from Malinka, 2014 that relates snow optical properties to the chord length distribution in the snow microstructure. For low and medium absorption, the model accurately reproduces the measurements but tends to slightly overestimate the anisotropy of the reflectance. The model indicates that the deviation of the ice chord length distribution from an exponential distribution, that can be understood as a characterization of snow types, does not impact the reflectance for such absorptions. The simulations are also impacted by the uncertainties in the ice refractive index values. At high absorption and high viewing/incident zenith angle, the simulations and the measurements disagree indicating that some of the assumptions made in the model are not met anymore. The study also indicates that crystal habits might play a significant role for the reflectance under such geometries and wavelengths. However quantitative relationship between crystal habits and reflectance alongside with potential optical methodologies to classify snow morphology would require an extended dataset over more snow types. This extended dataset can likely be obtained thanks to the use of ray tracing models on tomography images of the snow microstructure.

Microstructure characterization via stereological relations — A shortcut for beginners

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

Pabst, Willi, E-mail: pabstw@vscht.cz; Gregorová, Eva; Uhlířová, Tereza

Stereological relations that can be routinely applied for the quantitative characterization of microstructures of heterogeneous single- and two-phase materials via global microstructural descriptors are reviewed. It is shown that in the case of dense, single-phase polycrystalline materials (e.g., transparent yttrium aluminum garnet ceramics) two quantities have to be determined, the interface density (or, equivalently, the mean chord length of the grains) and the mean curvature integral density (or, equivalently, the Jeffries grain size), while for two-phase materials (e.g., highly porous, cellular alumina ceramics), one additional quantity, the volume fraction (porosity), is required. The Delesse–Rosiwal law is recalled and size measuresmore » are discussed. It is shown that the Jeffries grain size is based on the triple junction line length density, while the mean chord length of grains is based on the interface density (grain boundary area density). In contrast to widespread belief, however, these two size measures are not alternative, but independent (and thus complementary), measures of grain size. Concomitant with this fact, a clear distinction between linear and planar grain size numbers is proposed. Finally, based on our concept of phase-specific quantities, it is shown that under certain conditions it is possible to define a Jeffries size also for two-phase materials and that the ratio of the mean chord length and the Jeffries size has to be considered as an invariant number for a certain type of microstructure, i.e., a characteristic value that is independent of the absolute size of the microstructural features (e.g., grains, inclusions or pores). - Highlights: • Stereology-based image analysis is reviewed, including error considerations. • Recipes are provided for measuring global metric microstructural descriptors. • Size measures are based on interface density and mean curvature integral density. • Phase-specific quantities and a generalized Jeffries size are introduced. • Linear and planar grain size numbers are clearly distinguished and explained.« less

Analysis of in-service failures and advances in microstructural characterization. Microstructural science Volume 26

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

Abramovici, E.; Northwood, D.O.; Shehata, M.T.

1999-01-01

The contents include Analysis of In-Service Failures (tutorials, transportation industry, corrosion and materials degradation, electronic and advanced materials); 1998 Sorby Award Lecture by Kay Geels, Struers A/S (Metallographic Preparation from Sorby to the Present); Advances in Microstructural Characterization (characterization techniques using high resolution and focused ion beam, characterization of microstructural clustering and correlation with performance); Advanced Applications (advanced alloys and intermetallic compounds, plasma spray coatings and other surface coatings, corrosion, and materials degradation).

Multi-scale modeling of microstructure dependent intergranular brittle fracture using a quantitative phase-field based method

DOE PAGES

Chakraborty, Pritam; Zhang, Yongfeng; Tonks, Michael R.

2015-12-07

In this study, the fracture behavior of brittle materials is strongly influenced by their underlying microstructure that needs explicit consideration for accurate prediction of fracture properties and the associated scatter. In this work, a hierarchical multi-scale approach is pursued to model microstructure sensitive brittle fracture. A quantitative phase-field based fracture model is utilized to capture the complex crack growth behavior in the microstructure and the related parameters are calibrated from lower length scale atomistic simulations instead of engineering scale experimental data. The workability of this approach is demonstrated by performing porosity dependent intergranular fracture simulations in UO 2 and comparingmore » the predictions with experiments.« less

Multi-scale modeling of microstructure dependent intergranular brittle fracture using a quantitative phase-field based method

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

Chakraborty, Pritam; Zhang, Yongfeng; Tonks, Michael R.

In this study, the fracture behavior of brittle materials is strongly influenced by their underlying microstructure that needs explicit consideration for accurate prediction of fracture properties and the associated scatter. In this work, a hierarchical multi-scale approach is pursued to model microstructure sensitive brittle fracture. A quantitative phase-field based fracture model is utilized to capture the complex crack growth behavior in the microstructure and the related parameters are calibrated from lower length scale atomistic simulations instead of engineering scale experimental data. The workability of this approach is demonstrated by performing porosity dependent intergranular fracture simulations in UO 2 and comparingmore » the predictions with experiments.« less

Microstructural Development during Directional Solidification of Peritectic Alloys

NASA Technical Reports Server (NTRS)

Lograsso, Thomas A.

1996-01-01

A thorough understanding of the microstructures produced through solidification in peritectic systems has yet to be achieved, even though a large number of industrially and scientifically significant materials are in this class. One type of microstructure frequently observed during directional solidification consists of alternating layers of primary solid and peritectic solid oriented perpendicular to the growth direction. This layer formation is usually reported for alloy compositions within the two-phase region of the peritectic isotherm and for temperature gradient and growth rate conditions that result in a planar solid-liquid interface. Layered growth in peritectic alloys has not previously been characterized on a quantitative basis, nor has a mechanism for its formation been verified. The mechanisms that have been proposed for layer formation can be categorized as either extrinsic or intrinsic to the alloy system. The extrinsic mechanisms rely on externally induced perturbations to the system for layer formation, such as temperature oscillations, growth velocity variations, or vibrations. The intrinsic mechanisms approach layer formation as an alternative type of two phase growth that is inherent for certain peritectic systems and solidification conditions. Convective mixing of the liquid is an additional variable which can strongly influence the development and appearance of layers due to the requisite slow growth rate. The first quantitative description of layer formation is a model recently developed by Trivedi based on the intrinsic mechanism of cyclic accumulation and depiction of solute in the liquid ahead of the interface, linked to repeated nucleation events in the absence of convection. The objective of this research is to characterize the layered microstructures developed during ground-based experiments in which external influences have been minimized as much as possible and to compare these results to the current the model. Also, the differences between intrinsic and externally influenced layer formation were explored. The choice of alloy system is critical to a study of the formation of layered microstructures. The ideal system would have a well-characterized phase diagram, equal densities of both elements in the liquid state to minimize compositionally-driven convective flows, a low peritectic temperature to simplify directional solidification and the achievement of a high temperature gradient in the liquid, a broad composition range for the peritectic reaction, and a reasonable hardness at room temperature to facilitate handling and metallographic preparation. The In-Sn system was selected initially due to a very low peritectic temperature and the nearly equal densities of In and Sn in the liquid state. Since the In-rich peritectic reaction had apparently not been utilized previously for solidification research, experiments were conducted to check the phase diagram in the region of interest. The alloys in this system proved to be difficult to handle and prepare in bulk form with the equipment available, so experiments were initiated with the Sn-Cd system. Layered microstructures had been observed previously in Sn-Cd.

High-Resolution Characterization of UMo Alloy Microstructure

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

Devaraj, Arun; Kovarik, Libor; Joshi, Vineet V.

2016-11-30

This report highlights the capabilities and procedure for high-resolution characterization of UMo fuels in PNNL. Uranium-molybdenum (UMo) fuel processing steps, from casting to forming final fuel, directly affect the microstructure of the fuel, which in turn dictates the in-reactor performance of the fuel under irradiation. In order to understand the influence of processing on UMo microstructure, microstructure characterization techniques are necessary. Higher-resolution characterization techniques like transmission electron microscopy (TEM) and atom probe tomography (APT) are needed to interrogate the details of the microstructure. The findings from TEM and APT are also directly beneficial for developing predictive multiscale modeling tools thatmore » can predict the microstructure as a function of process parameters. This report provides background on focused-ion-beam–based TEM and APT sample preparation, TEM and APT analysis procedures, and the unique information achievable through such advanced characterization capabilities for UMo fuels, from a fuel fabrication capability viewpoint.« less

AxTract: Toward microstructure informed tractography.

PubMed

Girard, Gabriel; Daducci, Alessandro; Petit, Laurent; Thiran, Jean-Philippe; Whittingstall, Kevin; Deriche, Rachid; Wassermann, Demian; Descoteaux, Maxime

2017-11-01

Diffusion-weighted (DW) magnetic resonance imaging (MRI) tractography has become the tool of choice to probe the human brain's white matter in vivo. However, tractography algorithms produce a large number of erroneous streamlines (false positives), largely due to complex ambiguous tissue configurations. Moreover, the relationship between the resulting streamlines and the underlying white matter microstructure characteristics remains poorly understood. In this work, we introduce a new approach to simultaneously reconstruct white matter fascicles and characterize the apparent distribution of axon diameters within fascicles. To achieve this, our method, AxTract, takes full advantage of the recent development DW-MRI microstructure acquisition, modeling, and reconstruction techniques. This enables AxTract to separate parallel fascicles with different microstructure characteristics, hence reducing ambiguities in areas of complex tissue configuration. We report a decrease in the incidence of erroneous streamlines compared to the conventional deterministic tractography algorithms on simulated data. We also report an average increase in streamline density over 15 known fascicles of the 34 healthy subjects. Our results suggest that microstructure information improves tractography in crossing areas of the white matter. Moreover, AxTract provides additional microstructure information along the fascicle that can be studied alongside other streamline-based indices. Overall, AxTract provides the means to distinguish and follow white matter fascicles using their microstructure characteristics, bringing new insights into the white matter organization. This is a step forward in microstructure informed tractography, paving the way to a new generation of algorithms able to deal with intricate configurations of white matter fibers and providing quantitative brain connectivity analysis. Hum Brain Mapp 38:5485-5500, 2017. © 2017 Wiley Periodicals, Inc. © 2017 Wiley Periodicals, Inc.

Microstructural characterization of multiphase chocolate using X-ray microtomography.

PubMed

Frisullo, Pierangelo; Licciardello, Fabio; Muratore, Giuseppe; Del Nobile, Matteo Alessandro

2010-09-01

In this study, X-ray microtomography (μCT) was used for the image analysis of the microstructure of 12 types of Italian aerated chocolate chosen to exhibit variability in terms of cocoa mass content. Appropriate quantitative 3-dimensional parameters describing the microstructure were calculated, for example, the structure thickness (ST), object structure volume ratio (OSVR), and the percentage object volume (POV). Chemical analysis was also performed to correlate the microstructural data to the chemical composition of the samples. Correlation between the μCT parameters acquired for the pore microstructure evaluation and the chemical analysis revealed that the sugar crystals content does not influence the pore structure and content. On the other hand, it revealed that there is a strong correlation between the POV and the sugar content obtained by chemical analysis. The results from this study show that μCT is a suitable technique for the microstructural analysis of confectionary products such as chocolates and not only does it provide an accurate analysis of the pores and microstructure but the data obtained could also be used to aid in the assessment of its composition and consistency with label specifications. X-ray microtomography (μCT) is a noninvasive and nondestructive 3-D imaging technique that has several advantages over other methods, including the ability to image low-moisture materials. Given the enormous success of μCT in medical applications, material science, chemical engineering, geology, and biology, it is not surprising that in recent years much attention has been focused on extending this imaging technique to food science as a useful technique to aid in the study of food microstructure. X-ray microtomography provides in-depth information on the microstructure of the food product being tested; therefore, a better understanding of the physical structure of the product and from an engineering perspective, knowledge about the microstructure of foods can be used to identify the important processing parameters that affect the quality of a product.

Small angle neutron scattering study of nano sized microstructure in Fe-Cr ODS steels for gen IV in-core applications.

PubMed

Han, Young-Soo; Mao, Xiadong; Jang, Jinsung

2013-11-01

The nano-sized microstructures in Fe-Cr oxide dispersion strengthened steel for Gen IV in-core applications were studied using small angle neutron scattering. The oxide dispersion strengthened steel was manufactured through hot isostatic pressing with various chemical compositions and fabrication conditions. Small angle neutron scattering experiments were performed using a 40 m small angle neutron scattering instrument at HANARO. Nano sized microstructures, namely, yttrium oxides and Cr-oxides were quantitatively analyzed by small angle neutron scattering. The yttrium oxides and Cr-oxides were also observed by transmission electron microscopy. The microstructural analysis results from small angle neutron scattering were compared with those obtained by transmission electron microscopy. The effects of the chemical compositions and fabrication conditions on the microstructure were investigated in relation to the quantitative microstructural analysis results obtained by small angle neutron scattering. The volume fraction of Y-oxide increases after fabrication, and this result is considered to be due to the formation of non-stochiometric Y-Ti-oxides.

3D characterization of trans- and inter-lamellar fatigue crack in (α + β) Ti alloy

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

Babout, Laurent, E-mail: Laurent.babout@p.lodz.pl; Jopek, Łukasz; Preuss, Michael

2014-12-15

This paper presents a three dimensional image processing strategy that has been developed to quantitatively analyze and correlate the path of a fatigue crack with the lamellar microstructure found in Ti-6246. The analysis is carried out on X-ray microtomography images acquired in situ during uniaxial fatigue testing. The crack, the primary β-grain boundaries and the α lamellae have been segmented separately and merged for the first time to allow a better characterization and understanding of their mutual interaction. This has particularly emphasized the role of translamellar crack growth at a very high propagation angle with regard to the lamellar orientation,more » supporting the central role of colonies favorably oriented for basal 〈a〉 slip to guide the crack in the fully lamellar microstructure of Ti alloy. - Highlights: • 3D tomography images reveal strong short fatigue crack interaction with α lamellae. • Proposed 3D image processing methodology makes their segmentation possible. • Crack-lamellae orientation maps show prevalence of translamellar cracking. • Angle study comforts the influence of basal/prismatic slip on crack path.« less

Influence of the ferritic-pearlitic steel microstructure on surface roughness in broaching of automotive steels

NASA Astrophysics Data System (ADS)

Arrieta, I.; Courbon, C.; Cabanettes, F.; Arrazola, P.-J.; Rech, J.

2017-10-01

The aim of this work is to characterize the effect of microstructural parameters on surface roughness in dry broaching with a special emphasis on the ferrite-pearlite (FP) ratio. An experimental approach combining cutting and tribological tests has been developed on three grades 27MnCr5, C45, C60 covering a wide range of FP ratio. Fundamental broaching tests have been performed with a single tooth to analyse the resulting surface quality with uncoated M35 HSS tools. A specially designed open tribometer has been used to characterize the friction coefficient at the tool-chip-workpiece interface under appropriate conditions. Specific phenomena have been observed depending on the FP ratio and an interesting correlation with the tribological tests has been found. This clearly shows that friction has an important contribution in broaching and that phase distribution has to be highly considered when cutting a FP steel at a microscopic scale. This work also provides quantitative data of the friction coefficient depending on the sliding velocity and FP content which can be implemented in any analytical or numerical model of a broaching operation.

Ultrasound Imaging Techniques for Spatiotemporal Characterization of Composition, Microstructure, and Mechanical Properties in Tissue Engineering.

PubMed

Deng, Cheri X; Hong, Xiaowei; Stegemann, Jan P

2016-08-01

Ultrasound techniques are increasingly being used to quantitatively characterize both native and engineered tissues. This review provides an overview and selected examples of the main techniques used in these applications. Grayscale imaging has been used to characterize extracellular matrix deposition, and quantitative ultrasound imaging based on the integrated backscatter coefficient has been applied to estimating cell concentrations and matrix morphology in tissue engineering. Spectral analysis has been employed to characterize the concentration and spatial distribution of mineral particles in a construct, as well as to monitor mineral deposition by cells over time. Ultrasound techniques have also been used to measure the mechanical properties of native and engineered tissues. Conventional ultrasound elasticity imaging and acoustic radiation force imaging have been applied to detect regions of altered stiffness within tissues. Sonorheometry and monitoring of steady-state excitation and recovery have been used to characterize viscoelastic properties of tissue using a single transducer to both deform and image the sample. Dual-mode ultrasound elastography uses separate ultrasound transducers to produce a more potent deformation force to microscale characterization of viscoelasticity of hydrogel constructs. These ultrasound-based techniques have high potential to impact the field of tissue engineering as they are further developed and their range of applications expands.

Noninvasive Quantitative Imaging of Collagen Microstructure in Three-Dimensional Hydrogels Using High-Frequency Ultrasound

PubMed Central

Mercado, Karla P.; Helguera, María; Hocking, Denise C.

2015-01-01

Collagen I is widely used as a natural component of biomaterials for both tissue engineering and regenerative medicine applications. The physical and biological properties of fibrillar collagens are strongly tied to variations in collagen fiber microstructure. The goal of this study was to develop the use of high-frequency quantitative ultrasound to assess collagen microstructure within three-dimensional (3D) hydrogels noninvasively and nondestructively. The integrated backscatter coefficient (IBC) was employed as a quantitative ultrasound parameter to detect, image, and quantify spatial variations in collagen fiber density and diameter. Collagen fiber microstructure was varied by fabricating hydrogels with different collagen concentrations or polymerization temperatures. IBC values were computed from measurements of the backscattered radio-frequency ultrasound signals collected using a single-element transducer (38-MHz center frequency, 13–47 MHz bandwidth). The IBC increased linearly with increasing collagen concentration and decreasing polymerization temperature. Parametric 3D images of the IBC were generated to visualize and quantify regional variations in collagen microstructure throughout the volume of hydrogels fabricated in standard tissue culture plates. IBC parametric images of corresponding cell-embedded collagen gels showed cell accumulation within regions having elevated collagen IBC values. The capability of this ultrasound technique to noninvasively detect and quantify spatial differences in collagen microstructure offers a valuable tool to monitor the structural properties of collagen scaffolds during fabrication, to detect functional differences in collagen microstructure, and to guide fundamental research on the interactions of cells and collagen matrices. PMID:25517512

Noninvasive Quantitative Imaging of Collagen Microstructure in Three-Dimensional Hydrogels Using High-Frequency Ultrasound.

PubMed

Mercado, Karla P; Helguera, María; Hocking, Denise C; Dalecki, Diane

2015-07-01

Collagen I is widely used as a natural component of biomaterials for both tissue engineering and regenerative medicine applications. The physical and biological properties of fibrillar collagens are strongly tied to variations in collagen fiber microstructure. The goal of this study was to develop the use of high-frequency quantitative ultrasound to assess collagen microstructure within three-dimensional (3D) hydrogels noninvasively and nondestructively. The integrated backscatter coefficient (IBC) was employed as a quantitative ultrasound parameter to detect, image, and quantify spatial variations in collagen fiber density and diameter. Collagen fiber microstructure was varied by fabricating hydrogels with different collagen concentrations or polymerization temperatures. IBC values were computed from measurements of the backscattered radio-frequency ultrasound signals collected using a single-element transducer (38-MHz center frequency, 13-47 MHz bandwidth). The IBC increased linearly with increasing collagen concentration and decreasing polymerization temperature. Parametric 3D images of the IBC were generated to visualize and quantify regional variations in collagen microstructure throughout the volume of hydrogels fabricated in standard tissue culture plates. IBC parametric images of corresponding cell-embedded collagen gels showed cell accumulation within regions having elevated collagen IBC values. The capability of this ultrasound technique to noninvasively detect and quantify spatial differences in collagen microstructure offers a valuable tool to monitor the structural properties of collagen scaffolds during fabrication, to detect functional differences in collagen microstructure, and to guide fundamental research on the interactions of cells and collagen matrices.

The microstructure of capsule containing self-healing materials: A micro-computed tomography study

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

Van Stappen, Jeroen, E-mail: Jeroen.Vanstappen@uge

Autonomic self-healing materials are materials with built-in (micro-) capsules or vessels, which upon fracturing release healing agents in order to recover the material's physical and mechanical properties. In order to better understand and engineer these materials, a thorough characterization of the material's microstructural behavior is essential and often overlooked. In this context, micro-computed tomography (μCT) can be used to investigate the three dimensional distribution and (de)bonding of (micro-) capsules in their native state in a polymer system with self-healing properties. Furthermore, in-situ μCT experiments in a self-healing polymer and a self-healing concrete system can elucidate the breakage and leakage behaviormore » of (micro-) capsules at the micrometer scale. While challenges related to image resolution and contrast complicate the characterization in specific cases, non-destructive 3D imaging with μCT is shown to contribute to the understanding of the link between the microstructure and the self-healing behavior of these complex materials. - Highlights: • μCT imaging allows for the analysis of microcapsule distribution patterns in self-healing materials. • μCT allows for qualitative and quantitative measurements of healing agent release from carriers in self-healing materials. • Experimental set-ups can be optimized by changing chemical compounds in the system to ensure maximum quality imaging.« less

Role of Microstructure on the Performance of UHTCs

NASA Technical Reports Server (NTRS)

Johnson, Sylvia M.; Gasch, Matthew J.; Lawson, John W.; Gusman, Michael I.; Stackpoole, Mairead

2010-01-01

We have investigated a number of methods to control microstructure. We have routes to form: a) in situ "composites" b) Very fine microstructures. Arcjet testing and other characterization of monolithic materials. Control oxidation through microstructure and composition. Beginning to incorporate these materials as matrices for composites. Modeling effort to facilitate material design and characterization.

Characterization of European sword blades through neutron imaging techniques

NASA Astrophysics Data System (ADS)

Salvemini, F.; Grazzi, F.; Peetermans, S.; Gener, M.; Lehmann, E. H.; Zoppi, M.

2014-09-01

In the present work, we have studied two European rapier blades, dating back to the period ranging from the Late Renaissance to the Early Modern Age (about 17th to 18th century). In order to determine variation in quality and differences in technology, a study was undertaken with the purpose to observe variations in the blade microstructure (and consequently in the construction processes). The samples, which in the present case were expendable, have been investigated, preliminarily, through standard metallography and then by means of white beam and energy-selective neutron imaging. The comparison of the results, using the two techniques, turned out to be satisfactory, with a substantial quantitative agreement of the results obtained with the two techniques, and show the complementarity of the two methods. Metallography has been considered up to now the method of choice for metal material characterization. The correspondence between the two methods, as well as the non-invasive character of the neutron-based techniques and its possibility to obtain 3D reconstruction, candidate neutron imaging as an important and quantitatively reliable technique for metal characterization.

Micro-computed tomography characterization of tissue engineering scaffolds: effects of pixel size and rotation step.

PubMed

Cengiz, Ibrahim Fatih; Oliveira, Joaquim Miguel; Reis, Rui L

2017-08-01

Quantitative assessment of micro-structure of materials is of key importance in many fields including tissue engineering, biology, and dentistry. Micro-computed tomography (µ-CT) is an intensively used non-destructive technique. However, the acquisition parameters such as pixel size and rotation step may have significant effects on the obtained results. In this study, a set of tissue engineering scaffolds including examples of natural and synthetic polymers, and ceramics were analyzed. We comprehensively compared the quantitative results of µ-CT characterization using 15 acquisition scenarios that differ in the combination of the pixel size and rotation step. The results showed that the acquisition parameters could statistically significantly affect the quantified mean porosity, mean pore size, and mean wall thickness of the scaffolds. The effects are also practically important since the differences can be as high as 24% regarding the mean porosity in average, and 19.5 h and 166 GB regarding the characterization time and data storage per sample with a relatively small volume. This study showed in a quantitative manner the effects of such a wide range of acquisition scenarios on the final data, as well as the characterization time and data storage per sample. Herein, a clear picture of the effects of the pixel size and rotation step on the results is provided which can notably be useful to refine the practice of µ-CT characterization of scaffolds and economize the related resources.

Dielectric Characteristics of Microstructural Changes and Property Evolution in Engineered Materials

NASA Astrophysics Data System (ADS)

Clifford, Jallisa Janet

Heterogeneous materials are increasingly used in a wide range of applications such as aerospace, civil infrastructure, fuel cells and many others. The ability to take properties from two or more materials to create a material with properties engineered to needs is always very attractive. Hence heterogeneous materials are evolving into more complex formulations in multiple disciplines. Design of microstructure at multiple scales control the global functional properties of these materials and their structures. However, local microstructural changes do not directly cause a proportional change to the global properties (such as strength and stiffness). Instead, local changes follow an evolution process including significant interactions. Therefore, in order to understand property evolution of engineered materials, microstructural changes need to be effectively captured. Characterizing these changes and representing them by material variables will enable us to further improve our material level understanding. In this work, we will demonstrate how microstructural features of heterogeneous materials can be described quantitatively using broadband dielectric spectroscopy (BbDS). The frequency dependent dielectric properties can capture the change in material microstructure and represent these changes in terms of material variables, such as complex permittivity. These changes in terms of material properties can then be linked to a number of different conditions, such as increasing damage due to impact or fatigue. Two different broadband dielectric spectroscopy scanning modes are presented: bulk measurements and continuous scanning to measure dielectric property change as a function of position across the specimen. In this study, we will focus on ceramic materials and fiber reinforced polymer matrix composites as test bed material systems. In the first part of the thesis, we will present how different micro-structural design of porous ceramic materials can be captured quantitatively using BbDS. These materials are typically used in solid oxide fuel cells (SOFC). Results show significant effect of microstructural design on material properties at multiple temperatures (up to 800 °C). In the later part of the thesis, we will focus on microstructural changes of fiber reinforced composite materials due to impact and static loading. The changes in dielectric response can then be linked to the bulk mechanical properties of the material and various damage modes. Observing trends in dielectric response enables us to further determine local mechanisms and distribution of properties throughout the damaged specimens. A 3D X-ray microscope and a digital microscope have been used to visualize these changes in material microstructure and validate experimental observations. The increase in damage observed in the material microstructure can then also be linked to the changes in dielectric response. Results show that BbDS is an extremely useful tool for identifying microstructural changes within a heterogeneous material and particularly useful in relating remaining properties. Dielectric material variables can be used directly in property degradation laws and help develop a framework for future predictive modeling methodologies.

Mean apparent propagator (MAP) MRI: a novel diffusion imaging method for mapping tissue microstructure.

PubMed

Özarslan, Evren; Koay, Cheng Guan; Shepherd, Timothy M; Komlosh, Michal E; İrfanoğlu, M Okan; Pierpaoli, Carlo; Basser, Peter J

2013-09-01

Diffusion-weighted magnetic resonance (MR) signals reflect information about underlying tissue microstructure and cytoarchitecture. We propose a quantitative, efficient, and robust mathematical and physical framework for representing diffusion-weighted MR imaging (MRI) data obtained in "q-space," and the corresponding "mean apparent propagator (MAP)" describing molecular displacements in "r-space." We also define and map novel quantitative descriptors of diffusion that can be computed robustly using this MAP-MRI framework. We describe efficient analytical representation of the three-dimensional q-space MR signal in a series expansion of basis functions that accurately describes diffusion in many complex geometries. The lowest order term in this expansion contains a diffusion tensor that characterizes the Gaussian displacement distribution, equivalent to diffusion tensor MRI (DTI). Inclusion of higher order terms enables the reconstruction of the true average propagator whose projection onto the unit "displacement" sphere provides an orientational distribution function (ODF) that contains only the orientational dependence of the diffusion process. The representation characterizes novel features of diffusion anisotropy and the non-Gaussian character of the three-dimensional diffusion process. Other important measures this representation provides include the return-to-the-origin probability (RTOP), and its variants for diffusion in one- and two-dimensions-the return-to-the-plane probability (RTPP), and the return-to-the-axis probability (RTAP), respectively. These zero net displacement probabilities measure the mean compartment (pore) volume and cross-sectional area in distributions of isolated pores irrespective of the pore shape. MAP-MRI represents a new comprehensive framework to model the three-dimensional q-space signal and transform it into diffusion propagators. Experiments on an excised marmoset brain specimen demonstrate that MAP-MRI provides several novel, quantifiable parameters that capture previously obscured intrinsic features of nervous tissue microstructure. This should prove helpful for investigating the functional organization of normal and pathologic nervous tissue. Copyright © 2013 Elsevier Inc. All rights reserved.

Role of Dynamic Nucleation at Moving Boundaries in Phase and Microstructure Selection

NASA Technical Reports Server (NTRS)

Karma, Alain; Trivedi, Rohit

1999-01-01

Solidification microstructures that form under steady-state growth conditions (cells, dendrites, regular eutectics, etc.) are reasonably well understood in comparison to other, more complex microstructures, which form under intrinsically non-steady-state growth conditions due to the competition between the nucleation and growth of several phases. Some important practical examples in this latter class include microstructures forming in peritectic systems in highly undercooled droplets, and in strip cast stainless steels. Prediction of phase and microstructure selection in these systems has been traditionally based on (1) heterogeneous nucleation on a static interface, and (2) comparing the relative growth rate of different phase/microstructures under steady-state growth conditions. The formation of new phases, however, occurs via nucleation on, or ahead of, a moving boundary. In addition, the actual selection process is controlled by a complex interaction between the nucleation process and the growth competition between the nuclei and the pre-existing phase under non-steady-state conditions. As a result, it is often difficult to predict which microstructure will form and which phases will be selected under prescribed processing conditions. This research addresses this critical role of nucleation at moving boundaries in the selection of phases and solidification microstructures through quantitative experiments and numerical modeling in peritectic systems. In order to create a well characterized system in which to study this problem, we focus on the directional solidification of hypo- and hyper-peritectic alloys in the two-phase region, imposing a large enough ratio of temperature gradient/growth rate (G/V(sub p)) to suppress the morphological instability of both the parent (alpha) and peritectic (Beta) phases, i.e. each phase alone would grow as a planar front. Our combined experimental and theoretical results show that, already in this simplified case, the growth competition of these two phases leads to a rich variety of microstructures that depend sensitively upon the relative importance of nucleation, diffusion, and convection.

Non-Linear Association between Cerebral Amyloid Deposition and White Matter Microstructure in Cognitively Healthy Older Adults.

PubMed

Wolf, Dominik; Fischer, Florian U; Scheurich, Armin; Fellgiebel, Andreas

2015-01-01

Cerebral amyloid-β accumulation and changes in white matter (WM) microstructure are imaging characteristics in clinical Alzheimer's disease and have also been reported in cognitively healthy older adults. However, the relationship between amyloid deposition and WM microstructure is not well understood. Here, we investigated the impact of quantitative cerebral amyloid load on WM microstructure in a group of cognitively healthy older adults. AV45-positron emission tomography and diffusion tensor imaging (DTI) scans of forty-four participants (age-range: 60 to 89 years) from the Alzheimer's Disease Neuroimaging Initiative were analyzed. Fractional anisotropy (FA), mean diffusivity (MD), radial diffusivity (DR), and axial diffusivity (DA) were calculated to characterize WM microstructure. Regression analyses demonstrated non-linear (quadratic) relationships between amyloid deposition and FA, MD, as well as RD in widespread WM regions. At low amyloid burden, higher deposition was associated with increased FA as well as decreased MD and DR. At higher amyloid burden, higher deposition was associated with decreased FA as well as increased MD and DR. Additional regression analyses demonstrated an interaction effect between amyloid load and global WM FA, MD, DR, and DA on cognition, suggesting that cognition is only affected when amyloid is increasing and WM integrity is decreasing. Thus, increases in FA and decreases in MD and RD with increasing amyloid load at low levels of amyloid burden may indicate compensatory processes that preserve cognitive functioning. Potential mechanisms underlying the observed non-linear association between amyloid deposition and DTI metrics of WM microstructure are discussed.

Identification of ginseng root using quantitative X-ray microtomography.

PubMed

Ye, Linlin; Xue, Yanling; Wang, Yudan; Qi, Juncheng; Xiao, Tiqiao

2017-07-01

The use of X-ray phase-contrast microtomography for the investigation of Chinese medicinal materials is advantageous for its nondestructive, in situ , and three-dimensional quantitative imaging properties. The X-ray phase-contrast microtomography quantitative imaging method was used to investigate the microstructure of ginseng, and the phase-retrieval method is also employed to process the experimental data. Four different ginseng samples were collected and investigated; these were classified according to their species, production area, and sample growth pattern. The quantitative internal characteristic microstructures of ginseng were extracted successfully. The size and position distributions of the calcium oxalate cluster crystals (COCCs), important secondary metabolites that accumulate in ginseng, are revealed by the three-dimensional quantitative imaging method. The volume and amount of the COCCs in different species of the ginseng are obtained by a quantitative analysis of the three-dimensional microstructures, which shows obvious difference among the four species of ginseng. This study is the first to provide evidence of the distribution characteristics of COCCs to identify four types of ginseng, with regard to species authentication and age identification, by X-ray phase-contrast microtomography quantitative imaging. This method is also expected to reveal important relationships between COCCs and the occurrence of the effective medicinal components of ginseng.

Classification of micro-CT images using 3D characterization of bone canal patterns in human osteogenesis imperfecta

NASA Astrophysics Data System (ADS)

Abidin, Anas Z.; Jameson, John; Molthen, Robert; Wismüller, Axel

2017-03-01

Few studies have analyzed the microstructural properties of bone in cases of Osteogenenis Imperfecta (OI), or `brittle bone disease'. Current approaches mainly focus on bone mineral density measurements as an indirect indicator of bone strength and quality. It has been shown that bone strength would depend not only on composition but also structural organization. This study aims to characterize 3D structure of the cortical bone in high-resolution micro CT images. A total of 40 bone fragments from 28 subjects (13 with OI and 15 healthy controls) were imaged using micro tomography using a synchrotron light source (SRµCT). Minkowski functionals - volume, surface, curvature, and Euler characteristics - describing the topological organization of the bone were computed from the images. The features were used in a machine learning task to classify between healthy and OI bone. The best classification performance (mean AUC - 0.96) was achieved with a combined 4-dimensional feature of all Minkowski functionals. Individually, the best feature performance was seen using curvature (mean AUC - 0.85), which characterizes the edges within a binary object. These results show that quantitative analysis of cortical bone microstructure, in a computer-aided diagnostics framework, can be used to distinguish between healthy and OI bone with high accuracy.

Three-dimensional microstructural characterization of bulk plutonium and uranium metals using focused ion beam technique

NASA Astrophysics Data System (ADS)

Chung, Brandon W.; Erler, Robert G.; Teslich, Nick E.

2016-05-01

Nuclear forensics requires accurate quantification of discriminating microstructural characteristics of the bulk nuclear material to identify its process history and provenance. Conventional metallographic preparation techniques for bulk plutonium (Pu) and uranium (U) metals are limited to providing information in two-dimension (2D) and do not allow for obtaining depth profile of the material. In this contribution, use of dual-beam focused ion-beam/scanning electron microscopy (FIB-SEM) to investigate the internal microstructure of bulk Pu and U metals is demonstrated. Our results demonstrate that the dual-beam methodology optimally elucidate microstructural features without preparation artifacts, and the three-dimensional (3D) characterization of inner microstructures can reveal salient microstructural features that cannot be observed from conventional metallographic techniques. Examples are shown to demonstrate the benefit of FIB-SEM in improving microstructural characterization of microscopic inclusions, particularly with respect to nuclear forensics.

Three-dimensional microstructural characterization of bulk plutonium and uranium metals using focused ion beam technique

DOE PAGES

Chung, Brandon W.; Erler, Robert G.; Teslich, Nick E.

2016-03-03

Nuclear forensics requires accurate quantification of discriminating microstructural characteristics of the bulk nuclear material to identify its process history and provenance. Conventional metallographic preparation techniques for bulk plutonium (Pu) and uranium (U) metals are limited to providing information in two-dimension (2D) and do not allow for obtaining depth profile of the material. In this contribution, use of dual-beam focused ion-beam/scanning electron microscopy (FIB-SEM) to investigate the internal microstructure of bulk Pu and U metals is demonstrated. Our results demonstrate that the dual-beam methodology optimally elucidate microstructural features without preparation artifacts, and the three-dimensional (3D) characterization of inner microstructures can revealmore » salient microstructural features that cannot be observed from conventional metallographic techniques. As a result, examples are shown to demonstrate the benefit of FIB-SEM in improving microstructural characterization of microscopic inclusions, particularly with respect to nuclear forensics.« less

Predictive characterization of aging and degradation of reactor materials in extreme environments. Final report, December 20, 2013 - September 20, 2017

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

Qu, Jianmin

Understanding of reactor material behavior in extreme environments is vital not only to the development of new materials for the next generation nuclear reactors, but also to the extension of the operating lifetimes of the current fleet of nuclear reactors. To this end, this project conducted a suite of unique experimental techniques, augmented by a mesoscale computational framework, to understand and predict the long-term effects of irradiation, temperature, and stress on material microstructures and their macroscopic behavior. The experimental techniques and computational tools were demonstrated on two distinctive types of reactor materials, namely, Zr alloys and high-Cr martensitic steels. Thesemore » materials are chosen as the test beds because they are the archetypes of high-performance reactor materials (cladding, wrappers, ducts, pressure vessel, piping, etc.). To fill the knowledge gaps, and to meet the technology needs, a suite of innovative in situ transmission electron microscopy (TEM) characterization techniques (heating, heavy ion irradiation, He implantation, quantitative small-scale mechanical testing, and various combinations thereof) were developed and used to elucidate and map the fundamental mechanisms of microstructure evolution in both Zr and Cr alloys for a wide range environmental boundary conditions in the thermal-mechanical-irradiation input space. Knowledge gained from the experimental observations of the active mechanisms and the role of local microstructural defects on the response of the material has been incorporated into a mathematically rigorous and comprehensive three-dimensional mesoscale framework capable of accounting for the compositional variation, microstructural evolution and localized deformation (radiation damage) to predict aging and degradation of key reactor materials operating in extreme environments. Predictions from this mesoscale framework were compared with the in situ TEM observations to validate the model.« less

A combined microstructural and petrophysical study to analyse the mechanical behaviour of shales in the Flysch units, Glarus Alps, Switzerland

NASA Astrophysics Data System (ADS)

Akker, Vénice; Kaufmann, Josef; Berger, Alfons; Herwegh, Marco

2017-04-01

Crustal scale deformation is strongly controlled by the rheological behaviour of sheet-silicate-rich rock types. As these rocks have low rock strength, facilitated by the strong crystallographically controlled mechanical anisotropy and interstitial pore fluid in the aggregate, they are able to accommodate considerable amounts of strain. A close relationship is expected between microstructure, porosity and permeability as function of metamorphic conditions and strain gradients. Thereby, fluids set free by compaction, mineral reactions or deformation play an important role. Rising industries in underground storage such as nuclear waste disposal, shale gas exploration or geological carbon sequestration make use of the advantageous properties of such rock types. Therefore, there is a great demand for research on the interaction of these processes. This study uses samples from Flysch-units of the Glarus Alps (Switzerland) collected along a metamorphic gradient (150-400°C) to unravel the link between the mechanical behaviour of these sheet-silicate-rich rocks at geological conditions and their present-day physical parameters. Investigations include two topics: (1) characterization of such rock types in terms of mineralogy, microstructure and petrophysical properties; and (2) possible reconstruction of deformation processes from microstructures. Quantitative information on the porosity, i.e. the pore sizes, distribution and their interconnectivity is crucial for both topics. Porosity is therefore estimated by: (1) image analysis of high resolution SEM images, (2) He-pycnometry, and (3) Hg-porosimetry. In a first step, differences in their present day physical parameters between low and high temperature sampling sites are shown. The variations inside and between the investigated samples is partly due to initial sedimentological heterogeneity and partly to the changes along the metamorphic gradient. This study will demonstrate how the characterized present day porosity evolved owing to these two prerequisites.

Microstructure-Sensitive Investigation of Fracture Using Acoustic Emission Coupled With Electron Microscopy

NASA Technical Reports Server (NTRS)

Wisner, Brian; Cabal, Mike; Vanniamparambiland, Prashanth A.; Leser, William; Hochhalter, Jacob; Kontsos, Antonios

2015-01-01

A novel technique using Scanning Electron Microscopy (SEM) in conjunction with Acoustic Emission (AE) monitoring is proposed to investigate microstructure-sensitive fatigue and fracture of metals. The coupling between quasi in situ microscopy with actual in situ nondestructive evaluation falls into the ICME framework and the idea of quantitative data-driven characterization of material behavior. To validate the use of AE monitoring inside the SEM chamber, Aluminum 2024-B sharp notch specimen were tested both inside and outside the microscope using a small scale mechanical testing device. Subsequently, the same type of specimen was tested inside the SEM chamber. Load data were correlated with both AE information and observations of microcracks around grain boundaries as well as secondary cracks, voids, and slip bands. The preliminary results are in excellent agreement with similar findings at the mesoscale. Extensions of the application of this novel technique are discussed.

The influence of copper precipitation and plastic deformation hardening on the impact-transition temperature of rolled structural steels

NASA Astrophysics Data System (ADS)

Aróztegui, Juan J.; Urcola, José J.; Fuentes, Manuel

1989-09-01

Commercial electric arc melted low-carbon steels, provided as I beams, were characterized both microstructurally and mechanically in the as-rolled, copper precipitation, and plastically pre-deformed conditions. Inclusion size distribution, ferrite grain size, pearlite volume fraction, precipitated volume fraction of copper, and size distribution of these precipitates were deter-mined by conventional quantitative optical and electron metallographic techniques. From the tensile tests conducted at a strain rate of 10-3 s-1 and impact Charpy V-notched tests carried out, stress/strain curves, yield stress, and impact-transition temperature were obtained. The spe-cific fractographic features of the fracture surfaces also were quantitatively characterized. The increases in yield stress and transition temperature experienced upon either aging or work hard-ening were related through empirical relationships. These dependences were analyzed semi-quantitatively by combining microscopic and macroscopic fracture criteria based on measured fundamental properties (fracture stress and yield stress) and observed fractographic parameters (crack nucleation distance and nuclei size). The rationale developed from these fracture criteria allows the semiquantitative prediction of the temperature transition shifts produced upon aging and work hardening. The values obtained are of the right order of magnitude.

Intrinsic property measurement of surfactant-templated mesoporous silica films using time-resolved single-molecule imaging.

PubMed

Kennard, Raymond; DeSisto, William J; Giririjan, Thanu Praba; Mason, Michael D

2008-04-07

Mesoporous silica membranes fabricated by the surfactant-templated sol-gel process have received attention because of the potential to prepare membranes with a narrow pore size distribution and ordering of the interconnected pores. Potential applications include ultrafiltration, biological separations and drug delivery, and separators in lithium-ion batteries. Despite advancements in synthesis and characterization of these membranes, a quantitative description of the membrane microstructure remains a challenge. Currently the membrane microstructure is characterized by the combination of results from several techniques, i.e., gas permeance testing, x-ray diffraction scanning electron microscopy, transmission electron microscopy, and permporometry. The results from these ensemble methods are then compiled and the data fitted to a particular flow model. Although these methods are very effective in determining membrane performance, general pore size distribution, and defect concentration, they are unable to monitor molecular paths through the membrane and quantitatively measure molecular interactions between the molecular specie and pore network. Single-molecule imaging techniques enable optical measurements that probe materials on nanometer length scales through observation of individual molecules without the influence of averaging. Using single-molecule imaging spectroscopy, we can quantitatively characterize the interaction between the probe molecule and the interior of the pore within mesoporous silica membranes. This approach is radically different from typical membrane characterization methods in that it has the potential to spatially sample the underlying pore structure distribution, the surface energy, and the transport properties. Our hope is that this new fundamental knowledge can be quantitatively linked to both the preparation and the performance of membranes, leading to the advancement of membrane science and technology. Fluorescent molecules, 1,1-dioctadecyl-3,3,3,3-tetramethylindo-carbocyanine perchlorate, used to interrogate the available free volume in their vicinity, were loaded into the mesoporous silica membranes at subnanomolar concentrations. The mesoporous silica films were prepared using a nonionic ethylene oxide-propylene oxide-ethylene oxide triblock copolymer surfactant, Pluronic P123, on single crystal silicon substrates using dip coating of a silica sol. Membranes were prepared resulting in an average pore diameter of approximately 5 nm as measured by helium, nitrogen permeance, and porosimetry. Fluorescent images and time transient experiments were recorded using a custom built single-molecule scanning confocal microscope at differing temperatures (10, 20, 30, 40, and 50 degrees C). Time-dependent polarization anisotropy was used to obtain the enthalpy of adsorption and Henry's law constant of the probe molecule.

Intrinsic property measurement of surfactant-templated mesoporous silica films using time-resolved single-molecule imaging

NASA Astrophysics Data System (ADS)

Kennard, Raymond; DeSisto, William J.; Giririjan, Thanu Praba; Mason, Michael D.

2008-04-01

Mesoporous silica membranes fabricated by the surfactant-templated sol-gel process have received attention because of the potential to prepare membranes with a narrow pore size distribution and ordering of the interconnected pores. Potential applications include ultrafiltration, biological separations and drug delivery, and separators in lithium-ion batteries. Despite advancements in synthesis and characterization of these membranes, a quantitative description of the membrane microstructure remains a challenge. Currently the membrane microstructure is characterized by the combination of results from several techniques, i.e., gas permeance testing, x-ray diffraction scanning electron microscopy, transmission electron microscopy, and permporometry. The results from these ensemble methods are then compiled and the data fitted to a particular flow model. Although these methods are very effective in determining membrane performance, general pore size distribution, and defect concentration, they are unable to monitor molecular paths through the membrane and quantitatively measure molecular interactions between the molecular specie and pore network. Single-molecule imaging techniques enable optical measurements that probe materials on nanometer length scales through observation of individual molecules without the influence of averaging. Using single-molecule imaging spectroscopy, we can quantitatively characterize the interaction between the probe molecule and the interior of the pore within mesoporous silica membranes. This approach is radically different from typical membrane characterization methods in that it has the potential to spatially sample the underlying pore structure distribution, the surface energy, and the transport properties. Our hope is that this new fundamental knowledge can be quantitatively linked to both the preparation and the performance of membranes, leading to the advancement of membrane science and technology. Fluorescent molecules, 1,1-dioctadecyl-3,3,3,3-tetramethylindo-carbocyanine perchlorate, used to interrogate the available free volume in their vicinity, were loaded into the mesoporous silica membranes at subnanomolar concentrations. The mesoporous silica films were prepared using a nonionic ethylene oxide-propylene oxide-ethylene oxide triblock copolymer surfactant, Pluronic P123, on single crystal silicon substrates using dip coating of a silica sol. Membranes were prepared resulting in an average pore diameter of approximately 5nm as measured by helium, nitrogen permeance, and porosimetry. Fluorescent images and time transient experiments were recorded using a custom built single-molecule scanning confocal microscope at differing temperatures (10, 20, 30, 40, and 50°C). Time-dependent polarization anisotropy was used to obtain the enthalpy of adsorption and Henry's law constant of the probe molecule.

Characterization of glass-infiltrated alumina-based ceramics

PubMed Central

Bona, Alvaro Della; Mecholsky, John J; Barrett, Allyson A; Griggs, Jason A

2010-01-01

Objective characterize the microstructure, composition, and important properties of glass-infiltrated alumina-based ceramics similar to the In-Ceram system. Methods Materials used were: IA- In-Ceram Alumina (Vita); IAE- IA electrophoretically deposited (Vita); AEM- IA using a vacuum driven method (Vita); VC- Vitro-Ceram (Angelus); TC- Turkom-Cera (Turkom-Ceramic); CC- Ceramcap (Foto-Ceram); and AG- Alglass (EDG). Ceramic specimens were fabricated following manufacturers’ instructions and ISO6872 standard and polished successively through 1μm alumina abrasive. Semi-quantitative and qualitative analyses were performed using scanning electron microscopy (SEM), energy dispersive spectroscopy (EDS), and stereology (Vv). The elastic modulus (E) and Poisson’s ratio (ν) were determined using time-of-flight data measured in an ultrasonic pulser/receiver and the density (ρ) was determined using a helium pycnometer. Vicker’s indentation was used to calculate hardness (H). Bar specimens (25×4×1.2mm3) were loaded in three-point bending to fracture using a universal testing machine with cross-head speed of 1mm/min. Flexural strength (σ3P) was calculated and statistically analyzed using ANOVA, Tukey (α=0.05) and Weibull (m= modulus, σ0= characteristic strength). Results SEM and EDS analyses revealed similar microstructure for all ceramics, except for a lead-based matrix in CC and a zirconia phase in VC. TC, AG and CC showed significantly lower mean σ3P values than the other ceramics (p 0.05). AEM showed the greatest m (16). Conclusion Despite few differences in microstructure and composition, the IA, IAE, AEM and VC ceramics have similar properties. Significance The glass-infiltrated alumina-based ceramics from different manufacturers presented distinct characteristics. It is necessary to characterize new commercially available materials to understand their properties. PMID:18692231

Power of Ultra Performance Liquid Chromatography/Electrospray Ionization-MS Reconstructed Ion Chromatograms in the Characterization of Small Differences in Polymer Microstructure.

PubMed

Epping, Ruben; Panne, Ulrich; Falkenhagen, Jana

2018-03-06

From simple homopolymers to functionalized, 3-dimensional structured copolymers, the complexity of polymeric materials has become more and more sophisticated. With new applications, for instance, in the semiconductor or pharmaceutical industry, the requirements for the characterization have risen with the complexity of the used polymers. For each additional distribution, an additional dimension in analysis is needed. Small, often isomeric heterogeneities in topology or microstructure can usually not be simply separated chromatographically or distinguished by any common detector but affect the properties of materials significantly. For a drug delivery system, for example, the degree of branching and branching distribution is crucial for the formation of micelles. Instead of a complicated, time-consuming, and/or expensive 2D-chromatography or ion mobility spectrometry (IMS) method, that also has its limitations, in this work, a simple approach using size exclusion chromatography (SEC) coupled with electrospray ionization (ESI) mass spectrometry is proposed. The online coupling allows the analysis of reconstructed ion chromatograms (RICs) of each degree of polymerization. While a complete separation often cannot be achieved, the derived retention times and peak widths lead to information on the existence and dispersity of heterogeneities. Although some microstructural heterogeneities like short chain branching can for large polymers be characterized with methods such as light scattering, for oligomers where the heterogeneities just start to form and their influence is at the maximum, they are inaccessible with these methods. It is also shown that with a proper calibration even quantitative information can be obtained. This method is suitable to detect small differences in, e.g., branching, 3D-structure, monomer sequence, or tacticity and could potentially be used in routine analysis to quickly determine deviations.

Containerless processing of undercooled melts

NASA Technical Reports Server (NTRS)

Perepezko, J. H.

1993-01-01

The investigation focused on the control of microstructural evolution in Mn-Al, Fe-Ni, Ni-V, and Au-Pb-Sb alloys through the high undercooling levels provided by containerless processing, and provided fundamental new information on the control of nucleation. Solidification analysis was conducted by means of thermal analysis, x-ray diffraction, and metallographic characterization on samples processed in a laboratory scale drop tube system. The Mn-Al alloy system offers a useful model system with the capability of phase separation on an individual particle basis, thus permitting a more complete understanding of the operative kinetics and the key containerless processing variables. This system provided the opportunity of analyzing the nucleation rate as a function of processing conditions and allowed for the quantitative assessment of the relevant processing parameters. These factors are essential in the development of a containerless processing model which has a predictive capability. Similarly, Ni-V is a model system that was used to study duplex partitionless solidification, which is a structure possible only in high under cooling solidification processes. Nucleation kinetics for the competing bcc and fcc phases were studied to determine how this structure can develop and the conditions under which it may occur. The Fe-Ni alloy system was studied to identify microstructural transitions with controlled variations in sample size and composition during containerless solidification. This work was forwarded to develop a microstructure map which delineates regimes of structural evolution and provides a unified analysis of experimental observations. The Au-Pb-Sb system was investigated to characterize the thermodynamic properties of the undercooled liquid phase and to characterize the glass transition under a variety of processing conditions. By analyzing key containerless processing parameters in a ground based drop tube study, a carefully designed flight experiment may be planned to utilize the extended duration microgravity conditions of orbiting spacecraft.

Transient rheology of stimuli responsive hydrogels: Integrating microrheology and microfluidics

NASA Astrophysics Data System (ADS)

Sato, Jun

Stimuli-responsive hydrogels have diverse potential applications in the field of drug delivery, tissue engineering, agriculture, cosmetics, gene therapy, and as sensors and actuators due to their unique responsiveness to external signals, such as pH, temperature, and ionic strength. Understanding the responsiveness of hydrogel structure and rheology to these stimuli is essential for designing materials with desirable performance. However, no instrumentation and well-defined methodology are available to characterize the structural and rheological responses to rapid solvent changes. In this thesis, a new microrheology set-up is described, which allows us to quantitatively measure the transient rheological properties and microstructure of a variety of solvent-responsive complex fluids. The device was constructed by integrating particle tracking microrheology and microfluidics and offers unique experimental capabilities for performing solvent-reponse measurements on soft fragile materials without applying external shear forces. Transient analysis methods to quantitatively obtain rheological properties were also constructed, and guidelines for the trade-off between statistical validity and temporal resolution were developed to accurately capture physical transitions. Employing the new device and methodology, we successfully quantified the transient rheological and microstructural responses during gel formation and break-up, and viscosity changes of solvent-responsive complex fluids. The analysis method was expanded for heterogeneous samples, incorporating methods to quantify the microrheology of samples with broad distributions of individual particle dynamics. Transient microrheology measurements of fragile, heterogeneous, self-assembled block copolypeptide hydrogels revealed that solvent exchange via convective mixing and dialysis can lead to significantly different gel properties and that commonly applied sample preparation protocols for the characterization of soft biomaterials could lead to erroneous conclusions about microstructural dynamics. Systematic investigations by varying key parameters, like molecular structure, gel concentration, salt concentration, and tracer particle size for microrheology, revealed that subtle variations in molecular architecture can cause major changes in response dynamics. Moreover, the results showed that the method can be applied for studying gel formation and breakup kinetics. The research in this thesis facilitates the design of solvent-responsive soft materials with appropriate microstructural dynamics for in vivo applications like tissue engineering and drug delivery, and can also be applied to study the effect of solvents on self-assembly mechanisms in other responsive soft materials, such as polymer solutions and colloidal dispersions.

Detecting the Extent of Cellular Decomposition after Sub-Eutectoid Annealing in Rolled UMo Foils

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

Kautz, Elizabeth J.; Jana, Saumyadeep; Devaraj, Arun

2017-07-31

This report presents an automated image processing approach to quantifying microstructure image data, specifically the extent of eutectoid (cellular) decomposition in rolled U-10Mo foils. An image processing approach is used here to be able to quantitatively describe microstructure image data in order to relate microstructure to processing parameters (time, temperature, deformation).

Associations Between White Matter Microstructure and Infants’ Working Memory

PubMed Central

Short, Sarah J.; Elison, Jed T.; Goldman, Barbara Davis; Styner, Martin; Gu, Hongbin; Connelly, Mark; Maltbie, Eric; Woolson, Sandra; Lin, Weili; Gerig, Guido; Reznick, J. Steven; Gilmore, John H.

2013-01-01

Working memory emerges in infancy and plays a privileged role in subsequent adaptive cognitive development. The neural networks important for the development of working memory during infancy remain unknown. We used diffusion tensor imaging (DTI) and deterministic fiber tracking to characterize the microstructure of white matter fiber bundles hypothesized to support working memory in 12-month-old infants (n=73). Here we show robust associations between infants’ visuospatial working memory performance and microstructural characteristics of widespread white matter. Significant associations were found for white matter tracts that connect brain regions known to support working memory in older children and adults (genu, anterior and superior thalamic radiations, anterior cingulum, arcuate fasciculus, and the temporal-parietal segment). Better working memory scores were associated with higher FA and lower RD values in these selected white matter tracts. These tract-specific brain-behavior relationships accounted for a significant amount of individual variation above and beyond infants’ gestational age and developmental level, as measured with the Mullen Scales of Early Learning. Working memory was not associated with global measures of brain volume, as expected, and few associations were found between working memory and control white matter tracts. To our knowledge, this study is among the first demonstrations of brain-behavior associations in infants using quantitative tractography. The ability to characterize subtle individual differences in infant brain development associated with complex cognitive functions holds promise for improving our understanding of normative development, biomarkers of risk, experience-dependent learning and neuro-cognitive periods of developmental plasticity. PMID:22989623

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

Pierce, D. T.; Coughlin, D. R.; Williamson, D. L.

Quenching and partitioning (Q&P) produces steel microstructures with martensite and austenite that exhibit promising property combinations for third generation advanced high strength steels. Understanding the kinetics of reactions that compete for available carbon, such as carbide formation, is critical for alloying and processing design and achieving austenite enrichment and retention during Q&P. Mössbauer effect spectroscopy (MES) was used to characterize Q&P microstructures in a 0.38C-1.54Mn-1.48Si wt.% steel after quenching to 225 °C and partitioning at 400 °C for 10 or 300 s, with an emphasis on transition carbides. The recoilless fraction for η-carbide was calculated and a correction for saturationmore » of the MES absorption spectrum was applied, making quantitative measurements of small amounts of η-carbide, including non-stoichiometric η-carbide, possible in Q&P microstructures. Complementary transmission electron microscopy confirmed the presence of η-carbides, and MES and X-ray diffraction were used to characterize the austenite. The amount of η-carbide formed during Q&P ranged from 1.4 to 2.4 at.%, accounting for a substantial portion (~24% to 41%) of the bulk carbon content of the steel. The amount (5.0 at.%) of η-carbide that formed after quenching and tempering (Q&T) at 400 °C for 300 s was significantly greater than after partitioning at 400 °C for 300 s (2.4 at.%), suggesting that carbon partitioning from martensite to austenite occurs in conjunction with η-carbide formation during Q&P in these specimens.« less

Modeling and characterization of as-welded microstructure of solid solution strengthened Ni-Cr-Fe alloys resistant to ductility-dip cracking Part II: Microstructure characterization

NASA Astrophysics Data System (ADS)

Unfried-Silgado, Jimy; Ramirez, Antonio J.

2014-03-01

In part II of this work is evaluated the as-welded microstructure of Ni-Cr-Fe alloys, which were selected and modeled in part I. Detailed characterization of primary and secondary precipitates, subgrain and grain structures, partitioning, and grain boundary morphology were developed. Microstructural characterization was carried out using optical microscopy, SEM, TEM, EBSD, and XEDS techniques. These results were analyzed and compared to modeling results displaying a good agreement. The Hf additions produced the highest waviness of grain boundaries, which were related to distribution of Hf-rich carbonitrides. Experimental evidences about Mo distribution into crystal lattice have provided information about its possible role in ductility-dip cracking (DDC). Characterization results of studied alloys were analyzed and linked to their DDC resistance data aiming to establish relationships between as-welded microstructure and hot deformation performance. Wavy grain boundaries, primary carbides distribution, and strengthened crystal lattice are metallurgical characteristics related to high DDC resistance.

Nondestructive techniques for characterizing mechanical properties of structural materials: An overview

NASA Technical Reports Server (NTRS)

Vary, A.; Klima, S. J.

1985-01-01

An overview of nondestructive evaluation (NDE) is presented to indicate the availability and application potentials of techniques for quantitative characterization of the mechanical properties of structural materials. The purpose is to review NDE techniques that go beyond the usual emphasis on flaw detection and characterization. Discussed are current and emerging NDE techniques that can verify and monitor entrinsic properties (e.g., tensile, shear, and yield strengths; fracture toughness, hardness, ductility; elastic moduli) and underlying microstructural and morphological factors. Most of the techniques described are, at present, neither widely applied nor widely accepted in commerce and industry because they are still emerging from the laboratory. The limitations of the techniques may be overcome by advances in applications research and instrumentation technology and perhaps by accommodations for their use in the design of structural parts.

Thermomechanical Testing and Microstructural Development of Class L Steel Wheel Alloy

DOT National Transportation Integrated Search

1994-03-01

Macrostructure, microstructure, and quantitative metallographic analysis is conducted on Association of American Railroads Class L wheel steel specimens tested in a Gleeble 1500 under combined mechanical compression and resistance heating to temperat...

Processing and mechanical properties of metal-ceramic composites with controlled microstructure formed by reactive metal penetration

NASA Astrophysics Data System (ADS)

Ellerby, Donald Thomas

1999-12-01

Compared to monolithic ceramics, metal-reinforced ceramic composites offer the potential for improved toughness and reliability in ceramic materials. As such, there is significant scientific and commercial interest in the microstructure and properties of metal-ceramic composites. Considerable work has been conducted on modeling the toughening behavior of metal reinforcements in ceramics; however, there has been limited application and testing of these concepts on real systems. Composites formed by newly developed reactive processes now offer the flexibility to systematically control metal-ceramic composite microstructure, and to test some of the property models that have been proposed for these materials. In this work, the effects of metal-ceramic composite microstructure on resistance curve (R-curve) behavior, strength, and reliability were systematically investigated. Al/Al2O3 composites were formed by reactive metal penetration (RMP) of aluminum metal into aluminosilicate ceramic preforms. Processing techniques were developed to control the metal content, metal composition, and metal ligament size in the resultant composite microstructure. Quantitative stereology and microscopy were used to characterize the composite microstructures, and then the influence of microstructure on strength, toughness, R-curve behavior, and reliability, was investigated. To identify the strength limiting flaws in the composite microstructure, fractography was used to determine the failure origins. Additionally, the crack bridging tractions produced by the metal ligaments in metal-ceramic composites formed by the RMP process were modeled. Due to relatively large flaws and low bridging stresses in RMP composites, no dependence of reliability on R-curve behavior was observed. The inherent flaws formed during reactive processing appear to limit the strength and reliability of composites formed by the RMP process. This investigation has established a clear relationship between processing, microstructure, and properties in metal-ceramic composites formed by the RMP process. RMP composite properties are determined by the metal-ceramic composite microstructure (e.g., metal content and ligament size), which can be systematically varied by processing. Furthermore, relative to the ceramic preforms used to make the composites, metal-ceramic composites formed by RMP generally have improved properties and combinations of properties that make them more desirable for advanced engineering applications.

Antisite defects in layered multiferroic CuCr0.9In0.1P2S6

NASA Astrophysics Data System (ADS)

He, Qian; Belianinov, Alex; Dziaugys, Andrius; Maksymovych, Petro; Vysochanskii, Yulian; Kalinin, Sergei V.; Borisevich, Albina Y.

2015-11-01

The CuCr1-xInxP2S6 system represents a large family of metal chalcogenophosphates that are unique and promising candidates for 2D materials with functionalities such as ferroelectricity. In this work, we carried out detailed microstructural and chemical characterization of these compounds using aberration-corrected STEM, in order to understand the origin of these different ordering phenomena. Quantitative STEM-HAADF imaging and analysis identified the stacking order of an 8-layer thin flake, which leads to the identification of anti-site In3+(Cu+) doping. We believe that these findings will pave the way towards understanding the ferroic coupling phenomena in van der Waals lamellar compounds, as well as their potential applications in 2-D electronics.The CuCr1-xInxP2S6 system represents a large family of metal chalcogenophosphates that are unique and promising candidates for 2D materials with functionalities such as ferroelectricity. In this work, we carried out detailed microstructural and chemical characterization of these compounds using aberration-corrected STEM, in order to understand the origin of these different ordering phenomena. Quantitative STEM-HAADF imaging and analysis identified the stacking order of an 8-layer thin flake, which leads to the identification of anti-site In3+(Cu+) doping. We believe that these findings will pave the way towards understanding the ferroic coupling phenomena in van der Waals lamellar compounds, as well as their potential applications in 2-D electronics. Electronic supplementary information (ESI) available. See DOI: 10.1039/c5nr04779j

Advanced single crystal for SSME turbopumps

NASA Technical Reports Server (NTRS)

Fritzemeier, L. G.

1989-01-01

The objective of this program was to evaluate the influence of high thermal gradient casting, hot isostatic pressing (HIP) and alternate heat treatments on the microstructure and mechanical properties of a single crystal nickel base superalloy. The alloy chosen for the study was PWA 1480, a well characterized, commercial alloy which had previously been chosen as a candidate for the Space Shuttle Main Engine high pressure turbopump turbine blades. Microstructural characterization evaluated the influence of casting thermal gradient on dendrite arm spacing, casting porosity distribution and alloy homogeneity. Hot isostatic pressing was evaluated as a means of eliminating porosity as a preferred fatigue crack initiation site. The alternate heat treatment was chosen to improve hydrogen environment embrittlement resistance and for potential fatigue life improvement. Mechanical property evaluation was aimed primarily at determining improvements in low cycle and high cycle fatigue life due to the advanced processing methods. Statistically significant numbers of tests were conducted to quantitatively demonstrate life differences. High thermal gradient casting improves as-cast homogeneity, which facilitates solution heat treatment of PWA 1480 and provides a decrease in internal pore size, leading to increases in low cycle and high cycle fatigue lives.

Correlation of microstructure, tensile properties and hole expansion ratio in cold rolled advanced high strength steels

NASA Astrophysics Data System (ADS)

Terrazas, Oscar R.

The demand for advanced high strength steels (AHSS) with higher strengths is increasing in the automotive industry. While there have been major improvements recently in the trade-off between ductility and strength, sheared-edge formability of AHSS remains a critical issue. AHSS sheets exhibit cracking during stamping and forming operations below the predictions of forming limits. It has become important to understand the correlation between microstructure and sheared edge formability. The present work investigates the effects of shearing conditions, microstructure, and tensile properties on sheared edge formability. Seven commercially produced steels with tensile strengths of 1000 +/- 100 MPa were evaluated: five dual-phase (DP) steels with different compositions and varying microstructural features, one trip aided bainitic ferrite (TBF) steel, and one press-hardened steel tempered to a tensile strength within the desired range. It was found that sheared edge formability is influenced by the martensite in DP steels. Quantitative stereology measurements provided results that showed martensite size and distribution affect hole expansion ratio (HER). The overall trend is that HER increases with more evenly dispersed martensite throughout the microstructure. This microstructure involves a combination of martensite size, contiguity, mean free distance, and number of colonies per unit area. Additionally, shear face characterization showed that the fracture and burr region affect HER. The HER decreases with increasing size of fracture and burr region. With a larger fracture and burr region more defects and/or micro-cracks will be present on the shear surface. This larger fracture region on the shear face facilitates cracking in sheared edge formability. Finally, the sheared edge formability is directly correlated to true fracture strain (TFS). The true fracture strain from tensile samples correlates to the HER values. HER increases with increasing true fracture strain.

Quantitative phase imaging by wide field lensless digital holographic microscope

NASA Astrophysics Data System (ADS)

Adinda-Ougba, A.; Koukourakis, N.; Essaidi, A.; Ger­hardt, N. C.; Hofmann, M. R.

2015-05-01

Wide field, lensless microscopes have been developed for telemedicine and for resource limited setting [1]. They are based on in-line digital holography which is capable to provide amplitude and phase information resulting from numerical reconstruction. The phase information enables achieving axial resolution in the nanometer range. Hence, such microscopes provide a powerful tool to determine three-dimensional topologies of microstructures. In this contribution, a compact, low-cost, wide field, lensless microscope is presented, which is capable of providing topological profiles of microstructures in transparent material. Our setup consist only of two main components: a CMOSsensor chip and a laser diode without any need of a pinhole. We use this very simple setup to record holograms of microobjects. A wide field of view of ~24 mm², and a lateral resolution of ~2 μm are achieved. Moreover, amplitude and phase information are obtained from the numerical reconstruction of the holograms using a phase retrieval algorithm together with the angular spectrum propagation method. Topographic information of highly transparent micro-objects is obtained from the phase data. We evaluate our system by recording holograms of lines with different depths written by a focused laser beam. A reliable characterization of laser written microstructures is crucial for their functionality. Our results show that this system is valuable for determination of topological profiles of microstructures in transparent material.

The Influence on Microstructure and Microtexture on Fatigue Crack Initiation and Growth in Alpha + Beta Titanium

DTIC Science & Technology

2011-10-01

crack growth, microstructure, EBSD, fractography 16. SECURITY CLASSIFICATION OF: 17. LIMITATION OF ABSTRACT: SAR NUMBER OF PAGES 6 19a...differences in thermomechanical processing routes have been correlated with variations in fatigue life through the use of quantitative fractography ...Keywords: fatigue, crack initiation, crack growth, microstructure, EBSD, fractography 1. Introduction Two-phase titanium alloys have the unique

Microstructural Quantification, Property Prediction, and Stochastic Reconstruction of Heterogeneous Materials Using Limited X-Ray Tomography Data

NASA Astrophysics Data System (ADS)

Li, Hechao

An accurate knowledge of the complex microstructure of a heterogeneous material is crucial for quantitative structure-property relations establishment and its performance prediction and optimization. X-ray tomography has provided a non-destructive means for microstructure characterization in both 3D and 4D (i.e., structural evolution over time). Traditional reconstruction algorithms like filtered-back-projection (FBP) method or algebraic reconstruction techniques (ART) require huge number of tomographic projections and segmentation process before conducting microstructural quantification. This can be quite time consuming and computationally intensive. In this thesis, a novel procedure is first presented that allows one to directly extract key structural information in forms of spatial correlation functions from limited x-ray tomography data. The key component of the procedure is the computation of a "probability map", which provides the probability of an arbitrary point in the material system belonging to specific phase. The correlation functions of interest are then readily computed from the probability map. Using effective medium theory, accurate predictions of physical properties (e.g., elastic moduli) can be obtained. Secondly, a stochastic optimization procedure that enables one to accurately reconstruct material microstructure from a small number of x-ray tomographic projections (e.g., 20 - 40) is presented. Moreover, a stochastic procedure for multi-modal data fusion is proposed, where both X-ray projections and correlation functions computed from limited 2D optical images are fused to accurately reconstruct complex heterogeneous materials in 3D. This multi-modal reconstruction algorithm is proved to be able to integrate the complementary data to perform an excellent optimization procedure, which indicates its high efficiency in using limited structural information. Finally, the accuracy of the stochastic reconstruction procedure using limited X-ray projection data is ascertained by analyzing the microstructural degeneracy and the roughness of energy landscape associated with different number of projections. Ground-state degeneracy of a microstructure is found to decrease with increasing number of projections, which indicates a higher probability that the reconstructed configurations match the actual microstructure. The roughness of energy landscape can also provide information about the complexity and convergence behavior of the reconstruction for given microstructures and projection number.

Quantitative assessment of submicron scale anisotropy in tissue multifractality by scattering Mueller matrix in the framework of Born approximation

NASA Astrophysics Data System (ADS)

Das, Nandan Kumar; Dey, Rajib; Chakraborty, Semanti; Panigrahi, Prasanta K.; Meglinski, Igor; Ghosh, Nirmalya

2018-04-01

A number of tissue-like disordered media exhibit local anisotropy of scattering in the scaling behavior. Scaling behavior contains wealth of fractal or multifractal properties. We demonstrate that the spatial dielectric fluctuations in a sample of biological tissue exhibit multifractal anisotropy. Multifractal anisotropy encoded in the wavelength variation of the light scattering Mueller matrix and manifesting as an intriguing spectral diattenuation effect. We developed an inverse method for the quantitative assessment of the multifractal anisotropy. The method is based on the processing of relevant Mueller matrix elements in Fourier domain by using Born approximation, followed by the multifractal analysis. The approach promises for probing subtle micro-structural changes in biological tissues associated with the cancer and precancer, as well as for non-destructive characterization of a wide range of scattering materials.

Scanning mass spectrometer for quantitative reaction studies on catalytically active microstructures.

PubMed

Roos, M; Kielbassa, S; Schirling, C; Häring, T; Bansmann, J; Behm, R J

2007-08-01

We describe an apparatus for spatially resolving scanning mass spectrometry which is able to measure the gas composition above catalytically active microstructures or arrays of these microstructures with a lateral resolution of better than 100 mum under reaction conditions and which allows us to quantitatively determine reaction rates on individual microstructures. Measurements of the three-dimensional gas composition at different vertical distances and separations between active structures allow the evaluation of gas phase mass transport effects. The system is based on a piezoelectrically driven positioning substage for controlled lateral and vertical positioning of the sample under a rigidly mounted capillary probe connecting to a mass spectrometer. Measurements can be performed at pressures in the range of <10(-2)-10 mbars and temperatures between room temperature and 450 degrees C. The performance of the setup is demonstrated using the CO oxidation reaction on Pt microstructures on Si with sizes between 100 and 300 mum and distances in the same order of magnitude, evaluating CO(2) formation and CO consumption above the microstructures. The rapidly decaying lateral resolution with increasing distance between sample and probe underlines the effects of (lateral) gas transport in the room between sample and probe. The reaction rates and apparent activation energy obtained from such measurements agree with previous data on extended surfaces, demonstrating the feasibility of determining absolute reaction rates on individual microstructures.

New Mechanistic Models of Long Term Evolution of Microstructure and Mechanical Properties of Nickel Based Alloys

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

Kruzic, Jamie J.; Evans, T. Matthew; Greaney, P. Alex

The report describes the development of a discrete element method (DEM) based modeling approach to quantitatively predict deformation and failure of typical nickel based superalloys. A series of experimental data, including microstructure and mechanical property characterization at 600°C, was collected for a relatively simple, model solid solution Ni-20Cr alloy (Nimonic 75) to determine inputs for the model and provide data for model validation. Nimonic 75 was considered ideal for this study because it is a certified tensile and creep reference material. A series of new DEM modeling approaches were developed to capture the complexity of metal deformation, including cubic elasticmore » anisotropy and plastic deformation both with and without strain hardening. Our model approaches were implemented into a commercially available DEM code, PFC3D, that is commonly used by engineers. It is envisioned that once further developed, this new DEM modeling approach can be adapted to a wide range of engineering applications.« less

Gas tungsten arc welding and friction stir welding of ultrafine grained AISI 304L stainless steel: Microstructural and mechanical behavior characterization

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

Sabooni, S., E-mail: s.sabooni@ma.iut.ac.ir; Karimzadeh, F.; Enayati, M.H.

In the present study, an ultrafine grained (UFG) AISI 304L stainless steel with the average grain size of 650 nm was successfully welded by both gas tungsten arc welding (GTAW) and friction stir welding (FSW). GTAW was applied without any filler metal. FSW was also performed at a constant rotational speed of 630 rpm and different welding speeds from 20 to 80 mm/min. Microstructural characterization was carried out by High Resolution Scanning Electron Microscopy (HRSEM) with Electron Backscattered Diffraction (EBSD) and Transmission Electron Microscopy (TEM). Nanoindentation, microhardness measurements and tensile tests were also performed to study the mechanical properties ofmore » the base metal and weldments. The results showed that the solidification mode in the GTAW welded sample is FA (ferrite–austenite) type with the microstructure consisting of an austenite matrix embedded with lath type and skeletal type ferrite. The nugget zone microstructure in the FSW welded samples consisted of equiaxed dynamically recrystallized austenite grains with some amount of elongated delta ferrite. Sigma phase precipitates were formed in the region ahead the rotating tool during the heating cycle of FSW, which were finally fragmented into nanometric particles and distributed in the weld nugget. Also there is a high possibility that the existing delta ferrite in the microstructure rapidly transforms into sigma phase particles during the short thermal cycle of FSW. These suggest that high strain and deformation during FSW can promote sigma phase formation. The final austenite grain size in the nugget zone was found to decrease with increasing Zener–Hollomon parameter, which was obtained quantitatively by measuring the peak temperature, calculating the strain rate during FSW and exact examination of hot deformation activation energy by considering the actual grain size before the occurrence of dynamic recrystallization. Mechanical properties observations showed that the welding efficiency of the FSW welded sample is around 70%, which is more than 20% higher than the GTAW welded sample. - Highlights: • Microstructure and mechanical properties of UFG 304L stainless steel were studied during GTAW and FSW. • Sigma phase formation mechanism was studied during FSW of 304L stainless steel. • THERMOCALC analysis was performed to obtain possible formation temperatures for sigma phase. • Nano-mechanical twins were found in the TMAZ region.« less

Microstructural characterization and mechanical properties of Excel alloy pressure tube material

NASA Astrophysics Data System (ADS)

Sattari, Mohammad

Microstructural characterization and mechanical properties of Excel (Zr-3.5%Sn-0.8%Mo-0.8%Nb), a dual phase alphaZr -hcp and betaZr-bcc pressure tube material, is discussed in the current study which is presented in manuscript format. Chapter 3 discusses phase transformation temperatures using different techniques such as quantitative metallography, differential scanning calorimetry (DSC), and electrical resistivity. It was found that the alphaZr → alphaZr+beta Zr and alphaZr+betaZr → betaZr transformation temperatures are in the range of 600-690°C and 960-970°C respectively. Also it was observed that upon quenching from temperatures below ˜860°C the martensitic transformation of betaZr to alpha'--hcp is halted and instead the microstructure transforms into retained Zr with o hexagonal precipitates inside betaZr grains. Chapter 4 deals with aging response of Excel alloy. Precipitation hardening was observed in samples water-quenched from high in the alphaZr+beta Zr or betaZr regions followed by aging. The optimum aging conditions were found to be 450°C for 1 hour. Transmission electron microscopy (TEM) showed dispersion of fine precipitates (˜10nm) inside the martensitic phase. Energy dispersive X-ray spectroscopy (EDS) showed the chemical composition of precipitates to be Zr-30wt%Mo-25wt%Nb-2wt%Fe. Electron crystallography using whole pattern symmetry of the convergent beam electron diffraction (CBED) patterns together with selected area diffraction (SAD) polycrystalline ring patterns, suggests the -6m2 point group for the precipitates belonging to hexagonal crystal structure, with a= 2.936 A and c=4.481 A, i.e. c/a =1.526. Crystallographic texture and high temperature tensile properties as well as creep-rupture properties of different microstructures are discussed in Chapter 5. Texture analysis showed that solution treatment high in the alpha Zr+betaZr or betaZr regions followed by water quenching or air cooling results in a more random texture compared to typical pressure tube texture. Variant selection was observed upon water quenching while partial memory effect and some transformation texture with variant selection was observed in the air-cooled sample. The results of creep-rupture tests suggest that fully martensitic and aged microstructure has better creep properties at high stress levels (>700 MPa) while the microstructure from air cooling from high in the alphaZr+betaZr region is less sensitive to stress and shows better creep properties compared to the as-received annealed microstructure at lower stresses (<560 MPa).

Mapping axonal density and average diameter using non-monotonic time-dependent gradient-echo MRI

NASA Astrophysics Data System (ADS)

Nunes, Daniel; Cruz, Tomás L.; Jespersen, Sune N.; Shemesh, Noam

2017-04-01

White Matter (WM) microstructures, such as axonal density and average diameter, are crucial to the normal function of the Central Nervous System (CNS) as they are closely related with axonal conduction velocities. Conversely, disruptions of these microstructural features may result in severe neurological deficits, suggesting that their noninvasive mapping could be an important step towards diagnosing and following pathophysiology. Whereas diffusion based MRI methods have been proposed to map these features, they typically entail the application of powerful gradients, which are rarely available in the clinic, or extremely long acquisition schemes to extract information from parameter-intensive models. In this study, we suggest that simple and time-efficient multi-gradient-echo (MGE) MRI can be used to extract the axon density from susceptibility-driven non-monotonic decay in the time-dependent signal. We show, both theoretically and with simulations, that a non-monotonic signal decay will occur for multi-compartmental microstructures - such as axons and extra-axonal spaces, which were here used as a simple model for the microstructure - and that, for axons parallel to the main magnetic field, the axonal density can be extracted. We then experimentally demonstrate in ex-vivo rat spinal cords that its different tracts - characterized by different microstructures - can be clearly contrasted using the MGE-derived maps. When the quantitative results are compared against ground-truth histology, they reflect the axonal fraction (though with a bias, as evident from Bland-Altman analysis). As well, the extra-axonal fraction can be estimated. The results suggest that our model is oversimplified, yet at the same time evidencing a potential and usefulness of the approach to map underlying microstructures using a simple and time-efficient MRI sequence. We further show that a simple general-linear-model can predict the average axonal diameters from the four model parameters, and map these average axonal diameters in the spinal cords. While clearly further modelling and theoretical developments are necessary, we conclude that salient WM microstructural features can be extracted from simple, SNR-efficient multi-gradient echo MRI, and that this paves the way towards easier estimation of WM microstructure in vivo.

Mapping axonal density and average diameter using non-monotonic time-dependent gradient-echo MRI.

PubMed

Nunes, Daniel; Cruz, Tomás L; Jespersen, Sune N; Shemesh, Noam

2017-04-01

White Matter (WM) microstructures, such as axonal density and average diameter, are crucial to the normal function of the Central Nervous System (CNS) as they are closely related with axonal conduction velocities. Conversely, disruptions of these microstructural features may result in severe neurological deficits, suggesting that their noninvasive mapping could be an important step towards diagnosing and following pathophysiology. Whereas diffusion based MRI methods have been proposed to map these features, they typically entail the application of powerful gradients, which are rarely available in the clinic, or extremely long acquisition schemes to extract information from parameter-intensive models. In this study, we suggest that simple and time-efficient multi-gradient-echo (MGE) MRI can be used to extract the axon density from susceptibility-driven non-monotonic decay in the time-dependent signal. We show, both theoretically and with simulations, that a non-monotonic signal decay will occur for multi-compartmental microstructures - such as axons and extra-axonal spaces, which were here used as a simple model for the microstructure - and that, for axons parallel to the main magnetic field, the axonal density can be extracted. We then experimentally demonstrate in ex-vivo rat spinal cords that its different tracts - characterized by different microstructures - can be clearly contrasted using the MGE-derived maps. When the quantitative results are compared against ground-truth histology, they reflect the axonal fraction (though with a bias, as evident from Bland-Altman analysis). As well, the extra-axonal fraction can be estimated. The results suggest that our model is oversimplified, yet at the same time evidencing a potential and usefulness of the approach to map underlying microstructures using a simple and time-efficient MRI sequence. We further show that a simple general-linear-model can predict the average axonal diameters from the four model parameters, and map these average axonal diameters in the spinal cords. While clearly further modelling and theoretical developments are necessary, we conclude that salient WM microstructural features can be extracted from simple, SNR-efficient multi-gradient echo MRI, and that this paves the way towards easier estimation of WM microstructure in vivo. Copyright © 2017 Elsevier Inc. All rights reserved.

Characterization of ion irradiation effects on the microstructure, hardness, deformation and crack initiation behavior of austenitic stainless steel:Heavy ions vs protons

NASA Astrophysics Data System (ADS)

Gupta, J.; Hure, J.; Tanguy, B.; Laffont, L.; Lafont, M.-C.; Andrieu, E.

2018-04-01

Irradiation Assisted Stress Corrosion Cracking (IASCC) is a complex phenomenon of degradation which can have a significant influence on maintenance time and cost of core internals of a Pressurized Water Reactor (PWR). Hence, it is an issue of concern, especially in the context of lifetime extension of PWRs. Proton irradiation is generally used as a representative alternative of neutron irradiation to improve the current understanding of the mechanisms involved in IASCC. This study assesses the possibility of using heavy ions irradiation to evaluate IASCC mechanisms by comparing the irradiation induced modifications (in microstructure and mechanical properties) and cracking susceptibility of SA 304 L after both type of irradiations: Fe irradiation at 450 °C and proton irradiation at 350 °C. Irradiation-induced defects are characterized and quantified along with nano-hardness measurements, showing a correlation between irradiation hardening and density of Frank loops that is well captured by Orowan's formula. Both irradiations (iron and proton) increase the susceptibility of SA 304 L to intergranular cracking on subjection to Constant Extension Rate Tensile tests (CERT) in simulated nominal PWR primary water environment at 340 °C. For these conditions, cracking susceptibility is found to be quantitatively similar for both irradiations, despite significant differences in hardening and degree of localization.

Heart valve scaffold fabrication: Bioinspired control of macro-scale morphology, mechanics and micro-structure.

PubMed

D'Amore, Antonio; Luketich, Samuel K; Raffa, Giuseppe M; Olia, Salim; Menallo, Giorgio; Mazzola, Antonino; D'Accardi, Flavio; Grunberg, Tamir; Gu, Xinzhu; Pilato, Michele; Kameneva, Marina V; Badhwar, Vinay; Wagner, William R

2018-01-01

Valvular heart disease is currently treated with mechanical valves, which benefit from longevity, but are burdened by chronic anticoagulation therapy, or with bioprosthetic valves, which have reduced thromboembolic risk, but limited durability. Tissue engineered heart valves have been proposed to resolve these issues by implanting a scaffold that is replaced by endogenous growth, leaving autologous, functional leaflets that would putatively eliminate the need for anticoagulation and avoid calcification. Despite the diversity in fabrication strategies and encouraging results in large animal models, control over engineered valve structure-function remains at best partial. This study aimed to overcome these limitations by introducing double component deposition (DCD), an electrodeposition technique that employs multi-phase electrodes to dictate valve macro and microstructure and resultant function. Results in this report demonstrate the capacity of the DCD method to simultaneously control scaffold macro-scale morphology, mechanics and microstructure while producing fully assembled stent-less multi-leaflet valves composed of microscopic fibers. DCD engineered valve characterization included: leaflet thickness, biaxial properties, bending properties, and quantitative structural analysis of multi-photon and scanning electron micrographs. Quasi-static ex-vivo valve coaptation testing and dynamic organ level functional assessment in a pressure pulse duplicating device demonstrated appropriate acute valve functionality. Copyright © 2017. Published by Elsevier Ltd.

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

Automated Weld Characterization Using the Thermoelectric Method

NASA Technical Reports Server (NTRS)

Fulton, J. P.; Wincheski, B.; Namkung, M.

1992-01-01

The effective assessment of the integrity of welds is a complicated NDE problem that continues to be a challenge. To be able to completely characterize a weld, detailed knowledge of its tensile strength, ductility, hardness, microstructure, macrostructure, and chemical composition is needed. NDE techniques which can provide information on any of these features are extremely important. In this paper, we examine a seldom used approach based on the thermoelectric (TE) effect for characterizing welds and their associated heat affected zone (HAZ). The thermoelectric method monitors the thermoelectric power which is sensitive to small changes in the kinetics of the conduction electrons near the Fermi surface that can be caused by changes in the local microstructure. The technique has been applied to metal sorting, quality testing, flaw detection, thickness gauging of layers, and microscopic structural analysis. To demonstrate the effectiveness of the technique for characterizing welds, a series of tungsten-inert-gas welded Inconel-718 samples were scanned with a computer controlled TE probe. The samples were then analyzed using a scanning electron microscope and Rockwell hardness tests to characterize the weld and the associated HAZ. We then correlated the results with the TE measurements to provide quantitative information on the size of the HAZ and the degree of hardness of the material in the weld region. This provides potentially valuable information on the strength and fatigue life of the weld. We begin the paper by providing a brief review of the TE technique and then highlight some of the factors that can effect the measurements. Next, we provide an overview of the experimental procedure and discuss the results. Finally, we summarize our findings and consider areas for future research.

Grain Refinement and Improvement of Solidification Defects in Direct-Chill Cast Billets of A4032 Alloy by Melt Conditioning

NASA Astrophysics Data System (ADS)

Li, Hu-Tian; Zhao, Pizhi; Yang, Rongdong; Patel, Jayesh B.; Chen, Xiangfu; Fan, Zhongyun

2017-10-01

Melt-conditioned, direct-chill (MC-DC) casting is an emerging technology to manipulate the solidification process by melt conditioning via intensive shearing in the sump during DC casting to tailor the solidification microstructure and defect formation. When using MC-DC casting technology in an industrial scale DC cast billet of an A4032 aluminum alloy, significant grain refinement and uniform microstructure can be achieved in the primary α-Al phase with fine secondary dendritic arm spacing (SDAS). Improved macrosegregation is quantitatively characterized and correlated with the suppression of channel segregation. The mechanisms for the prevention of channel segregation are attributed to the increased local cooling rate in the liquid-solid phase region in the sump and the formation of fine equiaxed dendritic grains under intensive melt shearing during MC-DC casting. A critical cooling rate has been identified to be around 0.5 to 1 K/s (°C/s) for the channel segregation to happen in the investigated alloy based on quantitative metallographic results of SDAS. Reduction and refinement of microporosity is attributed to the improved permeability in the liquid-solid phase region estimated by the Kozeny-Carman relationship. The potential improvement in the mechanical properties achievable in MC-DC cast billets is indicated by the finer and more uniform forging streamline in the forgings of MC-DC cast billet.

Facile one-pot synthesis of flower-like AgCl microstructures and enhancing of visible light photocatalysis

PubMed Central

2013-01-01

Flower-like AgCl microstructures with enhanced visible light-driven photocatalysis are synthesized by a facile one-pot hydrothermal process for the first time. The evolution process of AgCl from dendritic structures to flower-like octagonal microstructures is investigated quantitatively. Furthermore, the flower-like AgCl microstructures exhibit enhanced ability of visible light-assisted photocatalytic degradation of methyl orange. The enhanced photocatalytic activity of the flower-like AgCl microstructure is attributed to its three-dimensional hierarchical structure exposing with [100] facets. This work provides a fresh view into the insight of electrochemical process and the application area of visible light photocatalysts. PMID:24153176

Stablization of Nanotwinned Microstructures in Stainless Steels Through Alloying and Microstructural Design

DTIC Science & Technology

2013-08-23

REPORT Stablization of Nanotwinned Microstructures in Stainless Steels Through Alloying and Microstructural Design 14. ABSTRACT 16. SECURITY...15. SUBJECT TERMS materials design, stainless steels , plastic deformation by twinning, computational materials science, experimental characterization...Standard Form 298 (Rev 8/98) Prescribed by ANSI Std. Z39.18 - 30-Jun-2013 Stablization of Nanotwinned Microstructures in Stainless Steels Through

Micro-to-nano-scale deformation mechanisms of a bimodal ultrafine eutectic composite

PubMed Central

Lee, Seoung Wan; Kim, Jeong Tae; Hong, Sung Hwan; Park, Hae Jin; Park, Jun-Young; Lee, Nae Sung; Seo, Yongho; Suh, Jin Yoo; Eckert, Jürgen; Kim, Do Hyang; Park, Jin Man; Kim, Ki Buem

2014-01-01

The outstading mechanical properties of bimodal ultrafine eutectic composites (BUECs) containing length scale hierarchy in eutectic structure were demonstrated by using AFM observation of surface topography with quantitative height measurements and were interpreted in light of the details of the deformation mechanisms by three different interface modes. It is possible to develop a novel strain accommodated eutectic structure for triggering three different interface-controlled deformation modes; (I) rotational boundary mode, (II) accumulated interface mode and (III) individual interface mode. A strain accommodated microstructure characterized by the surface topology gives a hint to design a novel ultrafine eutectic alloys with excellent mechanical properties. PMID:25265897

Development of 1500mm Wide Wrought Magnesium Alloys by Twin Roll Casting Technique in Turkey

NASA Astrophysics Data System (ADS)

Duygulu, Ozgur; Ucuncuoglu, Selda; Oktay, Gizem; Temur, Deniz Sultan; Yucel, Onuralp; Kaya, Ali Arslan

Magnesium alloy AZ31, AZ61, AZ91, AM50 and AM60 sheets were produced by twin roll casting first time in Turkey. Sheets of 4.5-6.5mm thick and 1500mm width were successfully achieved. Microstructure of the sheet was analyzed by optical microscope, scanning electron microscope (SEM) and transmission electron microscope (TEM). Semi-quantitative analyses were performed by SEM-EDS. In addition, X-ray studies were performed for both characterization and texture purposes. Mechanical properties were investigated by tensile tests and also hardness measurements. Homogenization and annealing heat treatments were performed on the produced sheets.

Application of X-ray phase contrast micro-tomography to the identification of traditional Chinese medicines

NASA Astrophysics Data System (ADS)

Ye, L. L.; Xue, Y. L.; Ni, L. H.; Tan, H.; Wang, Y. D.; Xiao, T. Q.

2013-07-01

Nondestructive and in situ investigation to the characteristic microstructures are important to the identification of traditional Chinese medicines (TCMs), especially for precious specimens and samples with oil contains. X-ray phase contrast micro-tomography (XPCMT) could be a practical solution for this kind of investigation. Fructus Foeniculi, a fruit kind of TCMs, is selected as the test sample. Experimental results show that the characteristic microstructures of Fructus Foeniculi, including vittae, vascular bundles, embryo, endosperm and the mesocarp reticulate cells around the vittae can be clearly distinguished and the integrated dissepiments microstructure in the vittae was observed successfully. Especially, for the first time, with virtual slice technique, it can investigate the liquid contains inside the TCMs. The results show that the vittae filled with volatile oil in the oil chamber were observed with this nondestructive and in situ 3-dimensional imaging technique. Furthermore, taking the advantage of micro-computed tomography, we can obtain the characteristic microstructures' quantitative information of the volume in liquid state. The volume of the oil chambers and the volatile oil, which are contained inside the vittae, was quantitatively analyzed. Accordingly, it can calculate the volume ratio of the volatile oil easily and accurately. As a result, we could conclude that XPCMT could be a useful tool for the nondestructive identification and quantitative analysis to TCMs.

Structural characterization of sol-gel derived oxide nanostuctures using synchrotron x-ray techniques

NASA Astrophysics Data System (ADS)

Sun, Tao

Ceramic oxides possess extraordinarily rich functionalities. With the advent of nanofabrication techniques, it is now possible to grow nanostructured oxides with precise control of composition, morphology, and microstructure, which has re-vitalized the research in the field of traditional ceramics. The unexpected behavior and enhanced properties of oxide nanostructures have been extensively reported. However, knowledge about the underlying mechanisms as well as structural implications is still quite limited. Therefore, it is imperative to develop and employ sophisticated characterization tools for unraveling the structure-property relationships for oxide nanostructures. The present thesis work aims at addressing the critical issues associated with fabrication, and more importantly, structural characterization of functional oxide nanostructures. The dissertation starts with introducing the strategy for synthesizing phase-pure and highly controlled oxide nanostructures using sol-gel deposition and an innovative approach called "soft" electron beam lithography. Some specific oxides are chosen for the present study, such as BiFeO3, CoFe2O4, and SnO2, because of their scientific and technological significance. Subsequent to fabrication of tailored oxide nanostructures, advanced synchrotron x-ray scattering techniques have been applied for structural characterization. The nucleation and growth behavior of BiFeO3 thin film was investigated using in situ grazing-incidence small-angle x-ray scattering (GISAXS) technique. The results reveal that the kinetics for early-stage nuclei growth are governed by the oriented-attachment model. Moreover, the porous structures of undoped and Pd-doped semiconducting SnOx thin films were quantitatively characterized using GISAXS. By correlating the structural parameters with H2 sensitivity of SnOx films, it is found out that the microstructure of doped film is favorable for gas sensing, but it is not the major reason for the overall property enhancement arising from the dopant. Furthermore, a novel method based on scanning x-ray microdiffraction technique is proposed and applied for probing the strain distribution around individual CoFe2O4 nanoline epitaxially grown on MgO substrate. It is demonstrated that x-ray diffuse scattering intensity can be used to gauge the edge-induced subtle strain variation. The dissertation underscores the need for quantitative understanding of structural underpinning in the mechanisms and behavior of oxide nanostructures, and highlights the role of advanced synchrotron x-ray scattering approaches.

Assessment of MARMOT Grain Growth Model

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

Fromm, B.; Zhang, Y.; Schwen, D.

2015-12-01

This report assesses the MARMOT grain growth model by comparing modeling predictions with experimental results from thermal annealing. The purpose here is threefold: (1) to demonstrate the validation approach of using thermal annealing experiments with non-destructive characterization, (2) to test the reconstruction capability and computation efficiency in MOOSE, and (3) to validate the grain growth model and the associated parameters that are implemented in MARMOT for UO 2. To assure a rigorous comparison, the 2D and 3D initial experimental microstructures of UO 2 samples were characterized using non-destructive Synchrotron x-ray. The same samples were then annealed at 2273K for grainmore » growth, and their initial microstructures were used as initial conditions for simulated annealing at the same temperature using MARMOT. After annealing, the final experimental microstructures were characterized again to compare with the results from simulations. So far, comparison between modeling and experiments has been done for 2D microstructures, and 3D comparison is underway. The preliminary results demonstrated the usefulness of the non-destructive characterization method for MARMOT grain growth model validation. A detailed analysis of the 3D microstructures is in progress to fully validate the current model in MARMOT.« less

Characterization and reconstruction of 3D stochastic microstructures via supervised learning.

PubMed

Bostanabad, R; Chen, W; Apley, D W

2016-12-01

The need for computational characterization and reconstruction of volumetric maps of stochastic microstructures for understanding the role of material structure in the processing-structure-property chain has been highlighted in the literature. Recently, a promising characterization and reconstruction approach has been developed where the essential idea is to convert the digitized microstructure image into an appropriate training dataset to learn the stochastic nature of the morphology by fitting a supervised learning model to the dataset. This compact model can subsequently be used to efficiently reconstruct as many statistically equivalent microstructure samples as desired. The goal of this paper is to build upon the developed approach in three major directions by: (1) extending the approach to characterize 3D stochastic microstructures and efficiently reconstruct 3D samples, (2) improving the performance of the approach by incorporating user-defined predictors into the supervised learning model, and (3) addressing potential computational issues by introducing a reduced model which can perform as effectively as the full model. We test the extended approach on three examples and show that the spatial dependencies, as evaluated via various measures, are well preserved in the reconstructed samples. © 2016 The Authors Journal of Microscopy © 2016 Royal Microscopical Society.

T1, diffusion tensor, and quantitative magnetization transfer imaging of the hippocampus in an Alzheimer's disease mouse model.

PubMed

Whittaker, Heather T; Zhu, Shenghua; Di Curzio, Domenico L; Buist, Richard; Li, Xin-Min; Noy, Suzanna; Wiseman, Frances K; Thiessen, Jonathan D; Martin, Melanie

2018-07-01

Alzheimer's disease (AD) pathology causes microstructural changes in the brain. These changes, if quantified with magnetic resonance imaging (MRI), could be studied for use as an early biomarker for AD. The aim of our study was to determine if T 1 relaxation, diffusion tensor imaging (DTI), and quantitative magnetization transfer imaging (qMTI) metrics could reveal changes within the hippocampus and surrounding white matter structures in ex vivo transgenic mouse brains overexpressing human amyloid precursor protein with the Swedish mutation. Delineation of hippocampal cell layers using DTI color maps allows more detailed analysis of T 1 -weighted imaging, DTI, and qMTI metrics, compared with segmentation of gross anatomy based on relaxation images, and with analysis of DTI or qMTI metrics alone. These alterations are observed in the absence of robust intracellular Aβ accumulation or plaque deposition as revealed by histology. This work demonstrates that multiparametric quantitative MRI methods are useful for characterizing changes within the hippocampal substructures and surrounding white matter tracts of mouse models of AD. Copyright © 2018. Published by Elsevier Inc.

A synchrotron-based local computed tomography combined with data-constrained modelling approach for quantitative analysis of anthracite coal microstructure

PubMed Central

Chen, Wen Hao; Yang, Sam Y. S.; Xiao, Ti Qiao; Mayo, Sherry C.; Wang, Yu Dan; Wang, Hai Peng

2014-01-01

Quantifying three-dimensional spatial distributions of pores and material compositions in samples is a key materials characterization challenge, particularly in samples where compositions are distributed across a range of length scales, and where such compositions have similar X-ray absorption properties, such as in coal. Consequently, obtaining detailed information within sub-regions of a multi-length-scale sample by conventional approaches may not provide the resolution and level of detail one might desire. Herein, an approach for quantitative high-definition determination of material compositions from X-ray local computed tomography combined with a data-constrained modelling method is proposed. The approach is capable of dramatically improving the spatial resolution and enabling finer details within a region of interest of a sample larger than the field of view to be revealed than by using conventional techniques. A coal sample containing distributions of porosity and several mineral compositions is employed to demonstrate the approach. The optimal experimental parameters are pre-analyzed. The quantitative results demonstrated that the approach can reveal significantly finer details of compositional distributions in the sample region of interest. The elevated spatial resolution is crucial for coal-bed methane reservoir evaluation and understanding the transformation of the minerals during coal processing. The method is generic and can be applied for three-dimensional compositional characterization of other materials. PMID:24763649

Effects of sparse sampling in combination with iterative reconstruction on quantitative bone microstructure assessment

NASA Astrophysics Data System (ADS)

Mei, Kai; Kopp, Felix K.; Fehringer, Andreas; Pfeiffer, Franz; Rummeny, Ernst J.; Kirschke, Jan S.; Noël, Peter B.; Baum, Thomas

2017-03-01

The trabecular bone microstructure is a key to the early diagnosis and advanced therapy monitoring of osteoporosis. Regularly measuring bone microstructure with conventional multi-detector computer tomography (MDCT) would expose patients with a relatively high radiation dose. One possible solution to reduce exposure to patients is sampling fewer projection angles. This approach can be supported by advanced reconstruction algorithms, with their ability to achieve better image quality under reduced projection angles or high levels of noise. In this work, we investigated the performance of iterative reconstruction from sparse sampled projection data on trabecular bone microstructure in in-vivo MDCT scans of human spines. The computed MDCT images were evaluated by calculating bone microstructure parameters. We demonstrated that bone microstructure parameters were still computationally distinguishable when half or less of the radiation dose was employed.

The relationship between structure and magnetic properties in ultra-fine grained/nanostructured FePd alloys

NASA Astrophysics Data System (ADS)

Okumura, Hideyuki

In this study, the magnetic behavior including coercivity and the magnetic phase transition (ferromagnetic ↔ paramagnetic) and related phenomena were qualitatively and quantitatively investigated in ultra-fine grained/nanostructured FePd permanent magnet alloys, in relation to the microstructure and defect structure, and the results were compared with bulk FePd. Most of the alloy specimens investigated were in the form of epoxybonded magnets or isostatically-pressed pellets, formed from powders which were produced with high energy ball milling. Some results of thin films and ribbons produced with sputtering and melt-spinning, respectively, are also included in this thesis. Characterization of the materials was performed by using X-ray diffraction techniques with texture measurement, transmission electron microscopy with Lorentz microscopy, scanning electron microscopy with EDS analysis, optical microscopy and vibrating sample magnetometry. X-ray line broadening analysis was utilized for the quantitative characterization of the nanoscale microstructure, and it was found that the Cauchy-Gaussian profile assumption best describes the broadening data. Enhanced coercivities ˜10 times those of the bulk FePd obtained using conventional heat treatments were explained as the result of statistical (stochastic) unpinning of interaction domain walls out of the potential well at the grain boundary, and there is also an additional effect ascribed to an increase of the magnetocrystalline anisotropy, which is mainly due to the metastable c/a ratio of the nanostructured ordered phase and possibly to stress anisotropy. At the same time, there is also a decrease of the coercivity for smaller grain sizes because of the "magnetically soft" grain boundary phase. A semi-quantitative theoretical model is proposed, which includes the effect of exchange coupling between the ordered grains. The so-called Kronmuller analysis based on the wall pinning model was self-consistent, supporting the notion that wall pinning by grain boundary is the dominant mechanism controlling the coercivity in the nanostructured aggregates in which the magnetic structure is comprised of interaction domains. Furthermore, conventionally structure-insensitive, intrinsic properties such as the saturation magnetization and Curie temperature were found to become structure-sensitive in these materials. The results were semi-quantitatively explained by consideration of the extraordinary microstructure and defect structure involving the high and complex strain fields, metastable tetragonalities, nonequilibrium grain boundaries, extremely high surface-to-volume ratios and perturbed coordination spheres. The possible change in the atomic bond character particularly around grain boundaries is also briefly discussed. It seems that there is a significant fluctuation in exchange couplings at the grain boundary volume, causing the variation of the saturation magnetization, while for the variation of the Curie temperature the powder surface instead of the grain boundary is more important. A modified localized moment model and thus Hund's rules seem applicable to the FePd alloy systems, and the spin density fluctuations seem small in the FePd alloys.

Microstructure of wave propagation during combustion synthesis of advanced materials: Experiments and theory

NASA Astrophysics Data System (ADS)

Hwang, Stephen

Combustion synthesis (CS) is an attractive method for producing advanced materials, including ceramics, intermetallics, and composites. In this process, after initiation by an external heat source, a highly exothermic reaction propagates through the sample in a self-sustained combustion wave. The process offers the possibility of producing materials with novel structures and properties. At conventional magnifications and imaging rates, the combustion wave appears to propagate in a planar, steady manner. However, using higher magnifications (>400X) and imaging rates (1000 frames/sec), fluctuations in the shape and propagation of the combustion front were observed. These variations in local conditions (i.e., the microstructure of the combustion wave) can influence the microstructure and properties of materials produced by combustion synthesis. In this work, the microstructure of wave propagation during combustion synthesis is investigated experimentally and theoretically. Using microscopic high-speed imaging, the spatial and temporal fluctuations of the combustion front shape and propagation were investigated. New image analysis methods were developed to characterize the heterogeneity of the combustion front quantitatively. The initial organization of the reaction medium was found to affect the heterogeneity of the combustion wave. Moreover, at the microscopic level, two different regimes of combustion propagation were observed. In the quasihomogeneous mechanism, the microstructure of the combustion wave resembles what is viewed macroscopically, and steady, planar propagation is observed. In the relay-race mechanism, while planar at the macroscopic level, the combustion front profiles are irregularly shaped, with arc-shaped convexities and concavities at the microscopic level. Also, the reaction front propagates as a series of rapid jumps and hesitations. Based on the combustion wave microstructure, new criteria were developed to determine the boundaries between quasihomogeneous and relay-race mechanisms, as functions of the initial organization of the reaction medium (i.e. particle size and porosity). In conjunction with the experiments, a microheterogeneous cell model was developed that simulates the local propagation of the combustion wave. Accounting for the stochastically organized medium with non-uniform properties, calculated results for the microstructural parameters of the combustion wave, and their dependence on density and reactant particle size, were in good qualitative agreement with experimental data.

Effect of Long-Term Service on Microstructure and Mechanical Properties of Martensitic 9% Cr Steel

NASA Astrophysics Data System (ADS)

Golański, Grzegorz; Zielińska-Lipiec, Anna; Zieliński, Adam; Sroka, Marek

2017-03-01

The paper presents the results of research on the X10CrMoVNbN9-1 (T91) steel after long-term service. The material for testing was taken from a pipe section of a boiler superheater coil serviced for around 105,000 h at the temperature of 540 °C, at the pressure of 12.5 MPa. A quantitative analysis including the measurement of mean diameter of subgrains and precipitates as well as the density of dislocations of the examined steel was performed by means of TEM. The microscopic tests of T91 steel were complemented with the results of tests on mechanical properties which included also the short creep tests. After service, the investigated steel was characterized by a retained lath microstructure of tempered martensite with fine subgrain and quite large density of dislocations as well as numerous precipitates. In the microstructure, apart from the particles of M23C6 and MX (VX, NbC, V-wings), the precipitates of Laves phase and single particles of Z phase were revealed. It has been shown that the extent of degradation of the T91 steel microstructure was minor, which resulted from its low temperature of service. Performed tests of mechanical properties showed that these properties fulfilled the minimum requirements for this steel in the as-received condition. A favorable influence of fine precipitates of Laves phase on mechanical properties was observed. Moreover, an insignificant influence of single precipitates of Z phase on the creep resistance of the examined steel was stated.

Microstructural analysis of aluminum high pressure die castings

NASA Astrophysics Data System (ADS)

David, Maria Diana

Microstructural analysis of aluminum high pressure die castings (HPDC) is challenging and time consuming. Automating the stereology method is an efficient way in obtaining quantitative data; however, validating the accuracy of this technique can also pose some challenges. In this research, a semi-automated algorithm to quantify microstructural features in aluminum HPDC was developed. Analysis was done near the casting surface where it exhibited fine microstructure. Optical and Secondary electron (SE) and backscatter electron (BSE) SEM images were taken to characterize the features in the casting. Image processing steps applied on SEM and optical micrographs included median and range filters, dilation, erosion, and a hole-closing function. Measurements were done on different image pixel resolutions that ranged from 3 to 35 pixel/μm. Pixel resolutions below 6 px/μm were too low for the algorithm to distinguish the phases from each other. At resolutions higher than 6 px/μm, the volume fraction of primary α-Al and the line intercept count curves plateaued. Within this range, comparable results were obtained validating the assumption that there is a range of image pixel resolution relative to the size of the casting features at which stereology measurements become independent of the image resolution. Volume fraction within this curve plateau was consistent with the manual measurements while the line intercept count was significantly higher using the computerized technique for all resolutions. This was attributed to the ragged edges of some primary α-Al; hence, the algorithm still needs some improvements. Further validation of the code using other castings or alloys with known phase amount and size may also be beneficial.

Sex- and Age-Related Differences in Bone Microarchitecture in Men Relative to Women Assessed by High-Resolution Peripheral Quantitative Computed Tomography

PubMed Central

Amin, Shreyasee; Khosla, Sundeep

2012-01-01

The trabecular and cortical compartments of bone each contributes to bone strength. Until recently, assessment of trabecular and cortical microstructure has required a bone biopsy. Now, trabecular and cortical microstructure of peripheral bone sites can be determined noninvasively using high-resolution peripheral quantitative computed tomography (HR-pQCT). Studies that have used HR-pQCT to evaluate cohorts of both men and women have provided novel insights into the changes in bone microarchitecture that occur with age between the sexes, which may help to explain the lower fracture incidence in older men relative to women. This review will highlight observations from these studies on both the sex- and age-related differences in trabecular and cortical microstructure that may underlie the differences in bone strength, and thereby fracture risk, between men and women. PMID:22496983

Anisotropic and Hierarchical Porosity in Multifunctional Ceramics

NASA Astrophysics Data System (ADS)

Lichtner, Aaron Zev

The performance of multifunctional porous ceramics is often hindered by the seemingly contradictory effects of porosity on both mechanical and non-structural properties and yet a sufficient body of knowledge linking microstructure to these properties does not exist. Using a combination of tailored anisotropic and hierarchical materials, these disparate effects may be reconciled. In this project, a systematic investigation of the processing, characterization and properties of anisotropic and isotropic hierarchically porous ceramics was conducted. The system chosen was a composite ceramic intended as the cathode for a solid oxide fuel cell (SOFC). Comprehensive processing investigations led to the development of approaches to make hierarchical, anisotropic porous microstructures using directional freeze-casting of well dispersed slurries. The effect of all the important processing parameters was investigated. This resulted in an ability to tailor and control the important microstructural features including the scale of the microstructure, the macropore size and total porosity. Comparable isotropic porous ceramics were also processed using fugitive pore formers. A suite of characterization techniques including x-ray tomography and 3-D sectional scanning electron micrographs (FIB-SEM) was used to characterize and quantify the green and partially sintered microstructures. The effect of sintering temperature on the microstructure was quantified and discrete element simulations (DEM) were used to explain the experimental observations. Finally, the comprehensive mechanical properties, at room temperature, were investigated, experimentally and using DEM, for the different microstructures.

In-situ 3D visualization of composite microstructure during polymer-to-ceramic conversion

DOE PAGES

Larson, Natalie M.; Zok, Frank W.

2017-10-31

One route for producing fiber-reinforced ceramic-matrix composites entails repeated impregnation and pyrolysis of a preceramic polymer in a fiber preform. The process relies crucially on the development of networks of contiguous cracks during pyrolysis, thereby allowing further impregnation to attain nearly-full densification. The present study employs in-situ x-ray computed tomography (XCT) to reveal in three dimensions the evolution of matrix structure during pyrolysis of a SiC-based preceramic polymer to 1200 °C. Observations are used to guide the development of a taxonomy of crack geometries and crack structures and to identify the temporal sequence of their formation. A quantitative analysis ismore » employed to characterize effects of local microstructural dimensions on the conditions required to form cracks of various types. Complementary measurements of gas evolution and mass loss of the preceramic polymer during pyrolysis as well as changes in mass density and Young's modulus provide context for the physical changes revealed by XCT. Furthermore, the findings provide a foundation for future development of physics-based models to guide composite fabrication processes.« less

Effect of Nb on microstructure and yield strength of a high temperature tempered martensitic steel

NASA Astrophysics Data System (ADS)

Wang, Qian; Sun, Yu; Zhang, Chuanyou; Wang, Qingfeng; Zhang, Fucheng

2018-04-01

Martensitic steels based on a composition of 25CrMo47NbVTi with different concentrations of Nb (0.003%–0.060%) were quenched (Q) at 900 °C and tempered (T) at 700 °C to obtain oil country tubular goods (OCTG) with higher yield strength. The precipitation and microstructures were characterized and quantified by optical microscopy (OM), scanning electron microscopy (SEM), transmission electron microscopy (TEM) and x-ray diffraction (XRD). The results show that the increased Nb content led to an enhanced overall precipitation, the rising solution-precipitation temperature, the increased mass or volume fraction of the Nb-containing precipitates, and the decreased average diameter of Nb-containing particles. With the enhanced precipitation of small sized Nb-containing particles, the austenite grain and corresponding martensitic packet and block were evidently refined. In addition, the dislocation density increased slightly with increasing Nb addition. The yield strength was experimentally measured and quantitatively estimated. The findings based on theoretical calculations indicated that as a consequence of intensified strengthening from grain boundaries, precipitates and dislocations, the yield strength was enhanced significantly by Nb addition.

Wave propagation in strain gradient poroelastic medium with microinertia: closed-form and finite element solutions

NASA Astrophysics Data System (ADS)

Rosi, Giuseppe; Scala, Ilaria; Nguyen, Vu-Hieu; Naili, Salah

2017-06-01

This article is about ultrasonic wave propagation in microstructured porous media. The classic Biot's model is enriched using a strain gradient approach to be able to capture high-order effects when the wavelength approaches the characteristic size of the microstructure. In order to reproduce actual transmission/reflection experiments performed on poroelastic samples, and to validate the choice of the model, the computation of the time domain response is necessary, as it allows for a direct comparison with experimental results. For obtaining the time response, we use two strategies: on the one hand we compute the closed form solution by using the Laplace and Fourier transforms techniques; on the other hand we used a finite element method. The results are presented for a transmission/reflection test performed on a poroelastic sample immersed in water. The effects introduced by the strain gradient terms are visible in the time response and in agreement with experimental observations. The results can be exploited in characterization of mechanical properties of poroelastic media by enhancing the reliability of quantitative ultrasound techniques.

Eutectic Experiment Development for Space Processing

NASA Technical Reports Server (NTRS)

Hopkins, R. H.

1972-01-01

A ground base test plan and a specimen evaluation scheme have been developed for the aluminum-copper eutectic solidification experiment to be run in the M518 multipurpose electric furnace during the Skylab mission. Besides thermal and solidification studies a detailed description is given of the quantitative metallographic technique which is appropriate for characterizing eutectic structures. This method should prove a key tool for evaluating specimen microstructure which is the most sensitive indicator of changes produced during solidification. It has been recommended that single grain pre-frozen eutectic specimens be used to simplify microstructural evaluation and to eliminate any porosity in the as-cast eutectic specimens. High purity (99.999%) materials from one supplier should be employed for all experiments. Laboratory studies indicate that porosity occurs in the MRC as-cast eutectic ingots but that this porosity can be eliminated by directional freezing. Chemical analysis shows that the MRC ingots are slightly Al rich and contain about .03% impurity. Because of the impurity content the lower cooldown rate (1.2 C/min) should be used for eutectic freezing if MRC material is used in the M518 furnace.

Strain Characterization and Microstructure Evolution Under Deformation in 2060 Alloy

NASA Astrophysics Data System (ADS)

Jin, X.; Zhang, G. D.; Zhao, Y. F.; Xue, F.

2018-05-01

A new method of DIC combined with EBSD is developed for the characterization of strain and microstructure evolution during bending. The traditional microhardness point and DIC methods are used to study the microstructure evolution in 2060 alloy during bending; the interested area suffers under tensile stress, the microstructure evolution is collected by SEM, EBSD, digital image correlation (DIC) method during bending. The results shows that the DIC method can both realize the strain tensor characterization of the interested area, and can also express the local strain tensor in the micro-area even more. The degree of grain division in the process of deformation is related to the strain in this region; the grains have larger strain of small angle grain boundary (SLGBs), which results in a new micro-organizational structure. The misorientation is smaller with larger strain degree while the misorientation is larger with smaller strain.

On the role of magnetic field intensity for better micro-structural characterization during Barkhausen Noise analysis

NASA Astrophysics Data System (ADS)

Yusufzai, Mohd Zaheer Khan; Vashista, M.

2018-04-01

Barkhausen Noise analysis is a popular and preferred technique for micro-structural characterization. The root mean square value and peak value of Barkhausen Noise burst are important parameters to assess the micro-hardness and residual stress. Barkhausen Noise burst can be enveloped using a curve known as Barkhausen Noise profile. Peak position of profile changes with change in micro-structure. In the present work, raw signal of Barkhausen Noise burst was obtained from Ni based sample at various magnetic field intensity to observe the effect of variation in field intensity on Barkhausen Noise burst. Raw signal was opened using MATLAB to further process for microstructure analysis. Barkhausen Noise analysis parameters such as magnetizing frequency, number of burst, high pass and low pass filter frequency were kept constant and magnetizing field was varied in wide range between 200 Oe to 1200 Oe. The processed profiles of Barkhausen Noise burst obtained at various magnetizing field intensity clearly reveals requirement of optimum magnetic field strength for better characterization of micro-structure.

Ex vivo multiscale quantitation of skin biomechanics in wild-type and genetically-modified mice using multiphoton microscopy

NASA Astrophysics Data System (ADS)

Bancelin, Stéphane; Lynch, Barbara; Bonod-Bidaud, Christelle; Ducourthial, Guillaume; Psilodimitrakopoulos, Sotiris; Dokládal, Petr; Allain, Jean-Marc; Schanne-Klein, Marie-Claire; Ruggiero, Florence

2015-12-01

Soft connective tissues such as skin, tendon or cornea are made of about 90% of extracellular matrix proteins, fibrillar collagens being the major components. Decreased or aberrant collagen synthesis generally results in defective tissue mechanical properties as the classic form of Elhers-Danlos syndrome (cEDS). This connective tissue disorder is caused by mutations in collagen V genes and is mainly characterized by skin hyperextensibility. To investigate the relationship between the microstructure of normal and diseased skins and their macroscopic mechanical properties, we imaged and quantified the microstructure of dermis of ex vivo murine skin biopsies during uniaxial mechanical assay using multiphoton microscopy. We used two genetically-modified mouse lines for collagen V: a mouse model for cEDS harboring a Col5a2 deletion (a.k.a. pN allele) and the transgenic K14-COL5A1 mice which overexpress the human COL5A1 gene in skin. We showed that in normal skin, the collagen fibers continuously align with stretch, generating the observed increase in mechanical stress. Moreover, dermis from both transgenic lines exhibited altered collagen reorganization upon traction, which could be linked to microstructural modifications. These findings show that our multiscale approach provides new crucial information on the biomechanics of dermis that can be extended to all collagen-rich soft tissues.

Evaluation of bone microstructure in CRPS-affected upper limbs by HR-pQCT.

PubMed

Mussawy, Haider; Schmidt, Tobias; Rolvien, Tim; Rüther, Wolfgang; Amling, Michael

2017-01-01

Complex regional pain syndrome (CRPS) is a major complication after trauma, surgery, and/or immobilization of an extremity. The disease often starts with clinical signs of local inflammation and develops into a prolonged phase that is characterized by trophic changes and local osteoporosis and sometimes results in functional impairment of the affected limb. While the pathophysiology of CRPS remains poorly understood, increased local bone resorption plays an undisputed pivotal role. The aim of this retrospective clinical study was to assess the bone microstructure in patients with CRPS. Patients with CRPS type I of the upper limb whose affected and unaffected distal radii were analyzed by high-resolution peripheral quantitative computed tomography (HR-pQCT) were identified retrospectively. The osteology laboratory data and dual-energy X-ray absorptiometry (DXA) images of the left femoral neck and lumbar spine, which were obtained on the same day as HR-pQCT, were extracted from the medical records. Five patients were identified. The CRPS-affected upper limbs had significantly lower trabecular numbers and higher trabecular thicknesses than the unaffected upper limbs. However, the trabecular bone volume to total bone volume and cortical thickness values of the affected and unaffected sides were similar. Trabecular thickness tended to increase with time since disease diagnosis. CRPS associated with significant alterations in the bone microstructure of the affected upper limb that may amplify as the duration of disease increases.

From Solidification Processing to Microstructure to Mechanical Properties: A Multi-scale X-ray Study of an Al-Cu Alloy Sample

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

Tourret, D.; Mertens, J. C. E.; Lieberman, E.

We follow an Al-12 at. pct Cu alloy sample from the liquid state to mechanical failure, using in situ X-ray radiography during directional solidification and tensile testing, as well as three-dimensional computed tomography of the microstructure before and after mechanical testing. The solidification processing stage is simulated with a multi-scale dendritic needle network model, and the micromechanical behavior of the solidified microstructure is simulated using voxelized tomography data and an elasto-viscoplastic fast Fourier transform model. This study demonstrates the feasibility of direct in situ monitoring of a metal alloy microstructure from the liquid processing stage up to its mechanical failure,more » supported by quantitative simulations of microstructure formation and its mechanical behavior.« less

Creep resistance. [of high temperature alloys

NASA Technical Reports Server (NTRS)

Tien, J. K.; Malu, M.; Purushothaman, S.

1976-01-01

High-temperature structural applications usually require creep resistance because some average stress is maintained for prolonged periods. Alloy and microstructural design guidelines for creep resistance are presented through established knowledge on creep behavior and its functional dependences on alloy microstructure. Important considerations related to creep resistance of alloys as well as those that are harmful to high-temperature properties are examined. Although most of the creep models do not predict observed creep behavior quantitatively, they are sophisticated enough to provide alloy or microstructural design guidelines. It is shown that creep-resistant microstructures are usually in conflict with microstructures that improve such other properties as stress rupture ductility. Greater understanding of the effects of environments on creep and stress rupture behavior of materials is necessary before one can optimally design alloys for applications in different environments.

From Solidification Processing to Microstructure to Mechanical Properties: A Multi-scale X-ray Study of an Al-Cu Alloy Sample

DOE PAGES

Tourret, D.; Mertens, J. C. E.; Lieberman, E.; ...

2017-09-13

We follow an Al-12 at. pct Cu alloy sample from the liquid state to mechanical failure, using in situ X-ray radiography during directional solidification and tensile testing, as well as three-dimensional computed tomography of the microstructure before and after mechanical testing. The solidification processing stage is simulated with a multi-scale dendritic needle network model, and the micromechanical behavior of the solidified microstructure is simulated using voxelized tomography data and an elasto-viscoplastic fast Fourier transform model. This study demonstrates the feasibility of direct in situ monitoring of a metal alloy microstructure from the liquid processing stage up to its mechanical failure,more » supported by quantitative simulations of microstructure formation and its mechanical behavior.« less

From Solidification Processing to Microstructure to Mechanical Properties: A Multi-scale X-ray Study of an Al-Cu Alloy Sample

NASA Astrophysics Data System (ADS)

Tourret, D.; Mertens, J. C. E.; Lieberman, E.; Imhoff, S. D.; Gibbs, J. W.; Henderson, K.; Fezzaa, K.; Deriy, A. L.; Sun, T.; Lebensohn, R. A.; Patterson, B. M.; Clarke, A. J.

2017-11-01

We follow an Al-12 at. pct Cu alloy sample from the liquid state to mechanical failure, using in situ X-ray radiography during directional solidification and tensile testing, as well as three-dimensional computed tomography of the microstructure before and after mechanical testing. The solidification processing stage is simulated with a multi-scale dendritic needle network model, and the micromechanical behavior of the solidified microstructure is simulated using voxelized tomography data and an elasto-viscoplastic fast Fourier transform model. This study demonstrates the feasibility of direct in situ monitoring of a metal alloy microstructure from the liquid processing stage up to its mechanical failure, supported by quantitative simulations of microstructure formation and its mechanical behavior.

Measuring and Modeling the Effects of Mechanical Twinning on the Behavior of Magnesium Alloys

NASA Astrophysics Data System (ADS)

Agnew, Sean; Wu, Peidong; Inal, Kaan; El Kadiri, Haitham; Wang, Jian; Tome, Carlos

Our community has learned a great deal about twinning in Mg alloys over the past decade. Some of these things were known qualitatively in prior decades, but we have now developed a proficiency in characterization and computational modeling which permits a quantitative description of these twinning-induced effects over a wide range of strain rates, temperatures, loading conditions, and in a variety of alloy families. These capabilities could only be dreamed of by prior generations. This lecture will review the effects of the main twinning mode, {10.2} extension twinning (e.g., tension-compression yield asymmetry, yield plateau, anisotropy, rapid strain hardening, detwinning, etc.); characterization, primarily by diffraction-based techniques (electron, X-ray, and neutron); and modeling by crystal plasticity-based methods. Strategies to control these effects through microstructure, texture, and alloy design will be proposed. Finally, outstanding questions which merit further research will be highlighted.

Microstructure Characterization Of Lead-Free Solders Depending On Alloy Composition

NASA Astrophysics Data System (ADS)

Panchenko, Iuliana; Mueller, Maik; Wolter, Klaus-Juergen

2010-11-01

Fatigue and crack nucleation in solder joints is basically associated with changes in the microstructure. Therefore the microstructure evolution of SnAgCu solder joints during solidification and subsequent application is an important subject for reliability investigations and physics of failure analysis. The scope of this study is a systematic overview of the as-cast microstructures in small sized lead-free SnAgCu solder spheres after solidification. A total of 32 alloy compositions have been investigated with varying Ag content from 0 to 5 wt.% and varying Cu content from 0 to 1.2 wt.%. The solder spheres had a diameter of approx. 270 μm and were all manufactured under the similar conditions. Subsequent cross-sectioning was carried out in order to analyze the microstructure by optical and electron microscopy as well as Electron Backscatter Diffraction and Energy Dispersive X-ray Spectroscopy. The results allow a comprehensive overview of the dependence of the as-cast microstructure on the solder composition. It is shown that strong changes in microstructure can be caused by small changes in solder composition. In addition, a solidification phenomenon known as cyclic twinning has been found in the samples. Three different microstructures related to that phenomenon will be presented and detailed characterizations of these structures are given in this study. These microstructures differ in their appearance by solidification morphology, phase distribution as well as grain structure and can be described as follows: 1. large dentritic areas of different grain orientations which are characterized by approx. 60° twin boundaries; 2. areas of small β-Sn cells with approx. 60° twin relation and larger intermetallic precipitates; 3. large grains consisting of a β-Sn matrix with very fine intermetallic precipitates and high angle grain boundaries between adjacent grains.

Three-dimensional hydrogen microscopy using a high-energy proton probe

NASA Astrophysics Data System (ADS)

Dollinger, G.; Reichart, P.; Datzmann, G.; Hauptner, A.; Körner, H.-J.

2003-01-01

It is a challenge to measure two-dimensional or three-dimensional (3D) hydrogen profiles on a micrometer scale. Quantitative hydrogen analyses of micrometer resolution are demonstrated utilizing proton-proton scattering at a high-energy proton microprobe. It has more than an-order-of-magnitude better position resolution and in addition higher sensitivity than any other technique for 3D hydrogen analyses. This type of hydrogen imaging opens plenty room to characterize microstructured materials, and semiconductor devices or objects in microbiology. The first hydrogen image obtained with a 10 MeV proton microprobe shows the hydrogen distribution of the microcapillary system being present in the wing of a mayfly and demonstrates the potential of the method.

Single-shot turbo spin echo acquisition for in vivo cardiac diffusion MRI.

PubMed

Edalati, Masoud; Lee, Gregory R; Hui Wang; Taylor, Michael D; Li, Yu Y

2016-08-01

Diffusion MRI offers the ability to noninvasively characterize the microstructure of myocardium tissue and detect disease related pathology in cardiovascular examination. This study investigates the feasibility of in vivo cardiac diffusion MRI under free-breathing condition. A high-speed imaging technique, correlation imaging, is used to enable single-shot turbo spin echo for free-breathing cardiac data acquisition. The obtained in vivo cardiac diffusion-weighted images illustrate robust image quality and minor geometry distortions. The resultant diffusion scalar maps show reliable quantitative values consistent with those previously published in the literature. It is demonstrated that this technique has the potential for in vivo free-breathing cardiac diffusion MRI.

Multiscale microstructural characterization of Sn-rich alloys by three dimensional (3D) X-ray synchrotron tomography and focused ion beam (FIB) tomography

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

Yazzie, K.E.; Williams, J.J.; Phillips, N.C.

2012-08-15

Sn-rich (Pb-free) alloys serve as electrical and mechanical interconnects in electronic packaging. It is critical to quantify the microstructures of Sn-rich alloys to obtain a fundamental understanding of their properties. In this work, the intermetallic precipitates in Sn-3.5Ag and Sn-0.7Cu, and globular lamellae in Sn-37Pb solder joints were visualized and quantified using 3D X-ray synchrotron tomography and focused ion beam (FIB) tomography. 3D reconstructions were analyzed to extract statistics on particle size and spatial distribution. In the Sn-Pb alloy the interconnectivity of Sn-rich and Pb-rich constituents was quantified. It will be shown that multiscale characterization using 3D X-ray and FIBmore » tomography enabled the characterization of the complex morphology, distribution, and statistics of precipitates and contiguous phases over a range of length scales. - Highlights: Black-Right-Pointing-Pointer Multiscale characterization by X-ray synchrotron and focused ion beam tomography. Black-Right-Pointing-Pointer Characterized microstructural features in several Sn-based alloys. Black-Right-Pointing-Pointer Quantified size, fraction, and clustering of microstructural features.« less

Utilization of FEM model for steel microstructure determination

NASA Astrophysics Data System (ADS)

Kešner, A.; Chotěborský, R.; Linda, M.; Hromasová, M.

2018-02-01

Agricultural tools which are used in soil processing, they are worn by abrasive wear mechanism cases by hard minerals particles in the soil. The wear rate is influenced by mechanical characterization of tools material and wear rate is influenced also by soil mineral particle contents. Mechanical properties of steel can be affected by a technology of heat treatment that it leads to a different microstructures. Experimental work how to do it is very expensive and thanks to numerical methods like FEM we can assumed microstructure at low cost but each of numerical model is necessary to be verified. The aim of this work has shown a procedure of prediction microstructure of steel for agricultural tools. The material characterizations of 51CrV4 grade steel were used for numerical simulation like TTT diagram, heat capacity, heat conduction and other physical properties of material. A relationship between predicted microstructure by FEM and real microstructure after heat treatment shows a good correlation.

An Integrated Approach Linking Process to Structural Modeling With Microstructural Characterization for Injections-Molded Long-Fiber Thermoplastics

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

Nguyen, Ba Nghiep; Bapanapalli, Satish K.; Smith, Mark T.

2008-09-01

The objective of our work is to enable the optimum design of lightweight automotive structural components using injection-molded long fiber thermoplastics (LFTs). To this end, an integrated approach that links process modeling to structural analysis with experimental microstructural characterization and validation is developed. First, process models for LFTs are developed and implemented into processing codes (e.g. ORIENT, Moldflow) to predict the microstructure of the as-formed composite (i.e. fiber length and orientation distributions). In parallel, characterization and testing methods are developed to obtain necessary microstructural data to validate process modeling predictions. Second, the predicted LFT composite microstructure is imported into amore » structural finite element analysis by ABAQUS to determine the response of the as-formed composite to given boundary conditions. At this stage, constitutive models accounting for the composite microstructure are developed to predict various types of behaviors (i.e. thermoelastic, viscoelastic, elastic-plastic, damage, fatigue, and impact) of LFTs. Experimental methods are also developed to determine material parameters and to validate constitutive models. Such a process-linked-structural modeling approach allows an LFT composite structure to be designed with confidence through numerical simulations. Some recent results of our collaborative research will be illustrated to show the usefulness and applications of this integrated approach.« less

Interrogating the origin and behavior of magnetic resonance diffusion tensor scalar parameters in the myocardium

NASA Astrophysics Data System (ADS)

Abdullah, Osama Mahmoud

Myocardial microstructure plays an important role in sustaining the orchestrated beating motion of the heart. Several microstructural components, including myocytes and auxiliary cells, extracellular space, and blood vessels provide the infrastructure for normal heart function, including excitation propagation, myocyte contraction, delivery of oxygen and nutrients, and removing byproduct wastes. Cardiac diseases cause deleterious changes to some or all of these microstructural components in the detrimental process of cardiac remodeling. Since heart failure is among the leading causes of death in the world, new and novel tools to noninvasively characterize heart microstructure are needed for monitoring and staging of cardiac disease. In this regards, diffusion magnetic resonance imaging (MRI) provides a promising framework to probe and quantify tissue microstructure without the need for exogenous contrast agent. As diffusion in 3-dimensional space is characterized by the diffusion tensor, MR diffusion tensor imaging (DTI) is being used to noninvasively measure anisotropic diffusion, and thus the magnitude and spatial orientation of microstructural organization of tissues, including the heart. However, even though in vivo cardiac DTI has become more clinically available, to date the origin and behavior of different microstructural components on the measured DTI signal remain to be explicitly specified. The presented studies in this work demonstrate that DTI can be used as a noninvasive and contrast-free imaging modality to characterize myocyte size and density, extracellular collagen content, and the directional magnitude of blood flow. The identified applications are expected to provide metrics to enable physicians to detect, quantify, and stage different microstructural components during progression of cardiac disease.

Investigation of radiation damage tolerance in interface-containing metallic nano structures

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

Greer, Julia R.

The proposed work seeks to conduct a basic study by applying experimental and computational methods to obtain quantitative influence of helium sink strength and proximity on He bubble nucleation and growth in He-irradiated nano-scale metallic structures, and the ensuing deformation mechanisms and mechanical properties. We utilized a combination of nano-scale in-situ tension and compression experiments on low-energy He-irradiated samples combined with site-specific microstructural characterization and modeling efforts. We also investigated the mechanical deformation of nano-architected materials, i.e. nanolattices which are comprised of 3-dimensional interwoven networks of hollow tubes, with the wall thickness in the nanometer range. This systematic approach willmore » provide us with critical information for identifying key factors that govern He bubble nucleation and growth upon irradiation as a function of both sink strength and sink proximity through an experimentally-confirmed physical understanding. As an outgrowth of these efforts, we performed irradiations with self-ions (Ni 2+) on Ni-Al-Zr metallic glass nanolattices to assess their resilience against radiation damage rather than He-ion implantation. We focused our attention on studying individual bcc/fcc interfaces within a single nano structure (nano-pillar or a hollow tube): a single Fe (bcc)-Cu (fcc) boundary per pillar oriented perpendicular to the pillar axes, as well as pure bcc and fcc nano structures. Additional interfaces of interest include bcc/bcc and metal/metallic glass all within a single nano-structure volume. The model material systems are: (1) pure single crystalline Fe and Cu, (2) a single Fe (bcc)-Cu (fcc) boundary per nano structure (3) a single metal–metallic glass, all oriented non-parallel to the loading direction so that their fracture strength can be tested. A nano-fabrication approach, which involves e-beam lithography and templated electroplating, as well as two-photon lithography, was utilized, which enabled precise control of the initial microstructure control. Experimentally determined stress-strain relationships were enhanced by in-situ SEM observations coupled with TEM microstructural characterization of the same samples before and after deformation (irradiated and as-fabricated) and atomistic (MD) modeling. A comprehensive suite of experiments was conducted to quantitatively assess the key parameters for He bubble nucleation and growth by independently varying the sink strength, sink proximity, and He implantation temperature and dose. The implantations were conducted at Sandia and Los Alamos National Labs (CINT). Nano structuress containing He-enriched interfaces and irradiation-damaged microstructure were tested under uniaxial tension to assess embrittlement, resulting boundary strength, and deformation mechanisms. Results of this work helped identify which types of interfaces are particularly resilient against radiation damage.« less

Transfer function concept for ultrasonic characterization of material microstructures

NASA Technical Reports Server (NTRS)

Vary, A.; Kautz, H. E.

1986-01-01

The approach given depends on treating material microstructures as elastomechanical filters that have analytically definable transfer functions. These transfer functions can be defined in terms of the frequency dependence of the ultrasonic attenuation coefficient. The transfer function concept provides a basis for synthesizing expressions that characterize polycrystalline materials relative to microstructural factors such as mean grain size, grain-size distribution functions, and grain boundary energy transmission. Although the approach is nonrigorous, it leads to a rational basis for combining the previously mentioned diverse and fragmented equations for ultrasonic attenuation coefficients.

Advanced imaging of the macrostructure and microstructure of bone

NASA Technical Reports Server (NTRS)

Genant, H. K.; Gordon, C.; Jiang, Y.; Link, T. M.; Hans, D.; Majumdar, S.; Lang, T. F.

2000-01-01

Noninvasive and/or nondestructive techniques are capable of providing more macro- or microstructural information about bone than standard bone densitometry. Although the latter provides important information about osteoporotic fracture risk, numerous studies indicate that bone strength is only partially explained by bone mineral density. Quantitative assessment of macro- and microstructural features may improve our ability to estimate bone strength. The methods available for quantitatively assessing macrostructure include (besides conventional radiographs) quantitative computed tomography (QCT) and volumetric quantitative computed tomography (vQCT). Methods for assessing microstructure of trabecular bone noninvasively and/or nondestructively include high-resolution computed tomography (hrCT), micro-computed tomography (muCT), high-resolution magnetic resonance (hrMR), and micromagnetic resonance (muMR). vQCT, hrCT and hrMR are generally applicable in vivo; muCT and muMR are principally applicable in vitro. Although considerable progress has been made in the noninvasive and/or nondestructive imaging of the macro- and microstructure of bone, considerable challenges and dilemmas remain. From a technical perspective, the balance between spatial resolution versus sampling size, or between signal-to-noise versus radiation dose or acquisition time, needs further consideration, as do the trade-offs between the complexity and expense of equipment and the availability and accessibility of the methods. The relative merits of in vitro imaging and its ultrahigh resolution but invasiveness versus those of in vivo imaging and its modest resolution but noninvasiveness also deserve careful attention. From a clinical perspective, the challenges for bone imaging include balancing the relative advantages of simple bone densitometry against the more complex architectural features of bone or, similarly, the deeper research requirements against the broader clinical needs. The considerable potential biological differences between the peripheral appendicular skeleton and the central axial skeleton have to be addressed further. Finally, the relative merits of these sophisticated imaging techniques have to be weighed with respect to their applications as diagnostic procedures requiring high accuracy or reliability on one hand and their monitoring applications requiring high precision or reproducibility on the other. Copyright 2000 S. Karger AG, Basel.

Modeling the Role of Dislocation Substructure During Class M and Exponential Creep. Revised

NASA Technical Reports Server (NTRS)

Raj, S. V.; Iskovitz, Ilana Seiden; Freed, A. D.

1995-01-01

The different substructures that form in the power-law and exponential creep regimes for single phase crystalline materials under various conditions of stress, temperature and strain are reviewed. The microstructure is correlated both qualitatively and quantitatively with power-law and exponential creep as well as with steady state and non-steady state deformation behavior. These observations suggest that creep is influenced by a complex interaction between several elements of the microstructure, such as dislocations, cells and subgrains. The stability of the creep substructure is examined in both of these creep regimes during stress and temperature change experiments. These observations are rationalized on the basis of a phenomenological model, where normal primary creep is interpreted as a series of constant structure exponential creep rate-stress relationships. The implications of this viewpoint on the magnitude of the stress exponent and steady state behavior are discussed. A theory is developed to predict the macroscopic creep behavior of a single phase material using quantitative microstructural data. In this technique the thermally activated deformation mechanisms proposed by dislocation physics are interlinked with a previously developed multiphase, three-dimensional. dislocation substructure creep model. This procedure leads to several coupled differential equations interrelating macroscopic creep plasticity with microstructural evolution.

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

General Analytical Schemes for the Characterization of Pectin-Based Edible Gelled Systems

PubMed Central

Haghighi, Maryam; Rezaei, Karamatollah

2012-01-01

Pectin-based gelled systems have gained increasing attention for the design of newly developed food products. For this reason, the characterization of such formulas is a necessity in order to present scientific data and to introduce an appropriate finished product to the industry. Various analytical techniques are available for the evaluation of the systems formulated on the basis of pectin and the designed gel. In this paper, general analytical approaches for the characterization of pectin-based gelled systems were categorized into several subsections including physicochemical analysis, visual observation, textural/rheological measurement, microstructural image characterization, and psychorheological evaluation. Three-dimensional trials to assess correlations among microstructure, texture, and taste were also discussed. Practical examples of advanced objective techniques including experimental setups for small and large deformation rheological measurements and microstructural image analysis were presented in more details. PMID:22645484

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

NASA Astrophysics Data System (ADS)

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

2014-08-01

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

Microstructure and inclusion of Ti-6Al-4V fabricated by selective laser melting

NASA Astrophysics Data System (ADS)

Huang, Qianli; Hu, Ningmin; Yang, Xing; Zhang, Ranran; Feng, Qingling

2016-12-01

Selective laser melting (SLM) was used in fabricating the dense part from pre-alloyed Ti-6Al-4V powder. The microstructural evolution and inclusion formation of as-fabricated part were characterized in depth. The microstructure was characterized by features of columnar prior β grains and acicular martensite α'. High density defects such as dislocations and twins can be produced in SLM process. Investigations on the inclusions find out that hard alpha inclusion, amorphous CaO and microcrystalline Al2O3 are three main inclusions formed in SLM. The inclusions formed at some specific sites on melt pool surface. The microstructural evolution and inclusion formation of as-fabricated material are closely related to the SLM process.

Quantitative in vivo assessment of lung microstructure at the alveolar level with hyperpolarized 3He diffusion MRI

NASA Astrophysics Data System (ADS)

Yablonskiy, Dmitriy A.; Sukstanskii, Alexander L.; Leawoods, Jason C.; Gierada, David S.; Bretthorst, G. Larry; Lefrak, Stephen S.; Cooper, Joel D.; Conradi, Mark S.

2002-03-01

The study of lung emphysema dates back to the beginning of the 17th century. Nevertheless, a number of important questions remain unanswered because a quantitative localized characterization of emphysema requires knowledge of lung structure at the alveolar level in the intact living lung. This information is not available from traditional imaging modalities and pulmonary function tests. Herein, we report the first in vivo measurements of lung geometrical parameters at the alveolar level obtained with 3He diffusion MRI in healthy human subjects and patients with severe emphysema. We also provide the first experimental data demonstrating that 3He gas diffusivity in the acinus of human lung is highly anisotropic. A theory of anisotropic diffusion is presented. Our results clearly demonstrate substantial differences between healthy and emphysematous lung at the acinar level and may provide new insights into emphysema progression. The technique offers promise as a clinical tool for early diagnosis of emphysema.

An optimized framework for quantitative magnetization transfer imaging of the cervical spinal cord in vivo

PubMed Central

Grussu, Francesco; Ianus, Andrada; Schneider, Torben; Prados, Ferran; Fairney, James; Ourselin, Sebastien; Alexander, Daniel C.; Cercignani, Mara; Gandini Wheeler‐Kingshott, Claudia A.M.; Samson, Rebecca S.

2017-01-01

Purpose To develop a framework to fully characterize quantitative magnetization transfer indices in the human cervical cord in vivo within a clinically feasible time. Methods A dedicated spinal cord imaging protocol for quantitative magnetization transfer was developed using a reduced field‐of‐view approach with echo planar imaging (EPI) readout. Sequence parameters were optimized based in the Cramer‐Rao‐lower bound. Quantitative model parameters (i.e., bound pool fraction, free and bound pool transverse relaxation times [ T2F, T2B], and forward exchange rate [k FB]) were estimated implementing a numerical model capable of dealing with the novelties of the sequence adopted. The framework was tested on five healthy subjects. Results Cramer‐Rao‐lower bound minimization produces optimal sampling schemes without requiring the establishment of a steady‐state MT effect. The proposed framework allows quantitative voxel‐wise estimation of model parameters at the resolution typically used for spinal cord imaging (i.e. 0.75 × 0.75 × 5 mm3), with a protocol duration of ∼35 min. Quantitative magnetization transfer parametric maps agree with literature values. Whole‐cord mean values are: bound pool fraction = 0.11(±0.01), T2F = 46.5(±1.6) ms, T2B = 11.0(±0.2) µs, and k FB = 1.95(±0.06) Hz. Protocol optimization has a beneficial effect on reproducibility, especially for T2B and k FB. Conclusion The framework developed enables robust characterization of spinal cord microstructure in vivo using qMT. Magn Reson Med 79:2576–2588, 2018. © 2017 The Authors Magnetic Resonance in Medicine published by Wiley Periodicals, Inc. on behalf of International Society for Magnetic Resonance in Medicine. This is an open access article under the terms of the Creative Commons Attribution License, which permits use, distribution and reproduction in any medium, provided the original work is properly cited. PMID:28921614

Optimizing Discharge Capacity of Li-O 2 Batteries by Design of Air-Electrode Porous Structure: Multifidelity Modeling and Optimization

DOE PAGES

Pan, Wenxiao; Yang, Xiu; Bao, Jie; ...

2017-01-01

We develop a new mathematical framework to study the optimal design of air electrode microstructures for lithium-oxygen (Li-O2) batteries. It can eectively reduce the number of expensive experiments for testing dierent air-electrodes, thereby minimizing the cost in the design of Li-O2 batteries. The design parameters to characterize an air-electrode microstructure include the porosity, surface-to-volume ratio, and parameters associated with the pore-size distribution. A surrogate model (also known as response surface) for discharge capacity is rst constructed as a function of these design parameters. The surrogate model is accurate and easy to evaluate such that an optimization can be performed basedmore » on it. In particular, a Gaussian process regression method, co-kriging, is employed due to its accuracy and eciency in predicting high-dimensional responses from a combination of multidelity data. Specically, a small amount of data from high-delity simulations are combined with a large number of data obtained from computationally ecient low-delity simulations. The high-delity simulation is based on a multiscale modeling approach that couples the microscale (pore-scale) and macroscale (device-scale) models. Whereas, the low-delity simulation is based on an empirical macroscale model. The constructed response surface provides quantitative understanding and prediction about how air electrode microstructures aect the discharge performance of Li-O2 batteries. The succeeding sensitivity analysis via Sobol indices and optimization via genetic algorithm ultimately oer a reliable guidance on the optimal design of air electrode microstructures. The proposed mathematical framework can be generalized to investigate other new energy storage techniques and materials.« less

Optimizing Discharge Capacity of Li-O 2 Batteries by Design of Air-Electrode Porous Structure: Multifidelity Modeling and Optimization

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

Pan, Wenxiao; Yang, Xiu; Bao, Jie

We develop a new mathematical framework to study the optimal design of air electrode microstructures for lithium-oxygen (Li-O2) batteries. It can eectively reduce the number of expensive experiments for testing dierent air-electrodes, thereby minimizing the cost in the design of Li-O2 batteries. The design parameters to characterize an air-electrode microstructure include the porosity, surface-to-volume ratio, and parameters associated with the pore-size distribution. A surrogate model (also known as response surface) for discharge capacity is rst constructed as a function of these design parameters. The surrogate model is accurate and easy to evaluate such that an optimization can be performed basedmore » on it. In particular, a Gaussian process regression method, co-kriging, is employed due to its accuracy and eciency in predicting high-dimensional responses from a combination of multidelity data. Specically, a small amount of data from high-delity simulations are combined with a large number of data obtained from computationally ecient low-delity simulations. The high-delity simulation is based on a multiscale modeling approach that couples the microscale (pore-scale) and macroscale (device-scale) models. Whereas, the low-delity simulation is based on an empirical macroscale model. The constructed response surface provides quantitative understanding and prediction about how air electrode microstructures aect the discharge performance of Li-O2 batteries. The succeeding sensitivity analysis via Sobol indices and optimization via genetic algorithm ultimately oer a reliable guidance on the optimal design of air electrode microstructures. The proposed mathematical framework can be generalized to investigate other new energy storage techniques and materials.« less

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

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

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

2014-06-01

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

Microstructural characterization of pressed HMX material sets at differing densities

NASA Astrophysics Data System (ADS)

Molek, C. D.; Welle, E. J.; Wixom, R. R.; Ritchey, M. B.; Samuels, P.; Horie, Y.

2017-01-01

The detonation physics community has embraced the idea that initiation of high explosives (HE) proceeds from an ignition event through subsequent growth to steady detonation. A weakness of all the commonly used ignition and growth models is the microstructural characteristics of the HE are not explicitly incorporated in their ignition and growth terms. This is the case in spite of a demonstrated, but not well-understood, empirical link between particle morphology and initiation of HE. Morphological effects have been parametrically studied in many ways, the majority of efforts focus on establishing a tie between bulk powder metrics and initiation of the pressed beds. More recently, there has been a shift toward characterizing the microstructure of pressed beds in order to understand the underlying mechanisms governing initiation behavior. In this work, we have characterized the microstructures of two HMX classes pressed at three densities using ion bombardment techniques. We find more significant compaction associated with the larger crystalline material - Class 3 - than the smaller fluid energy milled material. The Class 3 material exhibits evidence of crystal cracking. Finally, we discuss this evidence and our attempt to correlate microstructural features to observed changes in continuum level initiation behavior.

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

Characterization of the microstructure of Nb-1wt.%Zr-0.1wt.%C tubes as affected by thermomechanical processing

NASA Technical Reports Server (NTRS)

Uz, Mehmet; Titran, Robert H.

1993-01-01

Microstructure of Nb-1Zr-0.1C tubes were characterized as affected by extrusion temperature of the tube shell and its thermomechanical processing to tubing. Two tube shells of about 40-mm outside diameter (OD) and 25-mm inside diameter (ID) were extruded 8:1 from a vacuum arc-melted ingot at 1900 and 1550 K. Two different OD tubes of approximately 0.36-mm wall thickness were fabricated from each tube shell by a series of 26 cold drawing operations with two in process anneals. The microstructure of tube shells and the tubing before and after a 2-step heat treatment were characterized. Residue extracted chemically from each sample was also analyzed to identify the precipitates. The results concerning the effect of the initial extrusion temperature and subsequent processing on the microstructure of the tubes are presented together with a review of results from similar work on Nb-1Zr-0.1C sheet stock.

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

Vazehrad, S., E-mail: vazehrad@kth.se; Elfsberg, J., E-mail: jessica.elfsberg@scania.com; Diószegi, A., E-mail: attila.dioszegi@jth.hj.se

An investigation on silicon segregation of lamellar, compacted and nodular graphite iron was carried out by applying a selective, immersion color etching and a modified electron microprobe to study the microstructure. The color etched micrographs of the investigated cast irons by revealing the austenite phase have provided data about the chronology and mechanism of microstructure formation. Moreover, electron microprobe has provided two dimensional segregation maps of silicon. A good agreement was found between the segregation profile of silicon in the color etched microstructure and the silicon maps achieved by electron microprobe analysis. However, quantitative silicon investigation was found to bemore » more accurate than color etching results to study the size of the eutectic colonies. - Highlights: • Sensitivity of a color etchant to silicon segregation is quantitatively demonstrated. • Si segregation measurement by EMPA approved the results achieved by color etching. • Color etched micrographs provided data about solidification mechanism in cast irons. • Austenite grain boundaries were identified by measuring the local Si concentration.« less

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

Impact of pore space topology on permeability, cut-off frequencies and validity of wave propagation theories

NASA Astrophysics Data System (ADS)

Sarout, Joël.

2012-04-01

For the first time, a comprehensive and quantitative analysis of the domains of validity of popular wave propagation theories for porous/cracked media is provided. The case of a simple, yet versatile rock microstructure is detailed. The microstructural parameters controlling the applicability of the scattering theories, the effective medium theories, the quasi-static (Gassmann limit) and dynamic (inertial) poroelasticity are analysed in terms of pores/cracks characteristic size, geometry and connectivity. To this end, a new permeability model is devised combining the hydraulic radius and percolation concepts. The predictions of this model are compared to published micromechanical models of permeability for the limiting cases of capillary tubes and penny-shaped cracks. It is also compared to published experimental data on natural rocks in these limiting cases. It explicitly accounts for pore space topology around the percolation threshold and far above it. Thanks to this permeability model, the scattering, squirt-flow and Biot cut-off frequencies are quantitatively compared. This comparison leads to an explicit mapping of the domains of validity of these wave propagation theories as a function of the rock's actual microstructure. How this mapping impacts seismic, geophysical and ultrasonic wave velocity data interpretation is discussed. The methodology demonstrated here and the outcomes of this analysis are meant to constitute a quantitative guide for the selection of the most suitable modelling strategy to be employed for prediction and/or interpretation of rocks elastic properties in laboratory-or field-scale applications when information regarding the rock's microstructure is available.

Process Optimization and Microstructure Characterization of Ti6Al4V Manufactured by Selective Laser Melting

NASA Astrophysics Data System (ADS)

junfeng, Li; zhengying, Wei

2017-11-01

Process optimization and microstructure characterization of Ti6Al4V manufactured by selective laser melting (SLM) were investigated in this article. The relative density of sampled fabricated by SLM is influenced by the main process parameters, including laser power, scan speed and hatch distance. The volume energy density (VED) was defined to account for the combined effect of the main process parameters on the relative density. The results shown that the relative density changed with the change of VED and the optimized process interval is 55˜60J/mm3. Furthermore, compared with laser power, scan speed and hatch distance by taguchi method, it was found that the scan speed had the greatest effect on the relative density. Compared with the microstructure of the cross-section of the specimen at different scanning speeds, it was found that the microstructures at different speeds had similar characteristics, all of them were needle-like martensite distributed in the β matrix, but with the increase of scanning speed, the microstructure is finer and the lower scan speed leads to coarsening of the microstructure.

Microstructural and Defect Characterization in Ceramic Composites Using an Ultrasonic Guided Wave Scan System

NASA Technical Reports Server (NTRS)

Roth, D. J.; Cosgriff, L. M.; Martin, R. E.; Verrilli, M. J.; Bhatt, R. T.

2003-01-01

In this study, an ultrasonic guided wave scan system was used to characterize various microstructural and flaw conditions in two types of ceramic matrix composites, SiC/SiC and C/SiC. Rather than attempting to isolate specific lamb wave modes to use for characterization (as is desired for many types of guided wave inspection problems), the guided wave scan system utilizes the total (multi-mode) ultrasonic response in its inspection analysis. Several time and frequency-domain parameters are calculated from the ultrasonic guided wave signal at each scan location to form images. Microstructural and defect conditions examined include delamination, density variation, cracking, and pre/ post-infiltration. Results are compared with thermographic imaging methods. Although the guided wave technique is commonly used so scanning can be eliminated, applying the technique in the scanning mode allows a more precise characterization of defect conditions.

Preparation and Characterization of New Geopolymer-Epoxy Resin Hybrid Mortars

PubMed Central

Colangelo, Francesco; Roviello, Giuseppina; Ricciotti, Laura; Ferone, Claudio; Cioffi, Raffaele

2013-01-01

The preparation and characterization of metakaolin-based geopolymer mortars containing an organic epoxy resin are presented here for the first time. The specimens have been prepared by means of an innovative in situ co-reticulation process, in mild conditions, of commercial epoxy based organic resins and geopolymeric slurry. In this way, geopolymer based hybrid mortars characterized by a different content of normalized sand (up to 66% in weight) and by a homogeneous dispersion of the organic resin have been obtained. Once hardened, these new materials show improved compressive strength and toughness in respect to both the neat geopolymer and the hybrid pastes since the organic polymer provides a more cohesive microstructure, with a reduced amount of microcracks. The microstructural characterization allows to point out the presence of an Interfacial Transition Zone similar to that observed in cement based mortars and concretes. A correlation between microstructural features and mechanical properties has been studied too. PMID:28811418

Atomistic to continuum modeling of solidification microstructures

DOE PAGES

Karma, Alain; Tourret, Damien

2015-09-26

We summarize recent advances in modeling of solidification microstructures using computational methods that bridge atomistic to continuum scales. We first discuss progress in atomistic modeling of equilibrium and non-equilibrium solid–liquid interface properties influencing microstructure formation, as well as interface coalescence phenomena influencing the late stages of solidification. The latter is relevant in the context of hot tearing reviewed in the article by M. Rappaz in this issue. We then discuss progress to model microstructures on a continuum scale using phase-field methods. We focus on selected examples in which modeling of 3D cellular and dendritic microstructures has been directly linked tomore » experimental observations. Finally, we discuss a recently introduced coarse-grained dendritic needle network approach to simulate the formation of well-developed dendritic microstructures. The approach reliably bridges the well-separated scales traditionally simulated by phase-field and grain structure models, hence opening new avenues for quantitative modeling of complex intra- and inter-grain dynamical interactions on a grain scale.« less

Characterization of 3D interconnected microstructural network in mixed ionic and electronic conducting ceramic composites

NASA Astrophysics Data System (ADS)

Harris, William M.; Brinkman, Kyle S.; Lin, Ye; Su, Dong; Cocco, Alex P.; Nakajo, Arata; Degostin, Matthew B.; Chen-Wiegart, Yu-Chen Karen; Wang, Jun; Chen, Fanglin; Chu, Yong S.; Chiu, Wilson K. S.

2014-04-01

The microstructure and connectivity of the ionic and electronic conductive phases in composite ceramic membranes are directly related to device performance. Transmission electron microscopy (TEM) including chemical mapping combined with X-ray nanotomography (XNT) have been used to characterize the composition and 3-D microstructure of a MIEC composite model system consisting of a Ce0.8Gd0.2O2 (GDC) oxygen ion conductive phase and a CoFe2O4 (CFO) electronic conductive phase. The microstructural data is discussed, including the composition and distribution of an emergent phase which takes the form of isolated and distinct regions. Performance implications are considered with regards to the design of new material systems which evolve under non-equilibrium operating conditions.The microstructure and connectivity of the ionic and electronic conductive phases in composite ceramic membranes are directly related to device performance. Transmission electron microscopy (TEM) including chemical mapping combined with X-ray nanotomography (XNT) have been used to characterize the composition and 3-D microstructure of a MIEC composite model system consisting of a Ce0.8Gd0.2O2 (GDC) oxygen ion conductive phase and a CoFe2O4 (CFO) electronic conductive phase. The microstructural data is discussed, including the composition and distribution of an emergent phase which takes the form of isolated and distinct regions. Performance implications are considered with regards to the design of new material systems which evolve under non-equilibrium operating conditions. Electronic supplementary information (ESI) available. See DOI: 10.1039/c3nr06684c

Research on Formation Mechanism of Dynamic Response and Residual Stress of Sheet Metal Induced by Laser Shock Wave

NASA Astrophysics Data System (ADS)

Feng, Aixin; Cao, Yupeng; Wang, Heng; Zhang, Zhengang

2018-01-01

In order to reveal the quantitative control of the residual stress on the surface of metal materials, the relevant theoretical and experimental studies were carried out to investigate the dynamic response of metal thin plates and the formation mechanism of residual stress induced by laser shock wave. In this paper, the latest research trends on the surface residual stress of laser shock processing technology were elaborated. The main progress of laser shock wave propagation mechanism and dynamic response, laser shock, and surface residual stress were discussed. It is pointed out that the multi-scale characterization of laser and material, surface residual stress and microstructure change is a new hotspot in laser shock strengthening technology.

Is multidetector CT-based bone mineral density and quantitative bone microstructure assessment at the spine still feasible using ultra-low tube current and sparse sampling?

PubMed

Mei, Kai; Kopp, Felix K; Bippus, Rolf; Köhler, Thomas; Schwaiger, Benedikt J; Gersing, Alexandra S; Fehringer, Andreas; Sauter, Andreas; Münzel, Daniela; Pfeiffer, Franz; Rummeny, Ernst J; Kirschke, Jan S; Noël, Peter B; Baum, Thomas

2017-12-01

Osteoporosis diagnosis using multidetector CT (MDCT) is limited to relatively high radiation exposure. We investigated the effect of simulated ultra-low-dose protocols on in-vivo bone mineral density (BMD) and quantitative trabecular bone assessment. Institutional review board approval was obtained. Twelve subjects with osteoporotic vertebral fractures and 12 age- and gender-matched controls undergoing routine thoracic and abdominal MDCT were included (average effective dose: 10 mSv). Ultra-low radiation examinations were achieved by simulating lower tube currents and sparse samplings at 50%, 25% and 10% of the original dose. BMD and trabecular bone parameters were extracted in T10-L5. Except for BMD measurements in sparse sampling data, absolute values of all parameters derived from ultra-low-dose data were significantly different from those derived from original dose images (p<0.05). BMD, apparent bone fraction and trabecular thickness were still consistently lower in subjects with than in those without fractures (p<0.05). In ultra-low-dose scans, BMD and microstructure parameters were able to differentiate subjects with and without vertebral fractures, suggesting osteoporosis diagnosis is feasible. However, absolute values differed from original values. BMD from sparse sampling appeared to be more robust. This dose-dependency of parameters should be considered for future clinical use. • BMD and quantitative bone parameters are assessable in ultra-low-dose in vivo MDCT scans. • Bone mineral density does not change significantly when sparse sampling is applied. • Quantitative trabecular bone microstructure measurements are sensitive to dose reduction. • Osteoporosis subjects could be differentiated even at 10% of original dose. • Radiation exposure should be considered when comparing quantitative bone parameters.

Microstructure Characterization of RERTR Fuel

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

J. Gan; B. D. Miller; D. D. Keiser

2008-09-01

A variety of phases have the potential to develop in the irradiated fuels for the reduced enrichment research test reactor (RERTR) program. To study the radiation stability of these potential phases, three depleted uranium alloys were cast. The phases of interest were identified including U(Si,Al)3, (U,Mo)(Si,Al)3, UMo2Al20, UAl4, and U6Mo4Al43. These alloys were irradiated with 2.6 MeV protons at 200ºC up to 3.0 dpa. The microstructure is characterized using SEM and TEM. Microstructural characterization for an archive dispersion fuel plate (U-7Mo fuel particles in Al-2%Si cladding) was also carried out. TEM sample preparation for the irradiated dispersion fuel has beenmore » developed.« less

Fluorescence microscopy for the characterization of structural integrity

NASA Technical Reports Server (NTRS)

Street, Kenneth W.; Leonhardt, Todd A.

1991-01-01

The absorption characteristics of light and the optical technique of fluorescence microscopy for enhancing metallographic interpretation are presented. Characterization of thermally sprayed coatings by optical microscopy suffers because of the tendency for misidentification of the microstructure produced by metallographic preparation. Gray scale, in bright field microscopy, is frequently the only means of differentiating the actual structural details of porosity, cracking, and debonding of coatings. Fluorescence microscopy is a technique that helps to distinguish the artifacts of metallographic preparation (pullout, cracking, debonding) from the microstructure of the specimen by color contrasting structural differences. Alternative instrumentation and the use of other dye systems are also discussed. The combination of epoxy vacuum infiltration with fluorescence microscopy to verify microstructural defects is an effective means to characterize advanced materials and to assess structural integrity.

Evaluation of bone microstructure in CRPS-affected upper limbs by HR-pQCT

PubMed Central

Mussawy, Haider; Schmidt, Tobias; Rolvien, Tim; Rüther, Wolfgang; Amling, Michael

2017-01-01

Summary Introduction Complex regional pain syndrome (CRPS) is a major complication after trauma, surgery, and/or immobilization of an extremity. The disease often starts with clinical signs of local inflammation and develops into a prolonged phase that is characterized by trophic changes and local osteoporosis and sometimes results in functional impairment of the affected limb. While the pathophysiology of CRPS remains poorly understood, increased local bone resorption plays an undisputed pivotal role. The aim of this retrospective clinical study was to assess the bone microstructure in patients with CRPS. Methods Patients with CRPS type I of the upper limb whose affected and unaffected distal radii were analyzed by high-resolution peripheral quantitative computed tomography (HR-pQCT) were identified retrospectively. The osteology laboratory data and dual-energy X-ray absorptiometry (DXA) images of the left femoral neck and lumbar spine, which were obtained on the same day as HR-pQCT, were extracted from the medical records. Results Five patients were identified. The CRPS-affected upper limbs had significantly lower trabecular numbers and higher trabecular thicknesses than the unaffected upper limbs. However, the trabecular bone volume to total bone volume and cortical thickness values of the affected and unaffected sides were similar. Trabecular thickness tended to increase with time since disease diagnosis. Discussion CRPS associated with significant alterations in the bone microstructure of the affected upper limb that may amplify as the duration of disease increases. PMID:28740526

Differential porosimetry and permeametry for random porous media.

PubMed

Hilfer, R; Lemmer, A

2015-07-01

Accurate determination of geometrical and physical properties of natural porous materials is notoriously difficult. Continuum multiscale modeling has provided carefully calibrated realistic microstructure models of reservoir rocks with floating point accuracy. Previous measurements using synthetic microcomputed tomography (μ-CT) were based on extrapolation of resolution-dependent properties for discrete digitized approximations of the continuum microstructure. This paper reports continuum measurements of volume and specific surface with full floating point precision. It also corrects an incomplete description of rotations in earlier publications. More importantly, the methods of differential permeametry and differential porosimetry are introduced as precision tools. The continuum microstructure chosen to exemplify the methods is a homogeneous, carefully calibrated and characterized model for Fontainebleau sandstone. The sample has been publicly available since 2010 on the worldwide web as a benchmark for methodical studies of correlated random media. High-precision porosimetry gives the volume and internal surface area of the sample with floating point accuracy. Continuum results with floating point precision are compared to discrete approximations. Differential porosities and differential surface area densities allow geometrical fluctuations to be discriminated from discretization effects and numerical noise. Differential porosimetry and Fourier analysis reveal subtle periodic correlations. The findings uncover small oscillatory correlations with a period of roughly 850μm, thus implying that the sample is not strictly stationary. The correlations are attributed to the deposition algorithm that was used to ensure the grain overlap constraint. Differential permeabilities are introduced and studied. Differential porosities and permeabilities provide scale-dependent information on geometry fluctuations, thereby allowing quantitative error estimates.

Microstructure and mechanical properties of hip-consolidated Rene 95 powders. [hot-isostatic pressed nickel-based powder metal

NASA Technical Reports Server (NTRS)

Shimanuki, Y.; Nishino, Y.; Masui, M.; Doi, H.

1980-01-01

The effects of heat-treatments on the microstructure of P/M Rene 95 (a nickel-based powder metal), consolidated by the hot-isostatic pressing (HIP), were examined. The microstructure of as-HIP'd specimen was characterized by highly serrated grain boundaries. Mechanical tests and microstructural observations reveal that the serrated grain boundaries improved ductility at both room and elevated temperatures by retarding crack propagation along grain boundaries.

Microstructural Characterization of the Heat-Affected Zones in Grade 92 Steel Welds: Double-Pass and Multipass Welds

NASA Astrophysics Data System (ADS)

Xu, X.; West, G. D.; Siefert, J. A.; Parker, J. D.; Thomson, R. C.

2018-04-01

The microstructure in the heat-affected zone (HAZ) of multipass welds typical of those used in power plants and made from 9 wt pct chromium martensitic Grade 92 steel is complex. Therefore, there is a need for systematic microstructural investigations to define the different regions of the microstructure across the HAZ of Grade 92 steel welds manufactured using the traditional arc welding processes in order to understand possible failure mechanisms after long-term service. In this study, the microstructure in the HAZ of an as-fabricated two-pass bead-on-plate weld on a parent metal of Grade 92 steel has been systematically investigated and compared to a complex, multipass thick section weldment using an extensive range of electron and ion-microscopy-based techniques. A dilatometer has been used to apply controlled thermal cycles to simulate the microstructures in distinctly different regions in a multipass HAZ using sequential thermal cycles. A wide range of microstructural properties in the simulated materials were characterized and compared with the experimental observations from the weld HAZ. It has been found that the microstructure in the HAZ can be categorized by a combination of sequential thermal cycles experienced by the different zones within the complex weld metal, using the terminology developed for these regions based on a simpler, single-pass bead-on-plate weld, categorized as complete transformation, partial transformation, and overtempered.

Impact toughness of cellulose-fiber reinforced polypropylene : influence of microstructure in laminates and injection molded composites

Treesearch

Craig Clemons; Daniel Caulfield; A. Jeffrey Giacomin

2003-01-01

Unlike their glass reinforced counterparts, microstructure and dynamic fracture behavior of natural fiber-reinforced thermoplastics have hardly been investigated. Here, we characterize the microstructure of cellulose fiber-reinforced polypropylene and determined its effect on impact toughness. Fiber lengths were reduced by one-half when compounded in a high-intensity...

A quantitative and non-contact technique to characterise microstructural variations of skin tissues during photo-damaging process based on Mueller matrix polarimetry.

PubMed

Dong, Yang; He, Honghui; Sheng, Wei; Wu, Jian; Ma, Hui

2017-10-31

Skin tissue consists of collagen and elastic fibres, which are highly susceptible to damage when exposed to ultraviolet radiation (UVR), leading to skin aging and cancer. However, a lack of non-invasive detection methods makes determining the degree of UVR damage to skin in real time difficult. As one of the fundamental features of light, polarization can be used to develop imaging techniques capable of providing structural information about tissues. In particular, Mueller matrix polarimetry is suitable for detecting changes in collagen and elastic fibres. Here, we demonstrate a novel, quantitative, non-contact and in situ technique based on Mueller matrix polarimetry for monitoring the microstructural changes of skin tissues during UVR-induced photo-damaging. We measured the Mueller matrices of nude mouse skin samples, then analysed the transformed parameters to characterise microstructural changes during the skin photo-damaging and self-repairing processes. Comparisons between samples with and without the application of a sunscreen showed that the Mueller matrix-derived parameters are potential indicators for fibrous microstructure in skin tissues. Histological examination and Monte Carlo simulations confirmed the relationship between the Mueller matrix parameters and changes to fibrous structures. This technique paves the way for non-contact evaluation of skin structure in cosmetics and dermatological health.

In vivo correlation between axon diameter and conduction velocity in the human brain.

PubMed

Horowitz, Assaf; Barazany, Daniel; Tavor, Ido; Bernstein, Moran; Yovel, Galit; Assaf, Yaniv

2015-01-01

The understanding of the relationship between structure and function has always characterized biology in general and neurobiology in particular. One such fundamental relationship is that between axon diameter and the axon's conduction velocity (ACV). Measurement of these neuronal properties, however, requires invasive procedures that preclude direct elucidation of this relationship in vivo. Here we demonstrate that diffusion-based MRI is sensitive to the fine microstructural elements of brain wiring and can be used to quantify axon diameter in vivo. Moreover, we demonstrate the in vivo correlation between the diameter of an axon and its conduction velocity in the human brain. Using AxCaliber, a novel magnetic resonance imaging technique that enables us to estimate in vivo axon diameter distribution (ADD) and by measuring the interhemispheric transfer time (IHTT) by electroencephalography, we found significant linear correlation, across a cohort of subjects, between brain microstructure morphology (ADD) and its physiology (ACV) in the tactile and visual sensory domains. The ability to make a quantitative assessment of a fundamental physiological property in the human brain from in vivo measurements of ADD may shed new light on neurological processes occurring in neuroplasticity as well as in neurological disorders and neurodegenerative diseases.

Hydrogen-enhanced-plasticity mediated decohesion for hydrogen-induced intergranular and ``quasi-cleavage'' fracture of lath martensitic steels

NASA Astrophysics Data System (ADS)

Nagao, Akihide; Dadfarnia, Mohsen; Somerday, Brian P.; Sofronis, Petros; Ritchie, Robert O.

2018-03-01

Hydrogen embrittlement of lath martenistic steels is characterized by intergranular and "quasi-cleavage" transgranular fracture. Recent transmission electron microscopy (TEM) analyses (Nagao et al., 2012a, 2014a, 2014b, 2014c) of samples lifted from beneath fracture surfaces through focused ion beam machining (FIB) revealed a failure mechanism that can be termed hydrogen-enhanced-plasticity mediated decohesion. Fracture occurs by the synergistic action of the hydrogen-enhanced localized plasticity and decohesion. In particular, intergranular cracking takes place by dislocation pile-ups impinging on prior austenite grain boundaries and "quasi-cleavage" is the case when dislocation pile-ups impinge on block boundaries. These high-angle boundaries, which have already weakened by the presence of hydrogen, debond by the pile-up stresses. The micromechanical model of Novak et al. (2010) is used to quantitatively describe and predict the hydrogen-induced failure of these steels. The model predictions verify that introduction of nanosized (Ti,Mo)C precipitates in the steel microstructure enhances the resistance to hydrogen embrittlement. The results are used to discuss microstructural designs that are less susceptible to hydrogen-induced failure in systems with fixed hydrogen content (closed systems).

Structural integrity of additive materials: Microstructure, fatigue behavior, and surface processing

NASA Astrophysics Data System (ADS)

Book, Todd A.

Although Additive Manufacturing (AM) offers numerous performance advantages over existing methods, AM structures are not being utilized for critical aerospace and mechanical applications due to uncertainties in their structural integrity as a result of the microstructural variations and defects arising from the AM process itself. Two of these uncertainties are the observed scatter in tensile strength and fatigue lives of direct metal laser sintering (DMLS) parts. With strain localization a precursor for material failure, this research seeks to explore the impact of microstructural variations in DMLS produced materials on strain localization. The first part of this research explores the role of the microstructure in strain localization of DMLS produced IN718 and Ti6Al4V specimens (as-built and post-processed) through the characterization of the linkage between microstructural variations, and the accumulation of plastic strain during monotonic and low cycle fatigue loading. The second part of this research explores the feasibility for the application of select surface processing techniques in-situ during the DMLS build process to alter the microstructure in AlSi10Mg to reduce strain localization and improve material cohesion. This study is based on utilizing experimental observations through the employment of advanced material characterization techniques such as digital image correlation to illustrate the impacts of DMLS microstructural variation.

A multimodal MRI approach to identify and characterize microstructural brain changes in neuropsychiatric systemic lupus erythematosus.

PubMed

Ercan, Ece; Ingo, Carson; Tritanon, Oranan; Magro-Checa, Cesar; Smith, Alex; Smith, Seth; Huizinga, Tom; van Buchem, Mark A; Ronen, Itamar

2015-01-01

Systemic lupus erythematosus (SLE) is an autoimmune disease with multi-organ involvement and results in neurological and psychiatric (NP) symptoms in up to 40% of the patients. To date, the diagnosis of neuropsychiatric systemic lupus erythematosus (NPSLE) poses a challenge due to the lack of neuroradiological gold standards. In this study, we aimed to better localize and characterize normal appearing white matter (NAWM) changes in NPSLE by combining data from two quantitative MRI techniques, diffusion tensor imaging (DTI) and magnetization transfer imaging (MTI). 9 active NPSLE patients (37 ± 13 years, all females), 9 SLE patients without NP symptoms (44 ± 11 years, all females), and 14 healthy controls (HC) (40 ± 9 years, all females) were included in the study. MTI, DTI and fluid attenuated inversion recovery (FLAIR) images were collected from all subjects on a 3 T MRI scanner. Magnetization transfer ratio (MTR), mean diffusivity (MD), fractional anisotropy (FA), radial diffusivity (RD), axial diffusivity (AD) maps and white matter lesion maps based on the FLAIR images were created for each subject. MTR and DTI data were then co-analyzed using tract-based spatial statistics and a cumulative lesion map to exclude lesions. Significantly lower MTR and FA and significantly higher AD, RD and MD were found in NPSLE compared to HC in NAWM regions. The differences in DTI measures and in MTR, however, were only moderately co-localized. Additionally, significant differences in DTI measures, but not in MTR, were found between NPSLE and SLE patients, suggesting that the underlying microstructural changes detected by MD are linked to the onset of NPSLE. The co-analysis of the anatomical distribution of MTI and DTI measures can potentially improve the diagnosis of NPSLE and contribute to the understanding of the underlying microstructural damage.

Quantitative Characterization of the Microstructure and Transport Properties of Biopolymer Networks

PubMed Central

Jiao, Yang; Torquato, Salvatore

2012-01-01

Biopolymer networks are of fundamental importance to many biological processes in normal and tumorous tissues. In this paper, we employ the panoply of theoretical and simulation techniques developed for characterizing heterogeneous materials to quantify the microstructure and effective diffusive transport properties (diffusion coefficient De and mean survival time τ) of collagen type I networks at various collagen concentrations. In particular, we compute the pore-size probability density function P(δ) for the networks and present a variety of analytical estimates of the effective diffusion coefficient De for finite-sized diffusing particles, including the low-density approximation, the Ogston approximation, and the Torquato approximation. The Hashin-Strikman upper bound on the effective diffusion coefficient De and the pore-size lower bound on the mean survival time τ are used as benchmarks to test our analytical approximations and numerical results. Moreover, we generalize the efficient first-passage-time techniques for Brownian-motion simulations in suspensions of spheres to the case of fiber networks and compute the associated effective diffusion coefficient De as well as the mean survival time τ, which is related to nuclear magnetic resonance (NMR) relaxation times. Our numerical results for De are in excellent agreement with analytical results for simple network microstructures, such as periodic arrays of parallel cylinders. Specifically, the Torquato approximation provides the most accurate estimates of De for all collagen concentrations among all of the analytical approximations we consider. We formulate a universal curve for τ for the networks at different collagen concentrations, extending the work of Yeong and Torquato [J. Chem. Phys. 106, 8814 (1997)]. We apply rigorous cross-property relations to estimate the effective bulk modulus of collagen networks from a knowledge of the effective diffusion coefficient computed here. The use of cross-property relations to link other physical properties to the transport properties of collagen networks is also discussed. PMID:22683739

Probing sub-alveolar length scales with hyperpolarized-gas diffusion NMR

NASA Astrophysics Data System (ADS)

Miller, Wilson; Carl, Michael; Mooney, Karen; Mugler, John; Cates, Gordon

2009-05-01

Diffusion MRI of the lung is a promising technique for detecting alterations of normal lung microstructure in diseases such as emphysema. The length scale being probed using this technique is related to the time scale over which the helium-3 or xenon-129 diffusion is observed. We have developed new MR pulse sequence methods for making diffusivity measurements at sub-millisecond diffusion times, allowing one to probe smaller length scales than previously possible in-vivo, and opening the possibility of making quantitative measurements of the ratio of surface area to volume (S/V) in the lung airspaces. The quantitative accuracy of simulated and experimental measurements in microstructure phantoms will be discussed, and preliminary in-vivo results will be presented.

Application of Image Analysis for Characterization of Spatial Arrangements of Features in Microstructure

NASA Technical Reports Server (NTRS)

Louis, Pascal; Gokhale, Arun M.

1995-01-01

A number of microstructural processes are sensitive to the spatial arrangements of features in microstructure. However, very little attention has been given in the past to the experimental measurements of the descriptors of microstructural distance distributions due to the lack of practically feasible methods. We present a digital image analysis procedure to estimate the micro-structural distance distributions. The application of the technique is demonstrated via estimation of K function, radial distribution function, and nearest-neighbor distribution function of hollow spherical carbon particulates in a polymer matrix composite, observed in a metallographic section.

Application of X-ray micro-CT for micro-structural characterization of APCVD deposited SiC coatings on graphite conduit.

PubMed

Agrawal, A K; Sarkar, P S; Singh, B; Kashyap, Y S; Rao, P T; Sinha, A

2016-02-01

SiC coatings are commonly used as oxidation protective materials in high-temperature applications. The operational performance of the coating depends on its microstructure and uniformity. This study explores the feasibility of applying tabletop X-ray micro-CT for the micro-structural characterization of SiC coating. The coating is deposited over the internal surface of pipe structured graphite fuel tube, which is a prototype of potential components of compact high-temperature reactor (CHTR). The coating is deposited using atmospheric pressure chemical vapor deposition (APCVD) and properties such as morphology, porosity, thickness variation are evaluated. Micro-structural differences in the coating caused by substrate distance from precursor inlet in a CVD reactor are also studied. The study finds micro-CT a potential tool for characterization of SiC coating during its future course of engineering. We show that depletion of reactants at larger distances causes development of larger pores in the coating, which affects its morphology, density and thickness. Copyright © 2015 Elsevier Ltd. All rights reserved.

Microstructure Characterization and Wear-Resistant Properties Evaluation of an Intermetallic Composite in Ni-Mo-Si System.

PubMed

Huang, Boyuan; Song, Chunyan; Liu, Yang; Gui, Yongliang

2017-02-04

Intermetallic compounds have been studied for their potential application as structural wear materials or coatings on engineering steels. In the present work, a newly designed intermetallic composite in a Ni-Mo-Si system was fabricated by arc-melting process with commercially pure metal powders as starting materials. The chemical composition of this intermetallic composite is 45Ni-40Mo-15Si (at %), selected according to the ternary alloy diagram. The microstructure was characterized using optical microscopy (OM), scanning electron microscopy (SEM), X-ray diffraction (XRD), and energy dispersive spectroscopy (EDS), and the wear-resistant properties at room temperature were evaluated under different wear test conditions. Microstructure characterization showed that the composite has a dense and uniform microstructure. XRD results showed that the intermetallic composite is constituted by a binary intermetallic compound NiMo and a ternary Mo₂Ni₃Si metal silicide phase. Wear test results indicated that the intermetallic composite has an excellent wear-resistance at room-temperature, which is attributed to the high hardness and strong atomic bonding of constituent phases NiMo and Mo₂Ni₃Si.

Characterization of sputtered iridium oxide thin films on planar and laser micro-structured platinum thin film surfaces for neural stimulation applications

NASA Astrophysics Data System (ADS)

Thanawala, Sachin

Electrical stimulation of neurons provides promising results for treatment of a number of diseases and for restoration of lost function. Clinical examples include retinal stimulation for treatment of blindness and cochlear implants for deafness and deep brain stimulation for treatment of Parkinsons disease. A wide variety of materials have been tested for fabrication of electrodes for neural stimulation applications, some of which are platinum and its alloys, titanium nitride, and iridium oxide. In this study iridium oxide thin films were sputtered onto laser micro-structured platinum thin films by pulsed-DC reactive sputtering of iridium metal in oxygen-containing atmosphere, to obtain high charge capacity coatings for neural stimulation applications. The micro-structuring of platinum films was achieved by a pulsed-laser-based technique (KrF excimer laser emitting at lambda=248nm). The surface morphology of the micro-structured films was studied using different surface characterization techniques. In-vitro biocompatibility of these laser micro-structured films coated with iridium oxide thin films was evaluated using cortical neurons isolated from rat embryo brain. Characterization of these laser micro-structured films coated with iridium oxide, by cyclic voltammetry and impedance spectroscopy has revealed a considerable decrease in impedance and increase in charge capacity. A comparison between amorphous and crystalline iridium oxide thin films as electrode materials indicated that amorphous iridium oxide has significantly higher charge capacity and lower impedance making it preferable material for neural stimulation application. Our biocompatibility studies show that neural cells can grow and differentiate successfully on our laser micro-structured films coated with iridium oxide. This indicates that reactively sputtered iridium oxide (SIROF) is biocompatible.

Peculiar Features of Microstructure Formation and Microhardness Variations During Torsional Straining of Tantalum Specimens in Bridgman Anvils

NASA Astrophysics Data System (ADS)

Ditenberg, I. A.; Tymentsev, A. N.; Korznikov, A. V.

2015-04-01

Using the method of transmission electron microscopy, peculiar features of evolution of microstructure and variations in microhardness of Та are investigated under torsional loading in the Bridgman anvil as a function of plastic deformation at room temperature. A quantitative examination of grain and defect's structure of the material under study and the values of local internal stresses is performed in different loading stages. The mechanisms of formation of submicrocrystalline and nanostructured states are analyzed and so is the microstructure variation as a function of the defect-structure characteristics, strain level, and spacing from the axis of torsion.

Modeling of non-uniform spatial arrangement of fibers in a ceramic matrix composite

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

Yang, S.; Tewari, A.; Gokhale, A.M.

In the unidirectional fiber reinforced composites, the spatial agreement of fibers is often non-uniform. These non-uniformities are linked to the processing conditions, and they affect the properties of the composite. In this contribution, a recently developed digital image analysis technique is used to quantify the non-uniform spatial arrangement of Nicalon fibers in a ceramic matrix composite (CMC). These quantitative data are utilized to develop a six parameter computer simulated microstructure model that is statistically equivalent to the non-uniform microstructure of the CMC. The simulated microstructure can be utilized as a RVE for the micro-mechanical modeling studies.

Diffusion Lung Imaging with Hyperpolarized Gas MRI

PubMed Central

Yablonskiy, Dmitriy A; Sukstanskii, Alexander L; Quirk, James D

2015-01-01

Lung imaging using conventional 1H MRI presents great challenges due to low density of lung tissue, lung motion and very fast lung tissue transverse relaxation (typical T2* is about 1-2 ms). MRI with hyperpolarized gases (3He and 129Xe) provides a valuable alternative due to a very strong signal originated from inhaled gas residing in the lung airspaces and relatively slow gas T2* relaxation (typical T2* is about 20-30 ms). Though in vivo human experiments should be done very fast – usually during a single breath-hold. In this review we describe the recent developments in diffusion lung MRI with hyperpolarized gases. We show that a combination of modeling results of gas diffusion in lung airspaces and diffusion measurements with variable diffusion-sensitizing gradients allows extracting quantitative information on the lung microstructure at the alveolar level. This approach, called in vivo lung morphometry, allows from a less than 15-second MRI scan, providing quantitative values and spatial distributions of the same physiological parameters as are measured by means of the “standard” invasive stereology (mean linear intercept, surface-to-volume ratio, density of alveoli, etc.). Besides, the approach makes it possible to evaluate some advanced Weibel parameters characterizing lung microstructure - average radii of alveolar sacs and ducts, as well as the depth of their alveolar sleeves. Such measurements, providing in vivo information on the integrity of pulmonary acinar airways and their changes in different diseases, are of great importance and interest to a broad range of physiologists and clinicians. We also discuss a new type of experiments that are based on the in vivo lung morphometry technique combined with quantitative CT measurements as well as with the Gradient Echo MRI measurements of hyperpolarized gas transverse relaxation in the lung airspaces. Such experiments provide additional information on the blood vessel volume fraction, specific gas volume, the length of acinar airways, and allows evaluation of lung parenchymal and non-parenchymal tissue. PMID:26676342

Micro-structural study and Rietveld analysis of fast reactor fuels: U-Mo fuels

NASA Astrophysics Data System (ADS)

Chakraborty, S.; Choudhuri, G.; Banerjee, J.; Agarwal, Renu; Khan, K. B.; Kumar, Arun

2015-12-01

U-Mo alloys are the candidate fuels for both research reactors and fast breeder reactors. In-reactor performance of the fuel depends on the microstructural stability and thermal properties of the fuel. To improve the fuel performance, alloying elements viz. Zr, Mo, Nb, Ti and fissium are added in the fuel. The first reactor fuels are normally prepared by injection casting. The objective of this work is to compare microstructure, phase-fields and hardness of as-cast four different U-Mo alloy (2, 5, 10 and 33 at.% Mo) fuels with the equilibrium microstructure of the alloys. Scanning electron microscope with energy dispersive spectrometer and optical microscope have been used to characterize the morphology of the as-cast and annealed alloys. The monoclinic α'' phase in as-cast U-10 at.% Mo alloy has been characterized through Rietveld analysis. A comparison of metallographic and Rietveld analysis of as-cast (dendritic microstructure) and annealed U-33 at.% Mo alloy, corresponding to intermetallic compound, has been reported here for the first time. This study will provide in depth understanding of microstructural and phase evolution of U-Mo alloys as fast reactor fuel.

Representation and Reconstruction of Three-dimensional Microstructures in Ni-based Superalloys

DTIC Science & Technology

2010-12-20

Materiala, 56, pp. 427-437 (2009); • Application of joint histogram and mutual information to registration and data fusion problems in serial...sectioning data sets and synthetically generated microstructures. The method is easy to use, and allows for a quantitative description of shapes. Further...following objectives were achieved: • we have successfully applied 3-D moment invariant analysis to several experimental data sets; • we have extended 2-D

Utility of charge-transfer complexation for the assessment of macrocyclic polyethers: Spectroscopic, thermal and surface morphology characteristics of two highly crown ethers complexed with acido acceptors

NASA Astrophysics Data System (ADS)

Refat, Moamen S.; Adam, Abdel Majid A.; Saad, Hosam A.

2015-04-01

The study of the complexing ability of macrocyclic compounds to organic and inorganic substances is of great interest. The aim of this work is to provide basic data that can be used to the assessment of macrocyclic crown ethers quantitatively based on charge-transfer (CT) complexation. This goal was achieved by preparing CT complexes of two interesting mixed nitrogen-oxygen crown ethers with acido acceptors (chloranilic and picric acid), which were fully structurally characterized. The crown ethers are 4,7,13,16,21,24-hexaoxa-1,10-diazabicyclo[8.8.8]hexacosane (HDHC) and 1,4,10-trioxa-7,13-diaza-cyclopentadecane (TDPD). The obtained complexes were structurally characterized via elemental analysis, IR, Raman, 1H NMR, and UV-visible spectroscopy. Thermal properties of these complexes were also studied, and their kinetic thermodynamic parameters were calculated. Furthermore, the microstructure properties of these complexes have also been investigated using X-ray diffraction (XRD) and scanning electron microscope (SEM).

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.

Mapping White Matter Microstructure in the One Month Human Brain.

PubMed

Dean, D C; Planalp, E M; Wooten, W; Adluru, N; Kecskemeti, S R; Frye, C; Schmidt, C K; Schmidt, N L; Styner, M A; Goldsmith, H H; Davidson, R J; Alexander, A L

2017-08-29

White matter microstructure, essential for efficient and coordinated transmission of neural communications, undergoes pronounced development during the first years of life, while deviations to this neurodevelopmental trajectory likely result in alterations of brain connectivity relevant to behavior. Hence, systematic evaluation of white matter microstructure in the normative brain is critical for a neuroscientific approach to both typical and atypical early behavioral development. However, few studies have examined the infant brain in detail, particularly in infants under 3 months of age. Here, we utilize quantitative techniques of diffusion tensor imaging and neurite orientation dispersion and density imaging to investigate neonatal white matter microstructure in 104 infants. An optimized multiple b-value diffusion protocol was developed to allow for successful acquisition during non-sedated sleep. Associations between white matter microstructure measures and gestation corrected age, regional asymmetries, infant sex, as well as newborn growth measures were assessed. Results highlight changes of white matter microstructure during the earliest periods of development and demonstrate differential timing of developing regions and regional asymmetries. Our results contribute to a growing body of research investigating the neurobiological changes associated with neurodevelopment and suggest that characteristics of white matter microstructure are already underway in the weeks immediately following birth.

In Situ Atom Probe Deintercalation of Lithium-Manganese-Oxide.

PubMed

Pfeiffer, Björn; Maier, Johannes; Arlt, Jonas; Nowak, Carsten

2017-04-01

Atom probe tomography is routinely used for the characterization of materials microstructures, usually assuming that the microstructure is unaltered by the analysis. When analyzing ionic conductors, however, gradients in the chemical potential and the electric field penetrating dielectric atom probe specimens can cause significant ionic mobility. Although ionic mobility is undesirable when aiming for materials characterization, it offers a strategy to manipulate materials directly in situ in the atom probe. Here, we present experimental results on the analysis of the ionic conductor lithium-manganese-oxide with different atom probe techniques. We demonstrate that, at a temperature of 30 K, characterization of the materials microstructure is possible without measurable Li mobility. Also, we show that at 298 K the material can be deintercalated, in situ in the atom probe, without changing the manganese-oxide host structure. Combining in situ atom probe deintercalation and subsequent conventional characterization, we demonstrate a new methodological approach to study ionic conductors even in early stages of deintercalation.

Simulation of metal additive manufacturing microstructures using kinetic Monte Carlo

DOE PAGES

Rodgers, Theron M.; Madison, Jonathan D.; Tikare, Veena

2017-04-19

Additive manufacturing (AM) is of tremendous interest given its ability to realize complex, non-traditional geometries in engineered structural materials. But, microstructures generated from AM processes can be equally, if not more, complex than their conventionally processed counterparts. While some microstructural features observed in AM may also occur in more traditional solidification processes, the introduction of spatially and temporally mobile heat sources can result in significant microstructural heterogeneity. While grain size and shape in metal AM structures are understood to be highly dependent on both local and global temperature profiles, the exact form of this relation is not well understood. Wemore » implement an idealized molten zone and temperature-dependent grain boundary mobility in a kinetic Monte Carlo model to predict three-dimensional grain structure in additively manufactured metals. In order to demonstrate the flexibility of the model, synthetic microstructures are generated under conditions mimicking relatively diverse experimental results present in the literature. Simulated microstructures are then qualitatively and quantitatively compared to their experimental complements and are shown to be in good agreement.« less

Fast and robust method for the determination of microstructure and composition in butadiene, styrene-butadiene, and isoprene rubber by near-infrared spectroscopy.

PubMed

Vilmin, Franck; Dussap, Claude; Coste, Nathalie

2006-06-01

In the tire industry, synthetic styrene-butadiene rubber (SBR), butadiene rubber (BR), and isoprene rubber (IR) elastomers are essential for conferring to the product its properties of grip and rolling resistance. Their physical properties depend on their chemical composition, i. e., their microstructure and styrene content, which must be accurately controlled. This paper describes a fast, robust, and highly reproducible near-infrared analytical method for the quantitative determination of the microstructure and styrene content. The quantitative models are calculated with the help of pure spectral profiles estimated from a partial least squares (PLS) regression, using (13)C nuclear magnetic resonance (NMR) as the reference method. This versatile approach allows the models to be applied over a large range of compositions, from a single BR to an SBR-IR blend. The resulting quantitative predictions are independent of the sample path length. As a consequence, the sample preparation is solvent free and simplified with a very fast (five minutes) hot filming step of a bulk polymer piece. No precise thickness control is required. Thus, the operator effect becomes negligible and the method is easily transferable. The root mean square error of prediction, depending on the rubber composition, is between 0.7% and 1.3%. The reproducibility standard error is less than 0.2% in every case.

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.

Transport properties of porous media from the microstructure

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

Torquato, S.

The determination of the effective transport properties of a random porous medium remains a challenging area of research because the properties depend on the microstructure in a highly complex fashion. This paper reviews recent theoretical and experimental progress that we have made on various aspects of this problem. A unified approach is taken to characterize the microstructure and the seemingly disparate properties of the medium.

Predicting mesoscale microstructural evolution in electron beam welding

DOE PAGES

Rodgers, Theron M.; Madison, Jonathan D.; Tikare, Veena; ...

2016-03-16

Using the kinetic Monte Carlo simulator, Stochastic Parallel PARticle Kinetic Simulator, from Sandia National Laboratories, a user routine has been developed to simulate mesoscale predictions of a grain structure near a moving heat source. Here, we demonstrate the use of this user routine to produce voxelized, synthetic, three-dimensional microstructures for electron-beam welding by comparing them with experimentally produced microstructures. When simulation input parameters are matched to experimental process parameters, qualitative and quantitative agreement for both grain size and grain morphology are achieved. The method is capable of simulating both single- and multipass welds. As a result, the simulations provide anmore » opportunity for not only accelerated design but also the integration of simulation and experiments in design such that simulations can receive parameter bounds from experiments and, in turn, provide predictions of a resultant microstructure.« less

Microstructural and mechanical characterization of scarred vocal folds.

PubMed

Heris, Hossein K; Miri, Amir K; Ghattamaneni, Nageswara R; Li, Nicole Y K; Thibeault, Susan L; Wiseman, Paul W; Mongeau, Luc

2015-02-26

The goal of this study was to characterize the vocal folds microstructure and elasticity using nonlinear laser scanning microscopy and atomic force microscopy-based indentation, respectively. As a pilot study, the vocal folds of fourteen rats were unilaterally injured by full removal of lamina propria; the uninjured folds of the same animals served as controls. The area fraction of collagen fibrils was found to be greater in scarred tissues two months after injury than the uninjured controls. A novel mathematical model was also proposed to relate collagen concentration and tissue bulk modulus. This work presents a first step towards systematic investigation of microstructural and mechanical characteristics in scarred vocal fold tissue. Copyright © 2015 Elsevier Ltd. All rights reserved.

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

Zhang, Jiali, E-mail: j.zhang@mpie.de; Morsdorf, Lutz, E-mail: l.morsdorf@mpie.de; Tasan, Cemal Cem, E-mail: c.tasan@mpie.de

In-situ scanning electron microscopy observations of the microstructure evolution during heat treatments are increasingly demanded due to the growing number of alloys with complex microstructures. Post-mortem characterization of the as-processed microstructures rarely provides sufficient insight on the exact route of the microstructure formation. On the other hand, in-situ SEM approaches are often limited due to the arising challenges upon using an in-situ heating setup, e.g. in (i) employing different detectors, (ii) preventing specimen surface degradation, or (iii) controlling and measuring the temperature precisely. Here, we explore and expand the capabilities of the “mid-way” solution by step-wise microstructure tracking, ex-situ, atmore » selected steps of heat treatment. This approach circumvents the limitations above, as it involves an atmosphere and temperature well-controlled dilatometer, and high resolution microstructure characterization (using electron channeling contrast imaging, electron backscatter diffraction, atom probe tomography, etc.). We demonstrate the capabilities of this approach by focusing on three cases: (i) nano-scale carbide precipitation during low-temperature tempering of martensitic steels, (ii) formation of transformation-induced geometrically necessary dislocations in a dual-phase steel during intercritical annealing, and (iii) the partial recrystallization of a metastable β-Ti alloy. - Highlights: • A multi-probe method to track microstructures during heat treatment is developed. • It enables the analysis of various complex phenomena, even those at atomistic scale. • It circumvents some of the free surface effects of classical in-situ experiments.« less

Effect of Microstructural Parameters on the Relative Densities of Metal Foams

NASA Technical Reports Server (NTRS)

Raj, S. V.; Kerr, Jacob A.

2010-01-01

A detailed quantitative microstructural analyses of primarily open cell FeCrAlY and 314 stainless steel metal foams with different relative densities and pores per inch (p.p.i.) were undertaken in the present investigation to determine the effect of microstructural parameters on the relative densities of metal foams. Several elements of the microstructure, such as longitudinal and transverse cell sizes, cell areas and perimeters, ligament dimensions, cell shapes and volume fractions of closed and open cells, were measured. The cross-sections of the foam ligaments showed a large number of shrinkage cavities, and their circularity factors and average sizes were determined. The volume fractions of closed cells increased linearly with increasing relative density. In contrast, the volume fractions of the open cells and ligaments decreased with increasing relative density. The relative densities and p.p.i. were not significantly dependent on cell size, cell perimeter and ligament dimensions within the limits of experimental scatter. A phenomenological model is proposed to rationalize the present microstructural observations.

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

Rodgers, Theron M.; Madison, Jonathan D.; Tikare, Veena

Additive manufacturing (AM) is of tremendous interest given its ability to realize complex, non-traditional geometries in engineered structural materials. But, microstructures generated from AM processes can be equally, if not more, complex than their conventionally processed counterparts. While some microstructural features observed in AM may also occur in more traditional solidification processes, the introduction of spatially and temporally mobile heat sources can result in significant microstructural heterogeneity. While grain size and shape in metal AM structures are understood to be highly dependent on both local and global temperature profiles, the exact form of this relation is not well understood. Wemore » implement an idealized molten zone and temperature-dependent grain boundary mobility in a kinetic Monte Carlo model to predict three-dimensional grain structure in additively manufactured metals. In order to demonstrate the flexibility of the model, synthetic microstructures are generated under conditions mimicking relatively diverse experimental results present in the literature. Simulated microstructures are then qualitatively and quantitatively compared to their experimental complements and are shown to be in good agreement.« less

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.

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

Antisite Defects in Layered Multiferroic CuCr 0.9In 0.1P 2S 6

DOE PAGES

He, Qian; Belianinov, Alex; Dziaugys, Andrius; ...

2015-10-06

The CuCr 1-xIn xP 2S 6 system represents a large family of metal chalcogenophosphates that are unique and promising candidates for 2D materials with functionalities such as ferroelectricity. We carried out detailed microstructural and chemical characterization of these compounds using aberration-corrected STEM, in order to understand the origin of these different ordering phenomena. Quantitative STEM-HAADF imaging and analysis identified the stacking order of an 8-layer thin flake, which leads to the identification of anti-site In 3+(Cu +) doping. We believe that these findings will pave the way towards understanding the ferroic coupling phenomena in van der Waals lamellar compounds, asmore » well as the potential applications in 2-D electronics.« less

Antisite defects in layered multiferroic CuCr(0.9)In(0.1)P2S6.

PubMed

He, Qian; Belianinov, Alex; Dziaugys, Andrius; Maksymovych, Petro; Vysochanskii, Yulian; Kalinin, Sergei V; Borisevich, Albina Y

2015-11-28

The CuCr1-xInxP2S6 system represents a large family of metal chalcogenophosphates that are unique and promising candidates for 2D materials with functionalities such as ferroelectricity. In this work, we carried out detailed microstructural and chemical characterization of these compounds using aberration-corrected STEM, in order to understand the origin of these different ordering phenomena. Quantitative STEM-HAADF imaging and analysis identified the stacking order of an 8-layer thin flake, which leads to the identification of anti-site In(3+)(Cu(+)) doping. We believe that these findings will pave the way towards understanding the ferroic coupling phenomena in van der Waals lamellar compounds, as well as their potential applications in 2-D electronics.

Monitoring the effect of low-level laser therapy in healing process of skin with second harmonic generation imaging techniques

NASA Astrophysics Data System (ADS)

Zhang, Xiaoman; Yu, Biying; Weng, Cuncheng; Li, Hui

2014-11-01

The 632nm wavelength low intensity He-Ne laser was used to irradiated on 15 mice which had skin wound. The dynamic changes and wound healing processes were observed with nonlinear spectral imaging technology. We observed that:(1)The wound healing process was accelerated by the low-level laser therapy(LLLT);(2)The new tissues produced second harmonic generation (SHG) signals. Collagen content and microstructure differed dramatically at different time pointed along the wound healing. Our observation shows that the low intensity He-Ne laser irradiation can accelerate the healing process of skin wound in mice, and SHG imaging technique can be used to observe wound healing process, which is useful for quantitative characterization of wound status during wound healing process.

Microstructural characterization of pipe bomb fragments

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

Gregory, Otto, E-mail: gregory@egr.uri.edu; Oxley, Jimmie; Smith, James

2010-03-15

Recovered pipe bomb fragments, exploded under controlled conditions, have been characterized using scanning electron microscopy, optical microscopy and microhardness. Specifically, this paper examines the microstructural changes in plain carbon-steel fragments collected after the controlled explosion of galvanized, schedule 40, continuously welded, steel pipes filled with various smokeless powders. A number of microstructural changes were observed in the recovered pipe fragments: deformation of the soft alpha-ferrite grains, deformation of pearlite colonies, twin formation, bands of distorted pearlite colonies, slip bands, and cross-slip bands. These microstructural changes were correlated with the relative energy of the smokeless powder fillers. The energy of themore » smokeless powder was reflected in a reduction in thickness of the pipe fragments (due to plastic strain prior to fracture) and an increase in microhardness. Moreover, within fragments from a single pipe, there was a radial variation in microhardness, with the microhardness at the outer wall being greater than that at the inner wall. These findings were consistent with the premise that, with the high energy fillers, extensive plastic deformation and wall thinning occurred prior to pipe fracture. Ultimately, the information collected from this investigation will be used to develop a database, where the fragment microstructure and microhardness will be correlated with type of explosive filler and bomb design. Some analyses, specifically wall thinning and microhardness, may aid in field characterization of explosive devices.« less

Microstructural characterization of catalysis product of nanocement based materials: A review

NASA Astrophysics Data System (ADS)

Sutan, Norsuzailina Mohamed; Izaitul Akma Ideris, Nur; Taib, Siti Noor Linda; Lee, Delsye Teo Ching; Hassan, Alsidqi; Kudnie Sahari, Siti; Mohamad Said, Khairul Anwar; Rahman Sobuz, Habibur

2018-03-01

Cement as an essential element for cement-based products contributed to negative environmental issues due to its high energy consumption and carbon dioxide emission during its production. These issues create the need to find alternative materials as partial cement replacement where studies on the potential of utilizing silica based materials as partial cement replacement come into picture. This review highlights the effectiveness of microstructural characterization techniques that have been used in the studies that focus on characterization of calcium hydroxide (CH) and calcium silicate hydrate (C-S-H) formation during hydration process of cement-based product incorporating nano reactive silica based materials as partial cement replacement. Understanding the effect of these materials as cement replacement in cement based product focusing on the microstructural development will lead to a higher confidence in the use of industrial waste as a new non-conventional material in construction industry that can catalyse rapid and innovative advances in green technology.

Adaptive characterization of recrystallization kinetics in IF steel by electron backscatter diffraction.

PubMed

Kim, Dong-Kyu; Park, Won-Woong; Lee, Ho Won; Kang, Seong-Hoon; Im, Yong-Taek

2013-12-01

In this study, a rigorous methodology for quantifying recrystallization kinetics by electron backscatter diffraction is proposed in order to reduce errors associated with the operator's skill. An adaptive criterion to determine adjustable grain orientation spread depending on the recrystallization stage is proposed to better identify the recrystallized grains in the partially recrystallized microstructure. The proposed method was applied in characterizing the microstructure evolution during annealing of interstitial-free steel cold rolled to low and high true strain levels of 0.7 and 1.6, respectively. The recrystallization kinetics determined by the proposed method was found to be consistent with the standard method of Vickers microhardness. The application of the proposed method to the overall recrystallization stages showed that it can be used for the rigorous characterization of progressive microstructure evolution, especially for the severely deformed material. © 2013 The Authors Journal of Microscopy © 2013 Royal Microscopical Society.

Multiscale Modeling for the Analysis for Grain-Scale Fracture Within Aluminum Microstructures

NASA Technical Reports Server (NTRS)

Glaessgen, Edward H.; Phillips, Dawn R.; Yamakov, Vesselin; Saether, Erik

2005-01-01

Multiscale modeling methods for the analysis of metallic microstructures are discussed. Both molecular dynamics and the finite element method are used to analyze crack propagation and stress distribution in a nanoscale aluminum bicrystal model subjected to hydrostatic loading. Quantitative similarity is observed between the results from the two very different analysis methods. A bilinear traction-displacement relationship that may be embedded into cohesive zone finite elements is extracted from the nanoscale molecular dynamics results.

Surface microstructure of bitumen characterized by atomic force microscopy.

PubMed

Yu, Xiaokong; Burnham, Nancy A; Tao, Mingjiang

2015-04-01

Bitumen, also called asphalt binder, plays important roles in many industrial applications. It is used as the primary binding agent in asphalt concrete, as a key component in damping systems such as rubber, and as an indispensable additive in paint and ink. Consisting of a large number of hydrocarbons of different sizes and polarities, together with heteroatoms and traces of metals, bitumen displays rich surface microstructures that affect its rheological properties. This paper reviews the current understanding of bitumen's surface microstructures characterized by Atomic Force Microscopy (AFM). Microstructures of bitumen develop to different forms depending on crude oil source, thermal history, and sample preparation method. While some bitumens display surface microstructures with fine domains, flake-like domains, and dendrite structuring, 'bee-structures' with wavy patterns several micrometers in diameter and tens of nanometers in height are commonly seen in other binders. Controversy exists regarding the chemical origin of the 'bee-structures', which has been related to the asphaltene fraction, the metal content, or the crystallizing waxes in bitumen. The rich chemistry of bitumen can result in complicated intermolecular associations such as coprecipitation of wax and metalloporphyrins in asphaltenes. Therefore, it is the molecular interactions among the different chemical components in bitumen, rather than a single chemical fraction, that are responsible for the evolution of bitumen's diverse microstructures, including the 'bee-structures'. Mechanisms such as curvature elasticity and surface wrinkling that explain the rippled structures observed in polymer crystals might be responsible for the formation of 'bee-structures' in bitumen. Despite the progress made on morphological characterization of bitumen using AFM, the fundamental question whether the microstructures observed on bitumen surfaces represent its bulk structure remains to be addressed. In addition, critical technical challenges associated with AFM characterization of bitumen surface structures are discussed, with possible solutions recommended. For future work, combining AFM with other chemical analysis tools that can generate comparable high resolution to AFM would provide an avenue to linking bitumen's chemistry to its microscopic morphological and mechanical properties and consequently benefit the efforts of developing structure-related models for bituminous materials across the different length scales. Copyright © 2015 Elsevier B.V. All rights reserved.

The Effect of Microstructure On Transport Properties of Porous Electrodes

NASA Astrophysics Data System (ADS)

Peterson, Serena W.

The goal of this work is to further understand the relationships between porous electrode microstructure and mass transport properties. This understanding allows us to predict and improve cell performance from fundamental principles. The investigated battery systems are the widely used rechargeable Li-ion battery and the non-rechargeable alkaline battery. This work includes three main contributions in the battery field listed below. Direct Measurement of Effective Electronic Transport in Porous Li-ion Electrodes. An accurate assessment of the electronic conductivity of electrodes is necessary for understanding and optimizing battery performance. The bulk electronic conductivity of porous LiCoO2-based cathodes was measured as a function of porosity, pressure, carbon fraction, and the presence of an electrolyte. The measurements were performed by delamination of thin-film electrodes from their aluminum current collectors and by use of a four-line probe. Imaging and Correlating Microstructure To Conductivity. Transport properties of porous electrodes are strongly related to microstructure. An experimental 3D microstructure is needed not only for computation of direct transport properties, but also for a detailed electrode microstructure characterization. This work utilized X-ray tomography and focused ion beam (FIB)/scanning electron microscopy (SEM) to obtain the 3D structures of alkaline battery cathodes. FIB/SEM has the advantage of detecting carbon additives; thus, it was the main tomography tool employed. Additionally, protocols and techniques for acquiring, processing and segmenting series of FIB/SEM images were developed as part of this work. FIB/SEM images were also used to correlate electrodes' microstructure to their respective conductivities for both Li-ion and alkaline batteries. Electrode Microstructure Metrics and the 3D Stochastic Grid Model. A detailed characterization of microstructure was conducted in this work, including characterization of the volume fraction, nearest neighbor probability, domain size distribution, shape factor, and Fourier transform coefficient. These metrics are compared between 2D FIB/SEM, 3D FIB/SEM and X-ray structures. Among those metrics, the first three metrics are used as a basis for SG model parameterization. The 3D stochastic grid (SG) model is based on Monte Carlo techniques, in which a small set of fundamental inter-domain parameters are used to generate structures. This allows us to predict electrode microstructure and its effects on both electronic and ionic properties.

Quantitative study of Xanthosoma violaceum leaf surfaces using RIMAPS and variogram techniques.

PubMed

Favret, Eduardo A; Fuentes, Néstor O; Molina, Ana M

2006-08-01

Two new imaging techniques (rotated image with maximum averaged power spectrum (RIMAPS) and variogram) are presented for the study and description of leaf surfaces. Xanthosoma violaceum was analyzed to illustrate the characteristics of both techniques. Both techniques produce a quantitative description of leaf surface topography. RIMAPS combines digitized images rotation with Fourier transform, and it is used to detect patterns orientation and characteristics of surface topography. Variogram relates the mathematical variance of a surface with the area of the sample window observed. It gives the typical scale lengths of the surface patterns. RIMAPS detects the morphological variations of the surface topography pattern between fresh and dried (herbarium) samples of the leaf. The variogram method finds the characteristic dimensions of the leaf microstructure, i.e., cell length, papillae diameter, etc., showing that there are not significant differences between dry and fresh samples. The results obtained show the robustness of RIMAPS and variogram analyses to detect, distinguish, and characterize leaf surfaces, as well as give scale lengths. Both techniques are tools for the biologist to study variations of the leaf surface when different patterns are present. The use of RIMAPS and variogram opens a wide spectrum of possibilities by providing a systematic, quantitative description of the leaf surface topography.

Microscopical and elemental FESEM and Phenom ProX-SEM-EDS analysis of osteocyte- and blood vessel-like microstructures obtained from fossil vertebrates of the Eocene Messel Pit, Germany.

PubMed

Cadena, Edwin

2016-01-01

The Eocene (∾48 Ma) Messel Pit in Germany is a UNESCO World Heritage Site because of its exceptionally preserved fossils, including vertebrates, invertebrates, and plants. Messel fossil vertebrates are typically characterized by their articulated state, and in some cases the skin, hair, feathers, scales and stomach contents are also preserved. Despite the exceptional macroscopic preservation of Messel fossil vertebrates, the microstructural aspect of these fossils has been poorly explored. In particular, soft tissue structures such as hair or feathers have not been chemically analyzed, nor have bone microstructures. I report here the preservation and recovery of osteocyte-like and blood vessel-like microstructures from the bone of Messel Pit specimens, including the turtles Allaeochelys crassesculpta and Neochelys franzeni, the crocodile Diplocynodon darwini, and the pangolin Eomanis krebsi. I used a Field Emission Scanning Electron Microscope (FESEM) and a Phenom ProX desktop scanning electron microscope (LOT-QuantumDesign) equipped with a thermionic CeB6 source and a high sensitivity multi-mode backscatter electron (BSE) for microscopical and elemental characterization of these bone microstructures. Osteocyte-like and blood vessel-like microstructures are constituted by a thin layer (∾50 nm thickness), external and internal mottled texture with slightly marked striations. Circular to linear marks are common on the external surface of the osteocyte-like microstructures and are interpreted as microbial troughs. Iron (Fe) is the most abundant element found in the osteocyte-like and blood vessel-like microstructures, but not in the bone matrix or collagen fibril-like microstructures. The occurrence of well-preserved soft-tissue elements (at least their physical form) establishes a promising background for future studies on preservation of biomolecules (proteins or DNA) in Messel Pit fossils.

Automated Identification and Characterization of Secondary & Tertiary gamma’ Precipitates in Nickel-Based Superalloys (PREPRINT)

DTIC Science & Technology

2010-01-01

and intensity information from the EFTEM images. The microstructural statistics obtained from the segmented γ’ precipitates agreed with those of the...is its ability to automate segmentation of precipitates in a reproducible manner for acquiring microstructural statistics that relate to both...were identified using a combination of visual inspection and intensity information from the EFTEM images. The microstructural statistics obtained

Superlattice Microstructured Optical Fiber

PubMed Central

Tse, Ming-Leung Vincent; Liu, Zhengyong; Cho, Lok-Hin; Lu, Chao; Wai, Ping-Kong Alex; Tam, Hwa-Yaw

2014-01-01

A generic three-stage stack-and-draw method is demonstrated for the fabrication of complex-microstructured optical fibers. We report the fabrication and characterization of a silica superlattice microstructured fiber with more than 800 rhomboidally arranged air-holes. A polarization-maintaining fiber with a birefringence of 8.5 × 10−4 is demonstrated. The birefringent property of the fiber is found to be highly insensitive to external environmental effects, such as pressure. PMID:28788693

Synchrotron Radiation Microcomputed Tomography Guided Chromatographic Analysis for Displaying the Material Distribution in Tablets.

PubMed

Zhang, Liu; Wu, Li; Wang, Caifen; Zhang, Guoqing; Yu, Lin; Li, Haiyan; Maharjan, Abi; Tang, Yan; He, Dunwei; York, Peter; Sun, Huimin; Yin, Xianzhen; Zhang, Jiwen; Sun, Lixin

2018-03-06

One unusual and challenging scientific field that has received only cursory attention to date is the three-dimensional (3D) microstructure and spatial distribution of drug(s) and formulation materials in solid dosage forms. This study aims to provide deeper insight into the relationships between the microstructure of multiple-unit pellet system (MUPS) tablets and the spatial distribution of the active pharmaceutical ingredient (API) and excipients to facilitate the design of quantitative models for drug delivery systems. Synchrotron radiation X-ray microcomputed tomography (SR-μCT) was established as a 3D structure elucidation technique, which, in conjunction with liquid chromatography coupled to mass spectrometry (LC-MS) or liquid chromatography with evaporative light-scattering detector (LC-ELSD) enables chemical analysis of tablets. On the basis of the specific interior construction of theophylline MUPS tablets, the spatial distribution of materials was acquired by quantifying microregion samples that had been validated by SR-μCT for their locations in the MUPS tablets. The 3D structure of the MUPS tablets was catalogued as three structural domains: a matrix layer (ML), a protective cushion layer (PCL), and pellets (PL). Compared with the components in the ML, components in the PL had a larger proportion of theophylline, sucrose, and diethyl phthalate and a smaller proportion of lactose and sodium lauryl sulfate, whereas glyceryl monostearate was found to account for a large portion of the PCL. Microstructural characterization-guided zonal chemical determination represents a new approach for quality assessment and the development of drug delivery systems with in-depth insight into their constituent layers on a new scale.

Investigation of microstructural alterations in M50 and 52100 steel using nanoindentation

NASA Astrophysics Data System (ADS)

Paulson, Kristin R.

Bearing steels are used in rolling elements and are designed to withstand heavy loads for an extended period of time. At the end of life, microstructural alterations within the material have been observed and are linked to failure. In this study, a three ball-on-rod fatigue tester was used to test M50 and 52100 steel cylindrical rods at differing loads of 4.0 GPa, 4.5 GPa, and 5.0 GPa and in lubricated and unlubricated conditions to 108 cycles in an attempt to produce microstructural alterations. Microstructural alterations characterized as butterflies were observed and investigated further in two M50 samples that were tested at 4.5 GPa to 10 8 cycles in the lubricated and unlubricated condition. Microstructural alterations characterized as dark etching regions (DER), and white etching bands (WEBs) were not observed. Additionally, hardness was investigated cross sectionally as a function of depth and location within the wear track produced by the fatigue test. No conclusive evidence was derived from the hardness measurements as a function of depth in relation to the formation of microstructural alterations or the stress experienced subsurface within the material. Hardness measurements performed specifically within a butterfly wing, however, returned hardness values significantly higher than the matrix hardness values.

Experimental Characterization of Aluminum-Based Hybrid Composites Obtained Through Powder Metallurgy

NASA Astrophysics Data System (ADS)

Marcu, D. F.; Buzatu, M.; Ghica, V. G.; Petrescu, M. I.; Popescu, G.; Niculescu, F.; Iacob, G.

2018-06-01

The paper presents some experimental results concerning fabrication through powder metallurgy (P/M) of aluminum-based hybrid composites - Al/Al2O3/Gr. In order to understand the mechanisms that occur during the P/M processes of obtaining Al/Al2O3/Gr composite, we correlated the physical characteristics with their micro-structural characteristics. The characterization was performed using analysis techniques specific for P/M process, SEM-EDS and XRD analyses. Micro-structural characterization of the composites has revealed fairly uniform distribution this resulting in good properties of the final composite material.

An optimized framework for quantitative magnetization transfer imaging of the cervical spinal cord in vivo.

PubMed

Battiston, Marco; Grussu, Francesco; Ianus, Andrada; Schneider, Torben; Prados, Ferran; Fairney, James; Ourselin, Sebastien; Alexander, Daniel C; Cercignani, Mara; Gandini Wheeler-Kingshott, Claudia A M; Samson, Rebecca S

2018-05-01

To develop a framework to fully characterize quantitative magnetization transfer indices in the human cervical cord in vivo within a clinically feasible time. A dedicated spinal cord imaging protocol for quantitative magnetization transfer was developed using a reduced field-of-view approach with echo planar imaging (EPI) readout. Sequence parameters were optimized based in the Cramer-Rao-lower bound. Quantitative model parameters (i.e., bound pool fraction, free and bound pool transverse relaxation times [ T2F, T2B], and forward exchange rate [k FB ]) were estimated implementing a numerical model capable of dealing with the novelties of the sequence adopted. The framework was tested on five healthy subjects. Cramer-Rao-lower bound minimization produces optimal sampling schemes without requiring the establishment of a steady-state MT effect. The proposed framework allows quantitative voxel-wise estimation of model parameters at the resolution typically used for spinal cord imaging (i.e. 0.75 × 0.75 × 5 mm 3 ), with a protocol duration of ∼35 min. Quantitative magnetization transfer parametric maps agree with literature values. Whole-cord mean values are: bound pool fraction = 0.11(±0.01), T2F = 46.5(±1.6) ms, T2B = 11.0(±0.2) µs, and k FB  = 1.95(±0.06) Hz. Protocol optimization has a beneficial effect on reproducibility, especially for T2B and k FB . The framework developed enables robust characterization of spinal cord microstructure in vivo using qMT. Magn Reson Med 79:2576-2588, 2018. © 2017 The Authors Magnetic Resonance in Medicine published by Wiley Periodicals, Inc. on behalf of International Society for Magnetic Resonance in Medicine. This is an open access article under the terms of the Creative Commons Attribution License, which permits use, distribution and reproduction in any medium, provided the original work is properly cited. © 2017 The Authors Magnetic Resonance in Medicine published by Wiley Periodicals, Inc. on behalf of International Society for Magnetic Resonance in Medicine.

In Situ Microstructural Control and Mechanical Testing Inside the Transmission Electron Microscope at Elevated Temperatures

NASA Astrophysics Data System (ADS)

Wang, Baoming; Haque, M. A.

2015-08-01

With atomic-scale imaging and analytical capabilities such as electron diffraction and energy-loss spectroscopy, the transmission electron microscope has allowed access to the internal microstructure of materials like no other microscopy. It has been mostly a passive or post-mortem analysis tool, but that trend is changing with in situ straining, heating and electrical biasing. In this study, we design and demonstrate a multi-functional microchip that integrates actuators, sensors, heaters and electrodes with freestanding electron transparent specimens. In addition to mechanical testing at elevated temperatures, the chip can actively control microstructures (grain growth and phase change) of the specimen material. Using nano-crystalline aluminum, nickel and zirconium as specimen materials, we demonstrate these novel capabilities inside the microscope. Our approach of active microstructural control and quantitative testing with real-time visualization can influence mechanistic modeling by providing direct and accurate evidence of the fundamental mechanisms behind materials behavior.

Strength and microstructure of sintered Si3N4 with rare-earth-oxide additions

NASA Technical Reports Server (NTRS)

Sanders, W. A.; Mieskowski, D. M.

1985-01-01

Room temperature, 700-, 1000-, 1200-, and 1370-C examinations of the effect of 1.7-2.6 mol pct rare earth oxide additions to sintered Si3N4 are conducted. While the room temperature-1000 C bend strengths were higher for this material with Y2O3 additions than with CeO2, La2O3, or Sm2O3, the reverse was true at 1200-1370 C. This phenomenon is explained on the basis of microstructural differences, since quantitative microscopy of SEM replicas showed the Si3N4-Y2O3 composition to contain both a higher percentage of elongated grains and a coarser microstructure than the other three alternatives. The elongated grains appear to increase this composition's low temperature strength irrespective of microstructural coarseness; this coarseness, however, decreases strength relative to the other compositions at higher temperatures.

Segmentation-free image processing and analysis of precipitate shapes in 2D and 3D

NASA Astrophysics Data System (ADS)

Bales, Ben; Pollock, Tresa; Petzold, Linda

2017-06-01

Segmentation based image analysis techniques are routinely employed for quantitative analysis of complex microstructures containing two or more phases. The primary advantage of these approaches is that spatial information on the distribution of phases is retained, enabling subjective judgements of the quality of the segmentation and subsequent analysis process. The downside is that computing micrograph segmentations with data from morphologically complex microstructures gathered with error-prone detectors is challenging and, if no special care is taken, the artifacts of the segmentation will make any subsequent analysis and conclusions uncertain. In this paper we demonstrate, using a two phase nickel-base superalloy microstructure as a model system, a new methodology for analysis of precipitate shapes using a segmentation-free approach based on the histogram of oriented gradients feature descriptor, a classic tool in image analysis. The benefits of this methodology for analysis of microstructure in two and three-dimensions are demonstrated.

BiVO4 microstructures with various morphologies: Synthesis and characterization

NASA Astrophysics Data System (ADS)

Wu, Min; Jing, Qifeng; Feng, Xinyan; Chen, Limiao

2018-01-01

Bismuth vanadate (BiVO4) microstructures with dumbbell, rod, ellipsoid, sphere, and cake-like morphologies have been successfully fabricated by using a surfactant-free hydrothermal method, in which the morphology of the BiVO4 microstructures can be tuned by simply varying the molar ratio of Bi(NO)3·5H2O to NaVO3 in the starting materials. Based on a series of contrast experiments, the probable formation mechanism of the BiVO4 microstructures with multiple shapes have been proposed. The photocatalytic performances of the as-prepared BiVO4 microstructures have been evaluated by studying the degradation of Rhodamine B solutions under visible light irradiation. The results reveal that the cake-like BiVO4 microstructures exhibit the higher photocatalytic activity than other BiVO4 microstructures due to its high surface area and unique morphology.

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.

Correlations Between Micromagnetic, Microstructural and Microchemical Properties in Ultrathin Epitaxial Magnetic Structures. Magnetic Microstructure Observed With Electron Holography in STEM

DTIC Science & Technology

1998-06-10

and Small Particles, Marian Mankos, J.M. Cowley, M.R. Scheinfein, Material Reseach Society Bulletin, October 95’, 45, (1995). 77 Quantitative...Micromagnetics: Electron Holography of Magnetic Thin Films and Multilayers, Marian Mankos, M.R. Scheinfein, J.M. Cowley, IEEE Trans. MAG-32(5), 4150 (1996...Spatial Resolution, Marian . Mankos, Z.J. Yang, M.R. Scheinfein, J.M. Cowley, IEEE-Trans. MAG 30(6), 4497 (1994). 67 Far Out-of-Focus Electron Holography

Accelerated Irradiations for High Dose Microstructures in Fast Reactor Alloys

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

Jiao, Zhijie

The objective of this project is to determine the extent to which high dose rate, self-ion irradiation can be used as an accelerated irradiation tool to understand microstructure evolution at high doses and temperatures relevant to advanced fast reactors. We will accomplish the goal by evaluating phase stability and swelling of F-M alloys relevant to SFR systems at very high dose by combining experiment and modeling in an effort to obtain a quantitative description of the processes at high and low damage rates.

A simple microstructure return model explaining microstructure noise and Epps effects

NASA Astrophysics Data System (ADS)

Saichev, A.; Sornette, D.

2014-01-01

We present a novel simple microstructure model of financial returns that combines (i) the well-known ARFIMA process applied to tick-by-tick returns, (ii) the bid-ask bounce effect, (iii) the fat tail structure of the distribution of returns and (iv) the non-Poissonian statistics of inter-trade intervals. This model allows us to explain both qualitatively and quantitatively important stylized facts observed in the statistics of both microstructure and macrostructure returns, including the short-ranged correlation of returns, the long-ranged correlations of absolute returns, the microstructure noise and Epps effects. According to the microstructure noise effect, volatility is a decreasing function of the time-scale used to estimate it. The Epps effect states that cross correlations between asset returns are increasing functions of the time-scale at which the returns are estimated. The microstructure noise is explained as the result of the negative return correlations inherent in the definition of the bid-ask bounce component (ii). In the presence of a genuine correlation between the returns of two assets, the Epps effect is due to an average statistical overlap of the momentum of the returns of the two assets defined over a finite time-scale in the presence of the long memory process (i).

Characterization of a High Strength, Refractory High Entropy Alloy, AlMo0.5NbTa0.5TiZr

NASA Astrophysics Data System (ADS)

Jensen, Jacob

High entropy alloys (HEAs) are a relatively new class of materials that have garnered significant interest over the last decade due to their intriguing balance of properties including high strength, toughness, and corrosion resistance. In contrast to conventional alloy systems, HEAs are based on four or more principal elements with near equimolar concentrations and tend to have simple microstructures due to the preferential formation of solid solution phases. HEAs appear to offer new pathways to lightweighting in structural applications, new alloys for elevated temperature components, and new magnetic materials, but more thorough characterization studies are needed to assess the viability of the recently developed multicomponent materials. One such HEA, AlMo0.5NbTa0.5TiZr, was selected to be the basis for this characterization study in part due to its strength at elevated temperatures (sigma0.2 = 1600 MPa at T = 800 °C) and low density compared with commercially available Ni-based superalloys. The refractory element containing HEA composition was developed in order to balance the high temperature strength of the refractory elements with the desirable properties achieved by the high entropy alloying design approach for potential use in aerospace thermal protection and structural applications. Ingots of AlMo0.5NbTa0.5TiZr were cast by vacuum arc melting followed by hot isostatic pressing (HIP) and homogenization at 1400 °C for 24 hrs with a furnace cool of 10 °C/min. The resulting microstructure was characterized at multiple length scales using x-ray diffraction (XRD), scanning transmission electron microscopy (SEM), conventional and scanning transmission electron microscopy (TEM and STEM), and x-ray energy dispersive spectroscopy (XEDS). The microstructure was found to consist of a periodic, coherent two phase mixture, where a disordered bcc phase is aligned orthogonally in an ordered B2 phase. Through microstructural evolution heat treatment studies, the nanoscale interpenetrating microstructure was discovered to form via a conditional spinodal reaction pathway involving a congruent ordering transformation preceding spinodal decomposition. In order to gain a comprehensive understanding of the true morphology of these phases and obtain a novel perspective of 3D elemental segregation in the HEA, STEM-high angle annular darkfield (HAADF) micrographs and XEDS spectral images were utilized in the tomographic reconstruction of the microstructure, which was inherently difficult to observe through conventional characterization techniques. The microstructure of the alloy was ultimately refined by incremental variations to the base alloy composition in an effort to remove deleterious intermetallic phases adversely affecting ductility. Despite the excellent compressive strength across a wide range of temperatures and the ability to tailor the microstructure by compositional modifications, microstructural and phase transformations in the desired operating temperature range indicate that the AlMo0.5NbTa0.5TiZr alloy may not be a suitable material for high temperature aerospace structural components.

The effect of spark plasma sintering on lithium disilicate glass-ceramics.

PubMed

Al Mansour, Fatima; Karpukhina, Natalia; Grasso, Salvatore; Wilson, Rory M; Reece, Mike J; Cattell, Michael J

2015-10-01

To evaluate the effects of spark plasma sintering (SPS) on the microstructure of lithium disilicate glass-ceramics. IPS e.max CAD glass-ceramic samples were processed using spark plasma sintering (SPS) and conventionally sintered (CS) as a comparison. Specimens were sintered at varying temperatures (T1: 840°C, T2: 820°C, T3: 800°C), heating rates (HR1: 150°C/min, HR2: 300°C/min, HR3: 500°C/min) and pressures (P1: 15MPa, P2: 50MPa, P3: 70MPa). IPS e.max Press glass powder samples were densified at 750 and 800°C (50 or 200MPa pressure). Samples were characterized using XRD, HTXRD, and SEM and quantitative image analysis. There was a significant increase in median crystal size (MCS) between the CS and the SPS T1 groups. A statistical difference (p>0.05) in MCS between SPS T1 and SPS T2 groups was observed. The SPS HR3 sample produced a smaller MCS than the CS, SPS HR1 and HR2 groups (p<0.05). The SPS P3 sample had a reduction in MCS compared with the CS group (p<0.05). XRD of the SPS samples revealed major lithium disilicate/lithium metasilicate phases and minor lithium orthophosphate and cristobalite/quartz phases. Densified IPS e.max Press glass samples resulted in fine fibrils or graduated lithium disilicate crystals. The effects of SPS were used to refine the microstructure of IPS e.max CAD lithium disilicate glass-ceramics. Densification by SPS of IPS e.max Press glass resulted in textured and fine nano-crystalline microstructures. SPS generated glass-ceramic microstructures may have unique properties and could be useful in the production of CAD/CAM materials for dentistry. Copyright © 2015 Academy of Dental Materials. Published by Elsevier Ltd. All rights reserved.

Detecting diffusion-diffraction patterns in size distribution phantoms using double-pulsed field gradient NMR: Theory and experiments.

PubMed

Shemesh, Noam; Ozarslan, Evren; Basser, Peter J; Cohen, Yoram

2010-01-21

NMR observable nuclei undergoing restricted diffusion within confining pores are important reporters for microstructural features of porous media including, inter-alia, biological tissues, emulsions and rocks. Diffusion NMR, and especially the single-pulsed field gradient (s-PFG) methodology, is one of the most important noninvasive tools for studying such opaque samples, enabling extraction of important microstructural information from diffusion-diffraction phenomena. However, when the pores are not monodisperse and are characterized by a size distribution, the diffusion-diffraction patterns disappear from the signal decay, and the relevant microstructural information is mostly lost. A recent theoretical study predicted that the diffusion-diffraction patterns in double-PFG (d-PFG) experiments have unique characteristics, such as zero-crossings, that make them more robust with respect to size distributions. In this study, we theoretically compared the signal decay arising from diffusion in isolated cylindrical pores characterized by lognormal size distributions in both s-PFG and d-PFG methodologies using a recently presented general framework for treating diffusion in NMR experiments. We showed the gradual loss of diffusion-diffraction patterns in broadening size distributions in s-PFG and the robustness of the zero-crossings in d-PFG even for very large standard deviations of the size distribution. We then performed s-PFG and d-PFG experiments on well-controlled size distribution phantoms in which the ground-truth is well-known a priori. We showed that the microstructural information, as manifested in the diffusion-diffraction patterns, is lost in the s-PFG experiments, whereas in d-PFG experiments the zero-crossings of the signal persist from which relevant microstructural information can be extracted. This study provides a proof of concept that d-PFG may be useful in obtaining important microstructural features in samples characterized by size distributions.

A hybrid finite-element and cellular-automaton framework for modeling 3D microstructure of Ti–6Al–4V alloy during solid–solid phase transformation in additive manufacturing

NASA Astrophysics Data System (ADS)

Chen, Shaohua; Xu, Yaopengxiao; Jiao, Yang

2018-06-01

Additive manufacturing such as selective laser sintering and electron beam melting has become a popular technique which enables one to build near-net-shape product from packed powders. The performance and properties of the manufactured product strongly depends on its material microstructure, which is in turn determined by the processing conditions including beam power density, spot size, scanning speed and path etc. In this paper, we develop a computational framework that integrates the finite element method (FEM) and cellular automaton (CA) simulation to model the 3D microstructure of additively manufactured Ti–6Al–4V alloy, focusing on the β → α + β transition pathway in a consolidated alloy region as the power source moves away from this region. Specifically, the transient temperature field resulted from a scanning laser/electron beam following a zig-zag path is first obtained by solving nonlinear heat transfer equations using the FEM. Next, a CA model for the β → α + β phase transformation in the consolidated alloy is developed which explicitly takes into account the temperature dependent heterogeneous nucleation and anisotropic growth of α grains from the parent β phase field. We verify our model by reproducing the overall transition kinetics predicted by the Johnson–Mehl–Avrami–Kolmogorov theory under a typical processing condition and by quantitatively comparing our simulation results with available experimental data. The utility of the model is further demonstrated by generating large-field realistic 3D alloy microstructures for subsequent structure-sensitive micro-mechanical analysis. In addition, we employ our model to generate a wide spectrum of alloy microstructures corresponding to different processing conditions for establishing quantitative process-structure relations for the system.

Impact of Weight Loss With Intragastric Balloon on Bone Density and Microstructure in Obese Adults.

PubMed

Madeira, Eduardo; Madeira, Miguel; Guedes, Erika Paniago; Mafort, Thiago Thomaz; Moreira, Rodrigo Oliveira; de Mendonça, Laura Maria Carvalho; Lima, Inayá Correa Barbosa; Neto, Leonardo Vieira; de Pinho, Paulo Roberto Alves; Lopes, Agnaldo José; Farias, Maria Lucia Fleiuss

2018-03-21

The historical concept that obesity protects against bone fractures has been questioned. Weight loss appears to reduce bone mineral density (BMD); however, the results in young adults are inconsistent, and data on the effects of weight loss on bone microstructure are limited. This study aimed to evaluate the impact of weight loss using an intragastric balloon (IGB) on bone density and microstructure. Forty obese patients with metabolic syndrome (mean age 35.1 ± 7.3 yr) used an IGB continuously for 6 mo. Laboratory tests, areal BMD, and body composition measurements via dual-energy X-ray absorptiometry, and volumetric BMD and bone microstructure measurements via high-resolution peripheral quantitative computed tomography were conducted before IGB placement and after IGB removal. The mean weight loss was 11.5%. After 6 mo, there were significant increases in vitamin D and carboxyterminal telopeptide of type 1 collagen levels. After IGB use, areal BMD increased in the spine but decreased in the total femur and the 33% radius. Cortical BMD increased in the distal radius but tended to decrease in the distal tibia. The observed trabecular bone loss in the distal tibia contributed to the decline in the total volumetric BMD at this site. There was a negative correlation between the changes in leptin levels and the measures of trabecular quality in the tibia on high-resolution peripheral quantitative computed tomography. Weight loss may negatively impact bone microstructure in young patients, especially for weight-bearing bones, in which obesity has a more prominent effect. Copyright © 2018 The International Society for Clinical Densitometry. Published by Elsevier Inc. All rights reserved.

Investigation on the Size Effect in Large-Scale Beta-Processed Ti-17 Disks Based on Quantitative Metallography

NASA Astrophysics Data System (ADS)

Zhang, Saifei; Zeng, Weidong; Gao, Xiongxiong; Zhao, Xingdong; Li, Siqing

2017-10-01

The present study investigates the mechanical properties of large-scale beta-processed Ti-17 forgings because of the increasing interest in beta thermal-mechanical processing method for fabricating compressor disks or blisks in aero-engines due to its advantage in damage tolerance performance. Three Ti-17 disks with different weights of 57, 250 and 400 kg were prepared by beta processing techniques firstly for comparative study. The results reveal a significant `size effect' in beta-processed Ti-17 disks, i.e., dependences of high cycle fatigue, tensile properties and fracture toughness of beta-processed Ti-17 disks on disk size (or weight). With increasing disk weight from 57 to 400 kg, the fatigue limit (fatigue strength at 107 cycles, R = -1) was reduced from 583 to 495 MPa, tensile yield strength dropped from 1073 to 1030 MPa, while fracture toughness ( K IC) rose from 70.9 to 95.5 MPaṡm1/2. Quantitative metallography analysis shows that the `size effect' of mechanical properties can be attributed to evident differences between microstructures of the three disk forgings. With increasing disk size, nearly all microstructural components in the basket-weave microstructure, including prior β grain, α layers at β grain boundaries (GB- α) and α lamellas at the interior of the grains, get coarsened to different degrees. Further, the microstructural difference between the beta-processed disks is proved to be the consequence of longer pre-forging soaking time and lower post-forging cooling rate for large disks than small ones. Finally, suggestions are made from the perspective of microstructural control on how to improve mechanical properties of large-scale beta-processed Ti-17 forgings.

Solidification microstructures in single-crystal stainless steel melt pools

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

Sipf, J.B.; Boatner, L.A.; David, S.A.

1994-03-01

Development of microstructure of stationary melt pools of oriented stainless steel single crystals (70%Fe-15%Ni-15%Cr was analyzed. Stationary melt pools were formed by electron-beam and gas-tungsten-arc heating on (001), (011), and (111) oriented planes of the austenitic, fcc-alloy crystals. Characterization and analysis of resulting microstructure was carried out for each crystallographic plane and welding method. Results showed that crystallography which favors ``easy growth`` along the <100> family of directions is a controlling factor in the microstructural formation along with the melt-pool shape. The microstructure was found to depend on the melting method, since each method forms a unique melt-pool shape. Thesemore » results are used in making a three-dimensional reconstruction of the microstructure for each plane and melting method employed. This investigation also suggests avenues for future research into the microstructural properties of electron-beam welds as well as providing an experimental basis for mathematical models for the prediction of solidification microstructures.« less

Connectivity Measures in EEG Microstructural Sleep Elements.

PubMed

Sakellariou, Dimitris; Koupparis, Andreas M; Kokkinos, Vasileios; Koutroumanidis, Michalis; Kostopoulos, George K

2016-01-01

During Non-Rapid Eye Movement sleep (NREM) the brain is relatively disconnected from the environment, while connectedness between brain areas is also decreased. Evidence indicates, that these dynamic connectivity changes are delivered by microstructural elements of sleep: short periods of environmental stimuli evaluation followed by sleep promoting procedures. The connectivity patterns of the latter, among other aspects of sleep microstructure, are still to be fully elucidated. We suggest here a methodology for the assessment and investigation of the connectivity patterns of EEG microstructural elements, such as sleep spindles. The methodology combines techniques in the preprocessing, estimation, error assessing and visualization of results levels in order to allow the detailed examination of the connectivity aspects (levels and directionality of information flow) over frequency and time with notable resolution, while dealing with the volume conduction and EEG reference assessment. The high temporal and frequency resolution of the methodology will allow the association between the microelements and the dynamically forming networks that characterize them, and consequently possibly reveal aspects of the EEG microstructure. The proposed methodology is initially tested on artificially generated signals for proof of concept and subsequently applied to real EEG recordings via a custom built MATLAB-based tool developed for such studies. Preliminary results from 843 fast sleep spindles recorded in whole night sleep of 5 healthy volunteers indicate a prevailing pattern of interactions between centroparietal and frontal regions. We demonstrate hereby, an opening to our knowledge attempt to estimate the scalp EEG connectivity that characterizes fast sleep spindles via an "EEG-element connectivity" methodology we propose. The application of the latter, via a computational tool we developed suggests it is able to investigate the connectivity patterns related to the occurrence of EEG microstructural elements. Network characterization of specified physiological or pathological EEG microstructural elements can potentially be of great importance in the understanding, identification, and prediction of health and disease.

Connectivity Measures in EEG Microstructural Sleep Elements

PubMed Central

Sakellariou, Dimitris; Koupparis, Andreas M.; Kokkinos, Vasileios; Koutroumanidis, Michalis; Kostopoulos, George K.

2016-01-01

During Non-Rapid Eye Movement sleep (NREM) the brain is relatively disconnected from the environment, while connectedness between brain areas is also decreased. Evidence indicates, that these dynamic connectivity changes are delivered by microstructural elements of sleep: short periods of environmental stimuli evaluation followed by sleep promoting procedures. The connectivity patterns of the latter, among other aspects of sleep microstructure, are still to be fully elucidated. We suggest here a methodology for the assessment and investigation of the connectivity patterns of EEG microstructural elements, such as sleep spindles. The methodology combines techniques in the preprocessing, estimation, error assessing and visualization of results levels in order to allow the detailed examination of the connectivity aspects (levels and directionality of information flow) over frequency and time with notable resolution, while dealing with the volume conduction and EEG reference assessment. The high temporal and frequency resolution of the methodology will allow the association between the microelements and the dynamically forming networks that characterize them, and consequently possibly reveal aspects of the EEG microstructure. The proposed methodology is initially tested on artificially generated signals for proof of concept and subsequently applied to real EEG recordings via a custom built MATLAB-based tool developed for such studies. Preliminary results from 843 fast sleep spindles recorded in whole night sleep of 5 healthy volunteers indicate a prevailing pattern of interactions between centroparietal and frontal regions. We demonstrate hereby, an opening to our knowledge attempt to estimate the scalp EEG connectivity that characterizes fast sleep spindles via an “EEG-element connectivity” methodology we propose. The application of the latter, via a computational tool we developed suggests it is able to investigate the connectivity patterns related to the occurrence of EEG microstructural elements. Network characterization of specified physiological or pathological EEG microstructural elements can potentially be of great importance in the understanding, identification, and prediction of health and disease. PMID:26924980

The Relationships Between Microstructure, Tensile Properties and Fatigue Life in Ti-5Al-5V-5Mo-3Cr-0.4Fe (Ti-5553)

NASA Astrophysics Data System (ADS)

Foltz, John W., IV

beta-titanium alloys are being increasingly used in airframes as a way to decrease the weight of the aircraft. As a result of this movement, Ti-5Al-5V-5Mo-3Cr-0.4Fe (Timetal 555), a high-strength beta titanium alloy, is being used on the current generation of landing gear. This alloy features good combinations of strength, ductility, toughness and fatigue life in alpha+beta processed conditions, but little is known about beta-processed conditions. Recent work by the Center for the Accelerated Maturation of Materials (CAMM) research group at The Ohio State University has improved the tensile property knowledge base for beta-processed conditions in this alloy, and this thesis augments the aforementioned development with description of how microstructure affects fatigue life. In this work, beta-processed microstructures have been produced in a Gleeble(TM) thermomechanical simulator and subsequently characterized with a combination of electron and optical microscopy techniques. Four-point bending fatigue tests have been carried out on the material to characterize fatigue life. All the microstructural conditions have been fatigue tested with the maximum test stress equal to 90% of the measured yield strength. The subsequent results from tensile tests, fatigue tests, and microstructural quantification have been analyzed using Bayesian neural networks in an attempt to predict fatigue life using microstructural and tensile inputs. Good correlation has been developed between lifetime predictions and experimental results using microstructure and tensile inputs. Trained Bayesian neural networks have also been used in a predictive fashion to explore functional dependencies between these inputs and fatigue life. In this work, one section discusses the thermal treatments that led to the observed microstructures, and the possible sequence of precipitation that led to these microstructures. The thesis then describes the implications of microstructure on fatigue life and implications of tensile properties on fatigue life. Several additional experiments are then described that highlight possible causes for the observed dependence of microstructure on fatigue life, including fractographic evidence to provide support of microstructural dependencies.

Molecular modeling of the microstructure evolution during carbon fiber processing

NASA Astrophysics Data System (ADS)

Desai, Saaketh; Li, Chunyu; Shen, Tongtong; Strachan, Alejandro

2017-12-01

The rational design of carbon fibers with desired properties requires quantitative relationships between the processing conditions, microstructure, and resulting properties. We developed a molecular model that combines kinetic Monte Carlo and molecular dynamics techniques to predict the microstructure evolution during the processes of carbonization and graphitization of polyacrylonitrile (PAN)-based carbon fibers. The model accurately predicts the cross-sectional microstructure of the fibers with the molecular structure of the stabilized PAN fibers and physics-based chemical reaction rates as the only inputs. The resulting structures exhibit key features observed in electron microcopy studies such as curved graphitic sheets and hairpin structures. In addition, computed X-ray diffraction patterns are in good agreement with experiments. We predict the transverse moduli of the resulting fibers between 1 GPa and 5 GPa, in good agreement with experimental results for high modulus fibers and slightly lower than those of high-strength fibers. The transverse modulus is governed by sliding between graphitic sheets, and the relatively low value for the predicted microstructures can be attributed to their perfect longitudinal texture. Finally, the simulations provide insight into the relationships between chemical kinetics and the final microstructure; we observe that high reaction rates result in porous structures with lower moduli.

Chairside CAD/CAM materials. Part 1: Measurement of elastic constants and microstructural characterization.

PubMed

Belli, Renan; Wendler, Michael; de Ligny, Dominique; Cicconi, Maria Rita; Petschelt, Anselm; Peterlik, Herwig; Lohbauer, Ulrich

2017-01-01

A deeper understanding of the mechanical behavior of dental restorative materials requires an insight into the materials elastic constants and microstructure. Here we aim to use complementary methodologies to thoroughly characterize chairside CAD/CAM materials and discuss the benefits and limitations of different analytical strategies. Eight commercial CAM/CAM materials, ranging from polycrystalline zirconia (e.max ZirCAD, Ivoclar-Vivadent), reinforced glasses (Vitablocs Mark II, VITA; Empress CAD, Ivoclar-Vivadent) and glass-ceramics (e.max CAD, Ivoclar-Vivadent; Suprinity, VITA; Celtra Duo, Dentsply) to hybrid materials (Enamic, VITA; Lava Ultimate, 3M ESPE) have been selected. Elastic constants were evaluated using three methods: Resonant Ultrasound Spectroscopy (RUS), Resonant Beam Technique (RBT) and Ultrasonic Pulse-Echo (PE). The microstructures were characterized using Scanning Electron Microscopy (SEM), Energy Dispersive X-ray Spectroscopy (EDX), Raman Spectroscopy and X-ray Diffraction (XRD). Young's modulus (E), Shear modulus (G), Bulk modulus (B) and Poisson's ratio (ν) were obtained for each material. E and ν reached values ranging from 10.9 (Lava Ultimate) to 201.4 (e.max ZirCAD) and 0.173 (Empress CAD) to 0.47 (Lava Ultimate), respectively. RUS showed to be the most complex and reliable method, while the PE method the easiest to perform but most unreliable. All dynamic methods have shown limitations in measuring the elastic constants of materials showing high damping behavior (hybrid materials). SEM images, Raman spectra and XRD patterns were made available for each material, showing to be complementary tools in the characterization of their crystal phases. Here different methodologies are compared for the measurement of elastic constants and microstructural characterization of CAD/CAM restorative materials. The elastic properties and crystal phases of eight materials are herein fully characterized. Copyright © 2016 The Academy of Dental Materials. Published by Elsevier Ltd. All rights reserved.

Phased Array Ultrasonic Sound Field Mapping in Cast Austenitic Stainless Steel

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

Crawford, Susan L.; Prowant, Matthew S.; Cinson, Anthony D.

2014-05-31

This study maps the phased array-generated acoustic sound fields through three types of CASS microstructure in four specimens to quantitatively assess the beam formation effectiveness in these materials.

Latest Development and Application of High Strength and Heavy Gauge Pipeline Steel in China

NASA Astrophysics Data System (ADS)

Yongqing, Zhang; Aimin, Guo; Chengjia, Shang; Qingyou, Liu; Gray, J. Malcolm; Barbaro, Frank

Over the past twenty years, significant advances have been made in the field of microalloying and associated application, among which one of the most successful application cases is HTP practice for heavy gauge, high strength pipeline steels. Combined the strengthening effects of TMCP and retardation effects of austenite recrystallization with increasing Nb in austenite region, HTP conception with low carbon and high niobium alloy design has been successfully applied to develop X80 coil with a thickness of 18.4mm used for China's Second West-East pipeline. During this process, big efforts were made to further develop and enrich the application of microalloying technology, and at the same time the strengthening effects of Nb have been completely unfolded and fully utilized with improved metallurgical quality and quantitative analysis of microstructure. In this paper, the existing status and strengthening effect of Nb during reheating, rolling, cooling and welding have been analyzed and characterized based on mass production samples and laboratory analysis. As confirmed, grain refinement remains the most basic strengthening measure to reduce the microstructure gradient along the thickness, which in turn enlarges the processing window to improve upon low temperature toughness, and finally make it possible to develop heavy gauge, high strength pipeline steels with more challenging fracture toughness requirements.

Characterization of Semiconductor Nanocrystal Assemblies as Components of Optoelectronic Devices

NASA Astrophysics Data System (ADS)

Malfavon-Ochoa, Mario

This dissertation presents new insight into the ability of small molecule passivated NCs to achieve intimate approach distances, despite being well passivated, while developing guiding principles in the area of ligand mediated microstructure control and the resulting macroscopic optical and electronic properties that close packing of high quality NCs enables. NC ligand coverage will be characterized quantitatively through thermogravimetric analysis (TGA), and qualitatively by photoluminescence and electroluminescence, in the case of functional devices; illustrating the importance of practitioner dependent control of ligand coverage through variations in the dispersion precipitation purification procedure. A unique examination of the relative contribution of energy and charge transfer in NC LEDs will demonstrate the ability to achieve charge transfer, at a level competitive with energy transfer, to well passivated NCs at various wt% loading in a polymer matrix. The observation of potential dependent recombination zones within an active layer further suggest novel, NC surface passivation mediated control of blend microstructure during solution processing towards the development of a bi-continuous network. Next, NC self-assembly and resulting microstructure dependent optical and electronic properties will be examined through electroluminescence and high-resolution transmission electron microscopy (TEM) micrographs of functional NC/polymer bulk heterojunction LEDs. The joint characterization of NC optical properties, and self-assembly microstructure provide a deeper understanding of the significant and inseparable effects of minimal changes in NC surface passivation on structure and function, and emphasize the potential to rely on strongly passivating ligands to control physical properties and processing parameters concurrently towards higher efficiency devices via low cost processing. Finally, micro-contact printing of blazed transmission gratings, using stable dispersions of core and core/shell NCs will be shown to produce close packed assemblies of NCs forming near-wavelength luminescent superstructures separated in space. We show the dominant contribution of a two-monolayer thick sharp interface CdS shell to the diffraction efficiency, and necessarily the refractive index, of the NCs, independent of core size. Utilization of these gratings as in-coupling elements at various positions within a device architecture are also examined. These new observations were achieved by unprecedented control of NC architecture during dispersion processing, while maintaining high luminescence, made possible by optimized NC surface passivation. These studies enable the formation of new LED architectures, and new optoelectronic devices based on angle resolved, monochromatic fluorescence from diffraction gratings prepared from simple solution processing approaches. Further, the novel observation of angle amplified interfering fluorescence from these features is argued to be a result of long range radiative coupling and superradiance enabled by the monodispersity and high-quality NC surface passivation described herein.

Characterization of GaN microstructures grown by plasma-assisted molecular beam epitaxy

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

Lo, Ikai; Pang, Wen-Yuan; Hsu, Yu-Chi

2013-06-15

The characterization of GaN microstructures grown by plasma-assisted molecular beam epitaxy on LiAlO{sub 2} substrate was studied by cathodoluminescence and photoluminescence measurements. We demonstrated that the cathodoluminescence from oblique semi-polar surfaces of mushroom-shaped GaN was much brighter than that from top polar surface due to the reduction of polarization field on the oblique semi-polar surfaces. It implies that the oblique semi-polar surface is superior for the light-emitting surface of wurtzite nano-devices.

Characterization and microstructure of HPMC/Gly:AgNO3 polymer composites

NASA Astrophysics Data System (ADS)

Ananda, H. T.; Urs, G. Thejas; Somashekar, R.

2018-04-01

This study reports the synthesis and characterization of AgNo3 doped HPMC/Glycerol blend films. The microstructural parameters of these composites were evaluated employing whole powder pattern fitting method (WPPF) and the results obtained are related with other physical properties. AC conductivity results and optical band gap evaluated from UV/Vis studies are focused to establish structure property relations. These composite films are bio-degradable in nature and non-hazardous, this makes them very suitable candidates for applications in appropriate fields.

Toothpaste microstructure and rheological behaviors including aging and partial rejuvenation

NASA Astrophysics Data System (ADS)

Liu, Zhiwei; Liu, Lei; Zhou, Huan; Wang, Jiali; Deng, Linhong

2015-08-01

Toothpastes are mainly composed of a dense suspension of abrasive substances, flavors, and therapeutic ingredients in a background liquid of humectants and water, and usually exhibit complex rheological behaviors. However, the relationship between the rheology and microstructure of toothpaste remains to be studied. In this paper, three commonly used toothpastes, namely Colgate, Darlie and Yunnan Baiyao (Ynby), were qualitatively and quantitatively studied as soft glassy materials. We found that although the three toothpastes generally behaved in similar fashion in terms of rheology, each particular one was distinct from others in terms of the quantitative magnitude of the rheologcial properties including thixotropy, creep and relaxation, yield stress, and power-law dependence of modulus on frequency. In addition, the history-dependent effects were interpreted in terms of aging and rejuvenation phenomena, analogous to those existing in glassy systems, and Ynby seemed to result in greater extent of aging and rejuvenation as compared to the other two. All these differences in toothpaste rheology may well be attributed to the different microscopic network microstructures as observed in this study. Therefore, this study provides first evidence of microstructurebased rheological behaviors of toothpaste, which may be useful for optimizing its composition, manufacturing processing as well as end-user applications.

Mechanical characterization of collagen-glycosaminoglycan scaffolds.

PubMed

Harley, Brendan A; Leung, Janet H; Silva, Emilio C C M; Gibson, Lorna J

2007-07-01

Tissue engineering scaffolds are used extensively as three-dimensional analogs of the extracellular matrix (ECM). However, less attention has been paid to characterizing the scaffold microstructure and mechanical properties than to the processing and bioactivity of scaffolds. Collagen-glycosaminoglycan (CG) scaffolds have long been utilized as ECM analogs for the regeneration of skin and are currently being considered for the regeneration of nerve and conjunctiva. Recently a series of CG scaffolds with a uniform pore microstructure has been developed with a range of sizes of equiaxed pores. Experimental characterization and theoretical modeling techniques have previously been used to describe the pore microstructure, specific surface area, cell attachment and permeability of these variants. The results of tensile and compressive tests on these CG scaffolds and of bending tests on the individual struts that define the scaffold network are reported here. The CG scaffold variants exhibited stress-strain behavior characteristic of low-density, open-cell foams with distinct linear elastic, collapse plateau and densification regimes. Scaffolds with equiaxed pores were found to be mechanically isotropic. The independent effects of hydration level, pore size, crosslink density and relative density on the mechanical properties was determined. Independent control over scaffold stiffness and pore size was obtained. Good agreement was observed between experimental results of scaffold mechanical characterization and low-density, open-cell foam model predictions for uniform scaffolds. The characterized scaffold variants provide a standardized framework with defined extracellular environments (microstructure, mechanics) for in vitro studies of the mechanical interactions between cells and scaffolds as well as in vivo tissue engineering studies.

Microstructural characterization of high-carbon ferrochromium

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

Lesko, A.; Navara, E.

1996-04-01

Light optical and scanning electron microscopy techniques were used for high-carbon ferrochromium microstructural analysis. Different microstructures were observed for industrially and laboratory-produced ferroalloys. Primary carbides of M{sub 7}C{sub 3} with chromium ferrite were found in the industrially produced, slowly solidified, and cooled ferroalloy, while primary M{sub 7}C{sub 3} carbides accompanied a eutectic mixture of M{sub 7}C{sub 3} carbides and chromium ferrite in the laboratory-melted and in the water-solidified and water-cooled materials. Different microstructural arrangements are directly related to the friability properties of this material, which characterizes its resistance to abrasion on handling and impact. In ferrochromium upgraded by carbon contentmore » reduction, the eutectic M{sub 7}C{sub 3} hexagonal carbides are partly replaced by M{sub 23}C{sub 6} dendritic carbides. The presence of dendritic carbides in the ferrochromium eutectic microstructure can be interpreted as a proof of a lower carbon content, raising the commercial value of the ferroalloy. The hexagonal M{sub 7}C{sub 3} carbides exhibited a central hollow along the longitudinal axis, and on metallographic samples they looked like screw nuts. A model of the solidification mechanism for such crystals is proposed.« less

Imaging of Scleral Collagen Deformation Using Combined Confocal Raman Microspectroscopy and Polarized Light Microscopy Techniques.

PubMed

Chakraborty, Nilay; Wang, Mian; Solocinski, Jason; Kim, Wonsuk; Argento, Alan

2016-01-01

This work presents an optospectroscopic characterization technique for soft tissue microstructure using site-matched confocal Raman microspectroscopy and polarized light microscopy. Using the technique, the microstructure of soft tissue samples is directly observed by polarized light microscopy during loading while spatially correlated spectroscopic information is extracted from the same plane, verifying the orientation and arrangement of the collagen fibers. Results show the response and orientation of the collagen fiber arrangement in its native state as well as during tensile and compressive loadings in a porcine sclera model. An example is also given showing how the data can be used with a finite element program to estimate the strain in individual collagen fibers. The measurements demonstrate features that indicate microstructural reorganization and damage of the sclera's collagen fiber arrangement under loading. The site-matched confocal Raman microspectroscopic characterization of the tissue provides a qualitative measure to relate the change in fibrillar arrangement with possible chemical damage to the collagen microstructure. Tests and analyses presented here can potentially be used to determine the stress-strain behavior, and fiber reorganization of the collagen microstructure in soft tissue during viscoelastic response.

Characterization of ultra-fine grained aluminum produced by accumulative back extrusion (ABE)

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

Alihosseini, H., E-mail: hamid.alihossieni@gmail.com; Materials Science and Engineering Department, Engineering School, Amirkabir University, Tehran; Faraji, G.

2012-06-15

In the present work, the microstructural evolutions and microhardness of AA1050 subjected to one, two and three passes of accumulative back extrusion (ABE) were investigated. The microstructural evolutions were characterized using transmission electron microscopy. The results revealed that applying three passes of accumulative back extrusion led to significant grain refinement. The initial grain size of 47 {mu}m was refined to the grains of 500 nm after three passes of ABE. Increasing the number of passes resulted in more decrease in grain size, better microstructure homogeneity and increase in the microhardness. The cross-section of ABEed specimen consisted of two different zones:more » (i) shear deformation zone, and (ii) normal deformation zone. The microhardness measurements indicated that the hardness increased from the initial value of 31 Hv to 67 Hv, verifying the significant microstructural refinement via accumulative back extrusion. - Highlights: Black-Right-Pointing-Pointer A significant grain refinement can be achieved in AA1050, Al alloy by applying ABE. Black-Right-Pointing-Pointer Microstructural homogeneity of ABEed samples increased by increasing the number of ABE cycles. Black-Right-Pointing-Pointer A substantial increase in the hardness, from 31 Hv to 67 Hv, was recorded.« less

Microstructure Development in Electron Beam-Melted Inconel 718 and Associated Tensile Properties

DOE PAGES

Kirka, M. M.; Unocic, K. A.; Raghavan, N.; ...

2016-02-12

During the electron beam melting (EBM) process, builds occur at temperatures in excess of 800°C for nickel-base superalloys such as Inconel 718. When coupled with the temporal differences between the start and end of a build, a top-to-bottom microstructure gradient forms. Characterized in this study is the microstructure gradient and associated tensile property gradient that are common to all EBM Inconel 718 builds. From the characteristic microstructure elements observed in EBM Inconel 718 material, the microstructure gradient can be classified into three distinct regions. Region 1 (top of a build) and is comprised of a cored dendritic structure that includesmore » carbides and Laves phase within the interdendritic regions. Region 2 is an intermediate transition zone characterized by a diffuse dendritic structure, dissolution of the Laves phase, and precipitation of δ needle networks within the interdendritic regions. The bulk structure (Region 3) is comprised of a columnar grain structure lacking dendritic characteristics with δ networks having precipitated within the grain interiors. Mechanically at both 20°C and 650° C, the yield strength, ultimate tensile strength, and elongation at failure exhibit the general trend of increasing with increasing build height.« less

Size-dependent microstructures in rapidly solidified uranium-niobium powder particles

DOE PAGES

McKeown, Joseph T.; Hsiung, Luke L.; Park, Jong M.; ...

2016-06-14

The microstructures of rapidly solidified U-6wt%Nb powder particles synthesized by centrifugal atomization were characterized using scanning electron microscopy and transmission electron microscopy. Observed variations in microstructure are related to particle sizes. All of the powder particles exhibited a two-zone microstructure. The formation of this two-zone microstructure is described by a transition from solidification controlled by internal heat flow and high solidification rate during recalescence (micro-segregation-free or partitionless growth) to solidification controlled by external heat flow with slower solidification rates (dendritic growth with solute redistribution). The extent of partitionless solidification increased with decreasing particle size due to larger undercoolings in smallermore » particles prior to solidification. The metastable phases that formed are related to variations in Nb concentration across the particles. Lastly, the microstructures of the powders were heavily twinned.« less

Microstructural Characteristics of High Rate Plastic Deformation in Elektron™ WE43 Magnesium Alloy

NASA Astrophysics Data System (ADS)

Hamilton, Joseph; Brennan, Sarah T.; Sohn, Yongho; Davis, Bruce; DeLorme, Rick; Cho, Kyu

High strain rate deformation of WE43 magnesium alloy was carried out by high velocity impacts, and the characteristics and mechanisms of microstructural damage were examined. Six samples were subjected to a variety of high velocity impact loadings that resulted in both partial and full damage. Optical, scanning and transmission electron microscopy analyses were performed in order to identify regions of shear localization. These regions were used to map, both quantitatively and qualitatively, the effects of deformation on the microstructure. Shear localization was observed in every sample, and its depth was measured. Evidence of shear localization was observed to a greater extent in samples with partial damage while fracturing was observed more frequently in samples with full damage.

Micromechanical modeling of elastic properties of cortical bone accounting for anisotropy of dense tissue.

PubMed

Salguero, Laura; Saadat, Fatemeh; Sevostianov, Igor

2014-10-17

The paper analyzes the connection between microstructure of the osteonal cortical bone and its overall elastic properties. The existing models either neglect anisotropy of the dense tissue or simplify cortical bone microstructure (accounting for Haversian canals only). These simplifications (related mostly to insufficient mathematical apparatus) complicate quantitative analysis of the effect of microstructural changes - produced by age, microgravity, or some diseases - on the overall mechanical performance of cortical bone. The present analysis fills this gap; it accounts for anisotropy of the dense tissue and uses realistic model of the porous microstructure. The approach is based on recent results of Sevostianov et al. (2005) and Saadat et al. (2012) on inhomogeneities in a transversely-isotropic material. Bone's microstructure is modeled according to books of Martin and Burr (1989), Currey (2002), and Fung (1993) and includes four main families of pores. The calculated elastic constants for porous cortical bone are in agreement with available experimental data. The influence of each of the pore types on the overall moduli is examined. Copyright © 2014 Elsevier Ltd. All rights reserved.

Evaluation of Subsequent Heat Treatment Routes for Near-β Forged TA15 Ti-Alloy

PubMed Central

Sun, Zhichao; Wu, Huili; Yang, He

2016-01-01

TA15 Ti-alloy is widely used to form key load-bearing components in the aerospace field, where excellent service performance is needed. Near-β forging technology provides an attractive way to form these complicated Ti-alloy components but subsequent heat treatment has a great impact on the final microstructure and mechanical properties. Therefore evaluation and determination of the heat treatment route is of particular significance. In this paper, for the near-β forged TA15 alloy, the formation and evolution of microstructures under different subsequent heat treatment routes (annealing, solution and aging, toughening and strengthening) were studied and the cooling mode after forging was also considered. Then, the type and characteristics of the obtained microstructures were discussed through quantitative metallographic analysis. The corresponding mechanical properties (tensile, impact toughness, and fracture toughness) and effects of microstructural characteristics were investigated. Finally, for a required microstructure and performance a reasonable heat treatment route was recommended. The work is of importance for the application and development of near-β forging technology. PMID:28773994

Image-Based Macro-Micro Finite Element Models of a Canine Femur with Implant Design Implications

NASA Astrophysics Data System (ADS)

Ghosh, Somnath; Krishnan, Ganapathi; Dyce, Jonathan

2006-06-01

In this paper, a comprehensive model of a bone-cement-implant assembly is developed for a canine cemented femoral prosthesis system. Various steps in this development entail profiling the canine femur contours by computed tomography (CT) scanning, computer aided design (CAD) reconstruction of the canine femur from CT images, CAD modeling of the implant from implant blue prints and CAD modeling of the interface cement. Finite element analysis of the macroscopic assembly is conducted for stress analysis in individual components of the system, accounting for variation in density and material properties in the porous bone material. A sensitivity analysis is conducted with the macroscopic model to investigate the effect of implant design variables on the stress distribution in the assembly. Subsequently, rigorous microstructural analysis of the bone incorporating the morphological intricacies is conducted. Various steps in this development include acquisition of the bone microstructural data from histological serial sectioning, stacking of sections to obtain 3D renderings of void distributions, microstructural characterization and determination of properties and, finally, microstructural stress analysis using a 3D Voronoi cell finite element method. Generation of the simulated microstructure and analysis by the 3D Voronoi cell finite element model provides a new way of modeling complex microstructures and correlating to morphological characteristics. An inverse calculation of the material parameters of bone by combining macroscopic experiments with microstructural characterization and analysis provides a new approach to evaluating properties without having to do experiments at this scale. Finally, the microstructural stresses in the femur are computed using the 3D VCFEM to study the stress distribution at the scale of the bone porosity. Significant difference is observed between the macroscopic stresses and the peak microscopic stresses at different locations.

Acoustic activation of water-in-oil microemulsions for controlled salt dissolution.

PubMed

Baxamusa, Salmaan; Ehrmann, Paul; Ong, Jemi

2018-06-18

The dynamic nature of the oil-water interface allows for sequestration of material within the dispersed domains of a microemulsion. Microstructural changes should therefore change the dissolution rate of a solid surface in a microemulsion. We hypothesize that microstructural changes due to formulation and cavitation in an acoustic field will enable control over solid dissolution rates. Water-in-oil microemulsions were formulated using cyclohexane, water, Triton X-100, and hexanol. The microstructure and solvation properties of Winsor Type IV formulations were characterized. Dissolution rates of KH 2 PO 4 (KDP), were measured. A kinetic analysis isolated the effect of the microstructure, and rate enhancements due to cavitation effects on the microstructure were characterized by measuring dissolution rates in an ultrasonic field. Dispersed aqueous domains of 2-6 nm radius dissolve a solid block of KDP at 0-10 nm/min. Dissolution rate is governed not by the domain-surface collision frequency but rather by a dissolution probability per domain-surface encounter. Higher probabilities are correlated with larger domains. Rapid and reversible dissolution rate increases of up to 270× were observed under ultrasonic conditions, with <20% of the increase due to bulk heating effects. The rest is attributed to cavitation-induced changes to the domain microstructure, providing a simple method for remotely activating and de-activating dissolution. Copyright © 2018 Elsevier Inc. All rights reserved.

Anisotropic and Heterogeneous Development of Microstructures. Combining Laboratory/Synchrotron X-rays and EBSD on a few SPD Metallic Systems

NASA Astrophysics Data System (ADS)

Bolmaro, Raúl E.; De Vincentis, Natalia S.; Benatti, Emanuel; Kliauga, Andrea M.; Avalos, Martina C.; Schell, Norbert; Brokmeier, Heinz-Günter

2014-08-01

The onset of Severe Plastic Deformation (SPD) regime is quite instructive on the possible origins of the nano-microstructures developed in metals and alloys. It is known that grain fragmentation and dislocation accumulation, among other defects, proceed at different paces depending fundamentally on grain orientations and active deformation mechanisms. There have been many attempts to characterize nano-microstructure anisotropy, leading all of them to sometimes contradictory conclusions. Moreover, the characterizations rely on different measurements techniques and pos-processing approaches, which can be observing different manifestations of the same phenomena. On the current presentation we show a few experimental and computer pos-processing and simulation approaches, applied to some SPD/alloy systems. Williamson-Hall and Convolutional Multiple Whole Profile (CMWP) techniques will be applied to peak broadening analysis on experimental results stemming from laboratory Cu Ka X-rays, and synchrotron radiation from LNLS (Laboratório Nacional de Luz Síncrotron, Campinas, Brazil) and Petra III line (HEMS station, at DESY, Hamburg, Germany). Taking advantage of the EBSD capability of giving information on orientational and topological characteristics of grain boundaries, microstructures, grain sizes, etc., we also performed investigations on dislocation density and Geometrically Necessary Dislocation Boundaries (GNDB) and their correlation with texture components. Orientation dependent nano-microstructures and domain sizes are shown on the scheme of generalized pole figures and discussions provide some hints on nano-microstructure anisotropy.

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

A study of reduced chromium content in a nickel-base superalloy via element substitution and rapid solidification processing. Ph.D. ThesisFinal Report

NASA Technical Reports Server (NTRS)

Powers, William O.

1987-01-01

A study of reduced chromium content in a nickel base superalloy via element substitution and rapid solidification processing was performed. The two elements used as partial substitutes for chromium were Si and Zr. The microstructure of conventionally solidified materials was characterized using microscopy techniques. These alloys were rapidly solidified using the chill block melt spinning technique and the rapidly solidified microstructures were characterized using electron microscopy. The spinning technique and the rapidly solidified microstructures was assessed following heat treatments at 1033 and 1272 K. Rapidly solidified material of three alloys was reduced to particulate form and consolidated using hot isostatic pressing (HIP). The consolidated materials were also characterized using microscopy techniques. In order to evaluate the relative strengths of the consolidated alloys, compression tests were performed at room temperature and 1033 K on samples of as-HIPed and HIPed plus solution treated material. Yield strength, porosity, and oxidation resistance characteristics are given and compared.

Database on Performance of Neutron Irradiated FeCrAl Alloys

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

Field, Kevin G.; Briggs, Samuel A.; Littrell, Ken

The present report summarizes and discusses the database on radiation tolerance for Generation I, Generation II, and commercial FeCrAl alloys. This database has been built upon mechanical testing and microstructural characterization on selected alloys irradiated within the High Flux Isotope Reactor (HFIR) at Oak Ridge National Laboratory (ORNL) up to doses of 13.8 dpa at temperatures ranging from 200°C to 550°C. The structure and performance of these irradiated alloys were characterized using advanced microstructural characterization techniques and mechanical testing. The primary objective of developing this database is to enhance the rapid development of a mechanistic understanding on the radiation tolerancemore » of FeCrAl alloys, thereby enabling informed decisions on the optimization of composition and microstructure of FeCrAl alloys for application as an accident tolerant fuel (ATF) cladding. This report is structured to provide a brief summary of critical results related to the database on radiation tolerance of FeCrAl alloys.« less

Ultrasonic Guided-Wave Scan System Used to Characterize Microstructure and Defects in Ceramic Composites

NASA Technical Reports Server (NTRS)

Roth, Don J.; Cosgriff, Laura M.; Martin, Richard E.; Verrilli, Michael J.; Bhatt, Ramakrishna T.

2004-01-01

Ceramic matrix composites (CMCs) are being developed for advanced aerospace propulsion applications to save weight, improve reuse capability, and increase performance. However, mechanical and environmental loads applied to CMCs can cause discrete flaws and distributed microdamage, significantly reducing desirable physical properties. Such microdamage includes fiber/matrix debonding (interface failure), matrix microcracking, fiber fracture and buckling, oxidation, and second phase formation. A recent study (ref. 1) of the durability of a C/SiC CMC discussed the requirement for improved nondestructive evaluation (NDE) methods for monitoring degradation in these materials. Distributed microdamage in CMCs has proven difficult to characterize nondestructively because of the complex microstructure and macrostructure of these materials. This year, an ultrasonic guided-wave scan system developed at the NASA Glenn Research Center was used to characterize various microstructural and flaw conditions in SiC/SiC (silicon carbide fiber in silicon carbide matrix) and C/SiC (carbon fiber in silicon carbide matrix) CMC samples.

Modeling defect cluster evolution in irradiated structural materials: Focus on comparing to high-resolution experimental characterization studies

DOE PAGES

Wirth, Brian D.; Hu, Xunxiang; Kohnert, Aaron; ...

2015-03-02

Exposure of metallic structural materials to irradiation environments results in significant microstructural evolution, property changes, and performance degradation, which limits the extended operation of current generation light water reactors and restricts the design of advanced fission and fusion reactors. Further, it is well recognized that these irradiation effects are a classic example of inherently multiscale phenomena and that the mix of radiation-induced features formed and the corresponding property degradation depend on a wide range of material and irradiation variables. This inherently multiscale evolution emphasizes the importance of closely integrating models with high-resolution experimental characterization of the evolving radiation-damaged microstructure. Lastly,more » this article provides a review of recent models of the defect microstructure evolution in irradiated body-centered cubic materials, which provide good agreement with experimental measurements, and presents some outstanding challenges, which will require coordinated high-resolution characterization and modeling to resolve.« less

Characterization of bone microstructure using photoacoustic spectrum analysis

NASA Astrophysics Data System (ADS)

Feng, Ting; Kozloff, Kenneth M.; Xu, Guan; Du, Sidan; Yuan, Jie; Deng, Cheri X.; Wang, Xueding

2015-03-01

Osteoporosis is a progressive bone disease that is characterized by a decrease in bone mass and deterioration in microarchitecture. This study investigates the feasibility of characterizing bone microstructure by analyzing the frequency spectrum of the photoacoustic signals from the bone. Modeling and numerical simulation of photoacoustic signals and their frequency-domain analysis were performed on trabecular bones with different mineral densities. The resulting quasilinear photoacoustic spectra were fit by linear regression, from which spectral parameter slope can be quantified. The modeling demonstrates that, at an optical wavelength of 685 nm, bone specimens with lower mineral densities have higher slope. Preliminary experiment on osteoporosis rat tibia bones with different mineral contents has also been conducted. The finding from the experiment has a good agreement with the modeling, both demonstrating that the frequency-domain analysis of photoacoustic signals can provide objective assessment of bone microstructure and deterioration. Considering that photoacoustic measurement is non-ionizing, non-invasive, and has sufficient penetration in both calcified and noncalcified tissues, this new technology holds unique potential for clinical translation.

Droplet Breakup in Expansion-contraction Microchannels

PubMed Central

Zhu, Pingan; Kong, Tiantian; Lei, Leyan; Tian, Xiaowei; Kang, Zhanxiao; Wang, Liqiu

2016-01-01

We investigate the influences of expansion-contraction microchannels on droplet breakup in capillary microfluidic devices. With variations in channel dimension, local shear stresses at the injection nozzle and focusing orifice vary, significantly impacting flow behavior including droplet breakup locations and breakup modes. We observe transition of droplet breakup location from focusing orifice to injection nozzle, and three distinct types of recently-reported tip-multi-breaking modes. By balancing local shear stresses and interfacial tension effects, we determine the critical condition for breakup location transition, and characterize the tip-multi-breaking mode quantitatively. In addition, we identify the mechanism responsible for the periodic oscillation of inner fluid tip in tip-multi-breaking mode. Our results offer fundamental understanding of two-phase flow behaviors in expansion-contraction microstructures, and would benefit droplet generation, manipulation and design of microfluidic devices. PMID:26899018

Fiber networks amplify active stress

PubMed Central

Ronceray, Pierre; Broedersz, Chase P.

2016-01-01

Large-scale force generation is essential for biological functions such as cell motility, embryonic development, and muscle contraction. In these processes, forces generated at the molecular level by motor proteins are transmitted by disordered fiber networks, resulting in large-scale active stresses. Although these fiber networks are well characterized macroscopically, this stress generation by microscopic active units is not well understood. Here we theoretically study force transmission in these networks. We find that collective fiber buckling in the vicinity of a local active unit results in a rectification of stress towards strongly amplified isotropic contraction. This stress amplification is reinforced by the networks’ disordered nature, but saturates for high densities of active units. Our predictions are quantitatively consistent with experiments on reconstituted tissues and actomyosin networks and shed light on the role of the network microstructure in shaping active stresses in cells and tissue. PMID:26921325

Lifespan Trajectories of White Matter Changes in Rhesus Monkeys.

PubMed

Kubicki, M; Baxi, M; Pasternak, O; Tang, Y; Karmacharya, S; Chunga, N; Lyall, A E; Rathi, Y; Eckbo, R; Bouix, S; Mortazavi, F; Papadimitriou, G; Shenton, M E; Westin, C F; Killiany, R; Makris, N; Rosene, D L

2018-04-26

Progress in neurodevelopmental brain research has been achieved through the use of animal models. Such models not only help understanding biological changes that govern brain development, maturation and aging, but are also essential for identifying possible mechanisms of neurodevelopmental and age-related chronic disorders, and to evaluate possible interventions with potential relevance to human disease. Genetic relationship of rhesus monkeys to humans makes those animals a great candidate for such models. With the typical lifespan of 25 years, they undergo cognitive maturation and aging that is similar to this observed in humans. Quantitative structural neuroimaging has been proposed as one of the candidate in vivo biomarkers for tracking white matter brain maturation and aging. While lifespan trajectories of white matter changes have been mapped in humans, such knowledge is not available for nonhuman primates. Here, we analyze and model lifespan trajectories of white matter microstructure using in vivo diffusion imaging in a sample of 44 rhesus monkeys. We report quantitative parameters (including slopes and peaks) of lifespan trajectories for 8 individual white matter tracts. We show different trajectories for cellular and extracellular microstructural imaging components that are associated with white matter maturation and aging, and discuss similarities and differences between those in humans and rhesus monkeys, the importance of our findings, and future directions for the field.Significance Statement: Quantitative structural neuroimaging has been proposed as one of the candidate in vivo biomarkers for tracking brain maturation and aging. While lifespan trajectories of structural white matter changes have been mapped in humans, such knowledge is not available for rhesus monkeys. We present here results of the analysis and modeling of the lifespan trajectories of white matter microstructure using in vivo diffusion imaging in a sample of 44 rhesus monkeys (age 4-27). We report and anatomically map lifespan changes related to cellular and extracellular microstructural components that are associated with white matter maturation and aging.

Microstructure characterization and corrosion resistance properties of Pb-Sb alloys for lead acid battery spine produced by different casting methods.

PubMed

Seikh, Asiful H; Sherif, El-Sayed M; Khan Mohammed, Sohail M A; Baig, Muneer; Alam, Mohammad Asif; Alharthi, Nabeel

2018-01-01

The aim of this study is to find out the microstructure, hardness, and corrosion resistance of Pb-5%Sb spine alloy. The alloy has been produced by high pressure die casting (HPDC), medium pressure die casting (AS) and low pressure die casting (GS) methods, respectively. The microstructure was characterized by using optical microscopy and scanning electron microscopy (SEM). The hardness was also reported. The corrosion resistance of the spines in 0.5M H2SO4 solution has been analyzed by measuring the weight loss, impedance spectroscopy and the potentiodynamic polarization techniques. It has been found that the spine produced by HPDC has defect-free fine grain structure resulting improvement in hardness and excellent corrosion resistance.

Microstructure characterization and corrosion resistance properties of Pb-Sb alloys for lead acid battery spine produced by different casting methods

PubMed Central

Baig, Muneer; Alam, Mohammad Asif; Alharthi, Nabeel

2018-01-01

The aim of this study is to find out the microstructure, hardness, and corrosion resistance of Pb-5%Sb spine alloy. The alloy has been produced by high pressure die casting (HPDC), medium pressure die casting (AS) and low pressure die casting (GS) methods, respectively. The microstructure was characterized by using optical microscopy and scanning electron microscopy (SEM). The hardness was also reported. The corrosion resistance of the spines in 0.5M H2SO4 solution has been analyzed by measuring the weight loss, impedance spectroscopy and the potentiodynamic polarization techniques. It has been found that the spine produced by HPDC has defect-free fine grain structure resulting improvement in hardness and excellent corrosion resistance. PMID:29668709

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

Microstructural processes in irradiated materials

NASA Astrophysics Data System (ADS)

Byun, Thak Sang; Morgan, Dane; Jiao, Zhijie; Almer, Jonathan; Brown, Donald

2016-04-01

These proceedings contain the papers presented at two symposia, the Microstructural Processes in Irradiated Materials (MPIM) and Characterization of Nuclear Reactor Materials and Components with Neutron and Synchrotron Radiation, held in the TMS 2015, 144th Annual Meeting & Exhibition at Walt Disney World, Orlando, Florida, USA on March 15-19, 2015.

3D Microstructure Effects in Ni-YSZ Anodes: Influence of TPB Lengths on the Electrochemical Performance.

PubMed

Pecho, Omar M; Mai, Andreas; Münch, Beat; Hocker, Thomas; Flatt, Robert J; Holzer, Lorenz

2015-10-21

3D microstructure-performance relationships in Ni-YSZ anodes for electrolyte-supported cells are investigated in terms of the correlation between the triple phase boundary (TPB) length and polarization resistance ( R pol ). Three different Ni-YSZ anodes of varying microstructure are subjected to eight reduction-oxidation (redox) cycles at 950 °C. In general the TPB lengths correlate with anode performance . However, the quantitative results also show that there is no simplistic relationship between TPB and R pol . The degradation mechanism strongly depends on the initial microstructure. Finer microstructures exhibit lower degradation rates of TPB and R pol . In fine microstructures, TPB loss is found to be due to Ni coarsening, while in coarse microstructures reduction of active TPB results mainly from loss of YSZ percolation. The latter is attributed to weak bottlenecks associated with lower sintering activity of the coarse YSZ. The coarse anode suffers from complete loss of YSZ connectivity and associated drop of TPB active by 93%. Surprisingly, this severe microstructure degradation did not lead to electrochemical failure. Mechanistic scenarios are discussed for different anode microstructures. These scenarios are based on a model for coupled charge transfer and transport, which allows using TPB and effective properties as input. The mechanistic scenarios describe the microstructure influence on current distributions, which explains the observed complex relationship between TPB lengths and anode performances. The observed loss of YSZ percolation in the coarse anode is not detrimental because the electrochemical activity is concentrated in a narrow active layer. The anode performance can be predicted reliably if the volume-averaged properties (TPB active , effective ionic conductivity) are corrected for the so-called short-range effect, which is particularly important in cases with a narrow active layer.

3D Microstructure Effects in Ni-YSZ Anodes: Influence of TPB Lengths on the Electrochemical Performance

PubMed Central

Pecho, Omar M.; Mai, Andreas; Münch, Beat; Hocker, Thomas; Flatt, Robert J.; Holzer, Lorenz

2015-01-01

3D microstructure-performance relationships in Ni-YSZ anodes for electrolyte-supported cells are investigated in terms of the correlation between the triple phase boundary (TPB) length and polarization resistance (Rpol). Three different Ni-YSZ anodes of varying microstructure are subjected to eight reduction-oxidation (redox) cycles at 950 °C. In general the TPB lengths correlate with anode performance. However, the quantitative results also show that there is no simplistic relationship between TPB and Rpol. The degradation mechanism strongly depends on the initial microstructure. Finer microstructures exhibit lower degradation rates of TPB and Rpol. In fine microstructures, TPB loss is found to be due to Ni coarsening, while in coarse microstructures reduction of active TPB results mainly from loss of YSZ percolation. The latter is attributed to weak bottlenecks associated with lower sintering activity of the coarse YSZ. The coarse anode suffers from complete loss of YSZ connectivity and associated drop of TPBactive by 93%. Surprisingly, this severe microstructure degradation did not lead to electrochemical failure. Mechanistic scenarios are discussed for different anode microstructures. These scenarios are based on a model for coupled charge transfer and transport, which allows using TPB and effective properties as input. The mechanistic scenarios describe the microstructure influence on current distributions, which explains the observed complex relationship between TPB lengths and anode performances. The observed loss of YSZ percolation in the coarse anode is not detrimental because the electrochemical activity is concentrated in a narrow active layer. The anode performance can be predicted reliably if the volume-averaged properties (TPBactive, effective ionic conductivity) are corrected for the so-called short-range effect, which is particularly important in cases with a narrow active layer. PMID:28793624

Evaluation of factors affecting the edge formability of two hot rolled multiphase steels

NASA Astrophysics Data System (ADS)

Mukherjee, Monideepa; Tiwari, Sumit; Bhattacharya, Basudev

2018-02-01

In this study, the effect of various factors on the hole expansion ratio and hence on the edge formability of two hot rolled multiphase steels, one with a ferrite-martensite microstructure and the other with a ferrite-bainite microstructure, was investigated through systematic microstructural and mechanical characterization. The study revealed that the microstructure of the steels, which determines their strain hardening capacity and fracture resistance, is the principal factor controlling edge formability. The influence of other factors such as tensile strength, ductility, anisotropy, and thickness, though present, are secondary. A critical evaluation of the available empirical models for hole expansion ratio prediction is also presented.

A review: applications of the phase field method in predicting microstructure and property evolution of irradiated nuclear materials

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

Li, Yulan; Hu, Shenyang; Sun, Xin

Here, complex microstructure changes occur in nuclear fuel and structural materials due to the extreme environments of intense irradiation and high temperature. This paper evaluates the role of the phase field method in predicting the microstructure evolution of irradiated nuclear materials and the impact on their mechanical, thermal, and magnetic properties. The paper starts with an overview of the important physical mechanisms of defect evolution and the significant gaps in simulating microstructure evolution in irradiated nuclear materials. Then, the phase field method is introduced as a powerful and predictive tool and its applications to microstructure and property evolution in irradiatedmore » nuclear materials are reviewed. The review shows that (1) Phase field models can correctly describe important phenomena such as spatial-dependent generation, migration, and recombination of defects, radiation-induced dissolution, the Soret effect, strong interfacial energy anisotropy, and elastic interaction; (2) The phase field method can qualitatively and quantitatively simulate two-dimensional and three-dimensional microstructure evolution, including radiation-induced segregation, second phase nucleation, void migration, void and gas bubble superlattice formation, interstitial loop evolution, hydrate formation, and grain growth, and (3) The Phase field method correctly predicts the relationships between microstructures and properties. The final section is dedicated to a discussion of the strengths and limitations of the phase field method, as applied to irradiation effects in nuclear materials.« less

A review: applications of the phase field method in predicting microstructure and property evolution of irradiated nuclear materials

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

Li, Yulan; Hu, Shenyang; Sun, Xin

Complex microstructure changes occur in nuclear fuel and structural materials due to the extreme environments of intense irradiation and high temperature. This paper evaluates the role of the phase field (PF) method in predicting the microstructure evolution of irradiated nuclear materials and the impact on their mechanical, thermal, and magnetic properties. The paper starts with an overview of the important physical mechanisms of defect evolution and the significant gaps in simulating microstructure evolution in irradiated nuclear materials. Then, the PF method is introduced as a powerful and predictive tool and its applications to microstructure and property evolution in irradiated nuclearmore » materials are reviewed. The review shows that 1) FP models can correctly describe important phenomena such as spatial dependent generation, migration, and recombination of defects, radiation-induced dissolution, the Soret effect, strong interfacial energy anisotropy, and elastic interaction; 2) The PF method can qualitatively and quantitatively simulate 2-D and 3-D microstructure evolution, including radiation-induced segregation, second phase nucleation, void migration, void and gas bubble superlattice formation, interstitial loop evolution, hydrate formation, and grain growth, and 3) The FP method correctly predicts the relationships between microstructures and properties. The final section is dedicated to a discussion of the strengths and limitations of the PF method, as applied to irradiation effects in nuclear materials.« less

A review: applications of the phase field method in predicting microstructure and property evolution of irradiated nuclear materials

DOE PAGES

Li, Yulan; Hu, Shenyang; Sun, Xin; ...

2017-04-14

Here, complex microstructure changes occur in nuclear fuel and structural materials due to the extreme environments of intense irradiation and high temperature. This paper evaluates the role of the phase field method in predicting the microstructure evolution of irradiated nuclear materials and the impact on their mechanical, thermal, and magnetic properties. The paper starts with an overview of the important physical mechanisms of defect evolution and the significant gaps in simulating microstructure evolution in irradiated nuclear materials. Then, the phase field method is introduced as a powerful and predictive tool and its applications to microstructure and property evolution in irradiatedmore » nuclear materials are reviewed. The review shows that (1) Phase field models can correctly describe important phenomena such as spatial-dependent generation, migration, and recombination of defects, radiation-induced dissolution, the Soret effect, strong interfacial energy anisotropy, and elastic interaction; (2) The phase field method can qualitatively and quantitatively simulate two-dimensional and three-dimensional microstructure evolution, including radiation-induced segregation, second phase nucleation, void migration, void and gas bubble superlattice formation, interstitial loop evolution, hydrate formation, and grain growth, and (3) The Phase field method correctly predicts the relationships between microstructures and properties. The final section is dedicated to a discussion of the strengths and limitations of the phase field method, as applied to irradiation effects in nuclear materials.« less

On oscillatory microstructure during cellular growth of directionally solidified Sn–36at.%Ni peritectic alloy

PubMed Central

Peng, Peng; Li, Xinzhong; Li, Jiangong; Su, Yanqing; Guo, Jingjie

2016-01-01

An oscillatory microstructure has been observed during deep-cellular growth of directionally solidified Sn–36at.%Ni hyperperitectic alloy containing intermetallic compounds with narrow solubility range. This oscillatory microstructure with a dimension of tens of micrometers has been observed for the first time. The morphology of this wave-like oscillatory structure is similar to secondary dendrite arms, and can be observed only in some local positions of the sample. Through analysis such as successive sectioning of the sample, it can be concluded that this oscillatory microstructure is caused by oscillatory convection of the mushy zone during solidification. And the influence of convection on this oscillatory microstructure was characterized through comparison between experimental and calculations results on the wavelength. Besides, the change in morphology of this oscillatory microstructure has been proved to be caused by peritectic transformation during solidification. Furthermore, the melt concentration increases continuously during solidification of intermetallic compounds with narrow solubility range, which helps formation of this oscillatory microstructure. PMID:27066761

On oscillatory microstructure during cellular growth of directionally solidified Sn-36at.%Ni peritectic alloy.

PubMed

Peng, Peng; Li, Xinzhong; Li, Jiangong; Su, Yanqing; Guo, Jingjie

2016-04-12

An oscillatory microstructure has been observed during deep-cellular growth of directionally solidified Sn-36at.%Ni hyperperitectic alloy containing intermetallic compounds with narrow solubility range. This oscillatory microstructure with a dimension of tens of micrometers has been observed for the first time. The morphology of this wave-like oscillatory structure is similar to secondary dendrite arms, and can be observed only in some local positions of the sample. Through analysis such as successive sectioning of the sample, it can be concluded that this oscillatory microstructure is caused by oscillatory convection of the mushy zone during solidification. And the influence of convection on this oscillatory microstructure was characterized through comparison between experimental and calculations results on the wavelength. Besides, the change in morphology of this oscillatory microstructure has been proved to be caused by peritectic transformation during solidification. Furthermore, the melt concentration increases continuously during solidification of intermetallic compounds with narrow solubility range, which helps formation of this oscillatory microstructure.

Fe-Cr-Mo based ODS alloys via spark plasma sintering: A combinational characterization study by TEM and APT

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

Y. Q. Wu; K. N. Allahar; J. Burns

2013-08-01

Nanoscale oxides play an important role in oxide dispersion strengthened (ODS) alloys for improved high temperature creep resistance and enhanced radiation damage tolerance. In this study, transmission electron microscopy (TEM) and atom probe tomography (APT) were combined to investigate two novel Fe-16Cr-3Mo (wt.%) based ODS alloys. Spark plasma sintering (SPS) was used to consolidate the ODS alloys from powders that were milled with 0.5 wt.% Y2O3 powder only or with Y2O3 powder and 1 wt.% Ti. TEM characterization revealed that both alloys have a bimodal structure of nanometer-size (~ 100 – 500 nm) and micron-size grains with nanostructured oxide precipitatesmore » formed along and close to grain boundaries with diameters ranging from five to tens of nanometers. APT provides further quantitative analyses of the oxide precipitates, and also reveals Mo segregation at grain boundaries next to oxide precipitates. The alloys with and without Ti are compared based on their microstructures.« less

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.

Microstructure and mechanical properties of Al-3Fe alloy processed by equal channel angular extrusion

NASA Astrophysics Data System (ADS)

Fuxiao, Yu; Fang, Liu; Dazhi, Zhao; Toth, Laszlo S.

2014-08-01

Al-Fe alloys are attractive for applications at temperatures beyond those normally associated with the conventional aluminum alloys. Under proper solidification condition, a full eutectic microstructure can be generated in Al-Fe alloys at Fe concentration well in excess of the eutectic composition of 1.8 wt.% Fe. The microstructure in this case is characterized by the metastable regular eutectic Al-Al6Fe fibers of nano-scale in diameter, instead of the equilibrium eutectic Al-Al3Fe phase. In this study, the microstructure and mechanical properties of the Al-3Fe alloy with metastable Al6Fe particles deformed by equal channel angular extrusion were investigated. Severe plastic deformation results in a microstructure consisting of submicron equiaxed Al grains with a uniform distribution of submicron Al6Fe particles on the grain boundaries. The room temperature tensile properties of the alloy with this microstructure will be presented.

Microstructural Characterization of Friction Stir Welded Aluminum-Steel Joints

NASA Astrophysics Data System (ADS)

Patterson, Erin E.; Hovanski, Yuri; Field, David P.

2016-06-01

This work focuses on the microstructural characterization of aluminum to steel friction stir welded joints. Lap weld configuration coupled with scribe technology used for the weld tool have produced joints of adequate quality, despite the significant differences in hardness and melting temperatures of the alloys. Common to friction stir processes, especially those of dissimilar alloys, are microstructural gradients including grain size, crystallographic texture, and precipitation of intermetallic compounds. Because of the significant influence that intermetallic compound formation has on mechanical and ballistic behavior, the characterization of the specific intermetallic phases and the degree to which they are formed in the weld microstructure is critical to predicting weld performance. This study used electron backscatter diffraction, energy dispersive spectroscopy, scanning electron microscopy, and Vickers micro-hardness indentation to explore and characterize the microstructures of lap friction stir welds between an applique 6061-T6 aluminum armor plate alloy and a RHA homogeneous armor plate steel alloy. Macroscopic defects such as micro-cracks were observed in the cross-sectional samples, and binary intermetallic compound layers were found to exist at the aluminum-steel interfaces of the steel particles stirred into the aluminum weld matrix and across the interfaces of the weld joints. Energy dispersive spectroscopy chemical analysis identified the intermetallic layer as monoclinic Al3Fe. Dramatic decreases in grain size in the thermo-mechanically affected zones and weld zones that evidenced grain refinement through plastic deformation and recrystallization. Crystallographic grain orientation and texture were examined using electron backscatter diffraction. Striated regions in the orientations of the aluminum alloy were determined to be the result of the severe deformation induced by the complex weld tool geometry. Many of the textures observed in the weld zone and thermo-mechanically affected zones exhibited shear texture components; however, there were many textures that deviated from ideal simple shear. Factors affecting the microstructure which are characteristic of the friction stir welding process, such as post-recrystallization deformation and complex deformation induced by tool geometry were discussed as causes for deviation from simple shear textures.

Ultrasonic nondestructive evaluation, microstructure, and mechanical property interrelations

NASA Technical Reports Server (NTRS)

Vary, A.

1984-01-01

Ultrasonic techniques for mechanical property characterizations are reviewed and conceptual models are advanced for explaining and interpreting the empirically based results. At present, the technology is generally empirically based and is emerging from the research laboratory. Advancement of the technology will require establishment of theoretical foundations for the experimentally observed interrelations among ultrasonic measurements, mechanical properties, and microstructure. Conceptual models are applied to ultrasonic assessment of fracture toughness to illustrate an approach for predicting correlations found among ultrasonic measurements, microstructure, and mechanical properties.

Final Project Report CFA-14-6357: A New Paradigm for Understanding Multiphase Ceramic Waste Form Performance

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

Brinkman, Kyle; Bordia, Rajendra; Reifsnider, Kenneth

This project fabricated model multiphase ceramic waste forms with processing-controlled microstructures followed by advanced characterization with synchrotron and electron microscopy-based 3D tomography to provide elemental and chemical state-specific information resulting in compositional phase maps of ceramic composites. Details of 3D microstructural features were incorporated into computer-based simulations using durability data for individual constituent phases as inputs in order to predict the performance of multiphase waste forms with varying microstructure and phase connectivity.

Investigation of the microstructure and mineralogical composition of urinary calculi fragments by synchrotron radiation X-ray microtomography: a feasibility study.

PubMed

Kaiser, Jozef; Holá, Markéta; Galiová, Michaela; Novotný, Karel; Kanický, Viktor; Martinec, Petr; Sčučka, Jiří; Brun, Francesco; Sodini, Nicola; Tromba, Giuliana; Mancini, Lucia; Kořistková, Tamara

2011-08-01

The outcomes from the feasibility study on utilization of synchrotron radiation X-ray microtomography (SR-μCT) to investigate the texture and the quantitative mineralogical composition of selected calcium oxalate-based urinary calculi fragments are presented. The comparison of the results obtained by SR-μCT analysis with those derived from current standard analytical approaches is provided. SR-μCT is proved as a potential effective technique for determination of texture, 3D microstructure, and composition of kidney stones.

A fractal derivative model for the characterization of anomalous diffusion in magnetic resonance imaging

NASA Astrophysics Data System (ADS)

Liang, Yingjie; Ye, Allen Q.; Chen, Wen; Gatto, Rodolfo G.; Colon-Perez, Luis; Mareci, Thomas H.; Magin, Richard L.

2016-10-01

Non-Gaussian (anomalous) diffusion is wide spread in biological tissues where its effects modulate chemical reactions and membrane transport. When viewed using magnetic resonance imaging (MRI), anomalous diffusion is characterized by a persistent or 'long tail' behavior in the decay of the diffusion signal. Recent MRI studies have used the fractional derivative to describe diffusion dynamics in normal and post-mortem tissue by connecting the order of the derivative with changes in tissue composition, structure and complexity. In this study we consider an alternative approach by introducing fractal time and space derivatives into Fick's second law of diffusion. This provides a more natural way to link sub-voxel tissue composition with the observed MRI diffusion signal decay following the application of a diffusion-sensitive pulse sequence. Unlike previous studies using fractional order derivatives, here the fractal derivative order is directly connected to the Hausdorff fractal dimension of the diffusion trajectory. The result is a simpler, computationally faster, and more direct way to incorporate tissue complexity and microstructure into the diffusional dynamics. Furthermore, the results are readily expressed in terms of spectral entropy, which provides a quantitative measure of the overall complexity of the heterogeneous and multi-scale structure of biological tissues. As an example, we apply this new model for the characterization of diffusion in fixed samples of the mouse brain. These results are compared with those obtained using the mono-exponential, the stretched exponential, the fractional derivative, and the diffusion kurtosis models. Overall, we find that the order of the fractal time derivative, the diffusion coefficient, and the spectral entropy are potential biomarkers to differentiate between the microstructure of white and gray matter. In addition, we note that the fractal derivative model has practical advantages over the existing models from the perspective of computational accuracy and efficiency.

Deformation Behavior of Ultra-Strong and Ductile Mg-Gd-Y-Zn-Zr Alloy with Bimodal Microstructure

NASA Astrophysics Data System (ADS)

Xu, C.; Fan, G. H.; Nakata, T.; Liang, X.; Chi, Y. Q.; Qiao, X. G.; Cao, G. J.; Zhang, T. T.; Huang, M.; Miao, K. S.; Zheng, M. Y.; Kamado, S.; Xie, H. L.

2018-02-01

An ultra-strong and ductile Mg-8.2Gd-3.8Y-1Zn-0.4Zr (wt pct) alloy was developed by using hot extrusion to modify the microstructure via forced-air cooling and an artificial aging treatment. A superior strength-ductility balance was obtained that had a tensile yield strength of 466 MPa and an elongation to failure of 14.5 pct. The local strain evolution during the in situ testing of the ultra-strong and ductile alloy was quantitatively analyzed with high-resolution electron backscattered diffraction and digital image correlation. The fracture behavior during the tensile test was characterized by synchrotron X-ray tomography along with SEM and STEM observations. The alloy showed a bimodal microstructure, consisting of dynamically recrystallized (DRXed) grains with random orientations and elongated hot-worked grains with < { 10{\\bar{1}}0} > parallel to the extrusion direction. The DRXed grains were deformed by the basal <;a> slip and the hot-worked grains were deformed by the prismatic slip dominantly. The strain evolution analysis indicated that the multilayered structure relaxed the strain localization via strain transfer from the DRXed to the hot-worked regions, which led to the high ductility of the alloy. Precipitation of the γ' on basal planes and the β' phases on the prismatic planes of the α-Mg generated closed volumes, which enhanced the strength by pinning dislocations effectively, and contributed to the high ductility by impeding the propagation of micro-cracks inside the grains. The deformation incompatibility between the hot-worked grains and the arched block-shaped long-period stacking ordered (LPSO) phases induced the crack initiation and propagation, which fractured the alloy.

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

Ning, Yongquan, E-mail: luckyning@nwpu.edu.cn; Huang, Shibo; Fu, M.W.

Microstructural characterization, formation mechanism and fracture behavior of the needle δ phase in Fe–Ni–Cr type superalloys with high Nb content (GH4169, equivalent to Inconel 718) have been quantitatively investigated in this research. The typical microstructures of δ phases with the stick, mixed and needle shapes obviously present in Inconel 718 after the isothermal upsetting at the temperature of 980–1060 °C with the initial strain rate of 10{sup −3}–10{sup −1} s{sup −1}. It is found that the shape of the δ phase has a great effect on the mechanical properties of the alloy, viz., the stick δ phase behaves good plasticitymore » and the needle δ phase has good strength. In addition, the needle δ phase can be used to control the grain size as it can prevent grain growth. The combined effect of the localized necking and microvoid coalescence leads to the final ductile fracture of the GH4169 components with the needle δ phase. Both dislocation motion and atom diffusion are the root-cause for the needle δ phase to be firstly separated at grain boundary and then at sub-boundary. The formation mechanism of the needle δ phase is the new finding in this research. Furthermore, it is the primary mechanism for controlling the needle δ phase in Fe–Ni–Cr type superalloys with high Nb content. - Highlights: • Shape of the δ phase takes great effect on mechanical property. • Needle δ phase plays a great role to prevent grain growth. • Needle δ phase can enhance the fracture strength. • Microstructure mechanism of the needle δ phase has been investigated. • Fracture behavior of the needle δ phase has been studied.« less

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.

Analytical ultrasonics for structural materials

NASA Technical Reports Server (NTRS)

Kupperman, D. S.

1986-01-01

The application of ultrasonic velocity and attenuation measurements to characterize the microstructure of structural materials is discussed. Velocity measurements in cast stainless steel are correlated with microstructural variations ranging from equiaxed (elastically isotropic) to columnar (elastically anisotropic) grain structure. The effect of the anisotropic grain structure on the deviation of ultrasonic waves in cast stainless steel is also reported. Field-implementable techniques for distinguishing equiaxed from columnar grain structures in cast strainless steel structural members are presented. The application of ultrasonic velocity measurements to characterize structural ceramics in the green state is also discussed.

The NBS: Processing/Microstructure/Property Relationships in 2024 Aluminum Alloy Plates

NASA Technical Reports Server (NTRS)

Ives, L. K.; Swartzendruber, W. J.; Boettinger, W. J.; Rosen, M.; Ridder, S. D.

1983-01-01

As received plates of 2024 aluminum alloy were examined. Topics covered include: solidification segregation studies; microsegregation and macrosegregation in laboratory and commercially cast ingots; C-curves and nondestructive evaluation; time-temperature precipitation diagrams and the relationships between mechanical properties and NDE measurements; transmission electron microscopy studies; the relationship between microstructure and properties; ultrasonic characterization; eddy-current conductivity characterization; the study of aging process by means of dynamic eddy current measurements; and Heat flow-property predictions, property degradations due to improve quench from the solution heat treatment temperature.

Microstructures of BN/SiC coatings on nicalon fibers

NASA Technical Reports Server (NTRS)

Dickerson, R. M.; Singh, M.

1995-01-01

The microstructures of Nicalon silicon carbide (SiC) fibers and layered coatings of boron nitride (BN) followed by chemical vapor infiltrated silicon carbide (CVI-SiC) were characterized using optical and electron microscopy. Two different precursors and reactions were used to produce the BN layers while the deposition of CVI silicon carbide was nearly identical. Coated tows were examined in cross-section to characterize the chemistry and structures of the constituents and the interfaces. One BN precursor yielded three sublayers while the other gave a relatively homogeneous nanocrystalline layer.

A Sensory Material Approach for Reducing Variability in Additively Manufactured Metal Parts.

PubMed

Franco, B E; Ma, J; Loveall, B; Tapia, G A; Karayagiz, K; Liu, J; Elwany, A; Arroyave, R; Karaman, I

2017-06-15

Despite the recent growth in interest for metal additive manufacturing (AM) in the biomedical and aerospace industries, variability in the performance, composition, and microstructure of AM parts remains a major impediment to its widespread adoption. The underlying physical mechanisms, which cause variability, as well as the scale and nature of variability are not well understood, and current methods are ineffective at capturing these details. Here, a Nickel-Titanium alloy is used as a sensory material in order to quantitatively, and rather rapidly, observe compositional and/or microstructural variability in selective laser melting manufactured parts; thereby providing a means to evaluate the role of process parameters on the variability. We perform detailed microstructural investigations using transmission electron microscopy at various locations to reveal the origins of microstructural variability in this sensory material. This approach helped reveal how reducing the distance between adjacent laser scans below a critical value greatly reduces both the in-sample and sample-to-sample variability. Microstructural investigations revealed that when the laser scan distance is wide, there is an inhomogeneity in subgrain size, precipitate distribution, and dislocation density in the microstructure, responsible for the observed variability. These results provide an important first step towards understanding the nature of variability in additively manufactured parts.

Effect of pressure and shielding gas on the microstructure of hyperbaric metal cored GMAW welds down to 111 bar

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

Jorge, J.C.F.; Santos, V.R. dos; Santos, J.F. dos

1995-12-31

The microstructural evolution of hyperbaric C-Mn weld metals was studied by means of bead-on-plate welds deposit with GMAW process using a commercial metal cored wire. The welding was carried out in the flat position in the range of 51 bar to 111 bar with He+ CO{sub 2} as shielding gas, which CO{sub 2} content varied from 0.1% to 0.8 %. The microstructures were quantitatively analyzed by optical microscopy to evaluate the amount of constituents according to the IIW/IIS terminology. The results showed that all weld metals presented great amounts of acicular ferrite and a stronger influence of pressure on microstructuremore » compared to the influence of the shielding gas.« less

X-ray studies of dynamic aging in an aluminum alloy subjected to severe plastic deformation

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

Sitdikov, V.D., E-mail: svil@mail.rb.ru; Laboratory for Mechanics of Bulk Nanomaterials, Saint Petersburg State University, 28 Universitetsky pr., Saint Petersburg 198504; Chizhov, P.S.

In this work, X-ray scattering methods were applied for a quantitative characterization of the microstructure of an aluminum alloy of the Al–Mg–Si system during dynamic aging realized through the high pressure torsion technique. A qualitative and quantitative phase analysis of the alloy was performed, together with Al alloy lattice parameter determination. From the reflections broadening the effective size of the coherent scattering domains and the lattice microstrain were determined in the framework of the Halder–Wagner approach. Using the method of small-angle X-ray scattering, the quantitative characteristics of the size, shape and spatial distribution of the secondary phase particles formed inmore » the Al alloy during dynamic aging were established. In order to validate the obtained results, the method of small-angle X-ray scattering was preliminarily tested on similar samples after artificial aging and compared with the results from small-angle neutron diffraction widely known in literature. - Highlights: • Spherical fcc β-Mg2Si precipitates formed in Al 6201 alloy during dynamic aging in the course of severe plastic deformation. • The size, shape and distribution of the precipitates due to artificial and dynamic aging were revealed by SAXS method. • Monoclinic needle-like β' precipitates and Al5FeSi intermetallic phase were detected in 6201 alloy after T6 treatment.« less

Characterization of Microstructure and Thermal Properties of YSZ Coatings Obtained by Axial Suspension Plasma Spraying (ASPS)

NASA Astrophysics Data System (ADS)

Ganvir, Ashish; Curry, Nicholas; Björklund, Stefan; Markocsan, Nicolaie; Nylén, Per

2015-10-01

The paper aims at demonstrating various microstructures which can be obtained using the suspension spraying technique and their respective significance in enhancing the thermal insulation property of a thermal barrier coating. Three different types of coating microstructures are discussed which were produced by the Axial Suspension Plasma Spraying. Detailed characterization of coatings was then performed. Optical and scanning electron microscopy were utilized for microstructure evaluations; x-ray diffraction for phase analysis; water impregnation, image analysis, and mercury intrusion porosimetry for porosity analysis, and laser flash analysis for thermal diffusivity measurements were used. The results showed that Axial Suspension Plasma Spraying can generate vertically cracked, porous, and feathery columnar-type microstructures. Pore size distribution was found in micron, submicron, and nanometer range. Higher overall porosity, the lower density of vertical cracks or inter-column spacing, and higher inter-pass porosity favored thermal insulation property of the coating. Significant increase in thermal diffusivity and conductivity was found at higher temperature, which is believed to be due to the pore rearrangement (sintering and pore coarsening). Thermal conductivity values for these coatings were also compared with electron beam physical vapor deposition (EBPVD) thermal barrier coatings from the literature and found to be much lower.

Characterizing Suspension Plasma Spray Coating Formation Dynamics through Curvature Measurements

NASA Astrophysics Data System (ADS)

Chidambaram Seshadri, Ramachandran; Dwivedi, Gopal; Viswanathan, Vaishak; Sampath, Sanjay

2016-12-01

Suspension plasma spraying (SPS) enables the production of variety of microstructures with unique mechanical and thermal properties. In SPS, a liquid carrier (ethanol/water) is used to transport the sub-micrometric feedstock into the plasma jet. Considering complex deposition dynamics of SPS technique, there is a need to better understand the relationships among spray conditions, ensuing particle behavior, deposition stress evolution and resultant properties. In this study, submicron yttria-stabilized zirconia particles suspended in ethanol were sprayed using a cascaded arc plasma torch. The stresses generated during the deposition of the layers (termed evolving stress) were monitored via the change in curvature of the substrate measured using an in situ measurement apparatus. Depending on the deposition conditions, coating microstructures ranged from feathery porous to dense/cracked deposits. The evolving stresses and modulus were correlated with the observed microstructures and visualized via process maps. Post-deposition bi-layer curvature measurement via low temperature thermal cycling was carried out to quantify the thermo-elastic response of different coatings. Lastly, preliminary data on furnace cycle durability of different coating microstructures were evaluated. This integrated study involving in situ diagnostics and ex situ characterization along with process maps provides a framework to describe coating formation mechanisms, process parametrics and microstructure description.

Materials Science Laboratory - Columnar-to-Equiaxed Transition in Solidification Processing and Microstructure Formation in Casting of Technical Alloys under Diffusive and Magnetically Controlled Convective Conditions

NASA Technical Reports Server (NTRS)

Gandin, Charles-Andre; Ratke, Lorenz

2008-01-01

The Materials Science Laboratory - Columnar-to-Equiaxed Transition in Solidification Processing and Microstructure Formation in Casting of Technical Alloys under Diffusive and Magnetically Controlled Convective Conditions (MSL-CETSOL and MICAST) are two investigations which supports research into metallurgical solidification, semiconductor crystal growth (Bridgman and zone melting), and measurement of thermo-physical properties of materials. This is a cooperative investigation with the European Space Agency (ESA) and National Aeronautics and Space Administration (NASA) for accommodation and operation aboard the International Space Station (ISS). Research Summary: Materials Science Laboratory - Columnar-to-Equiaxed Transition in Solidification Processing (CETSOL) and Microstructure Formation in Casting of Technical Alloys under Diffusive and Magnetically Controlled Convective Conditions (MICAST) are two complementary investigations which will examine different growth patterns and evolution of microstructures during crystallization of metallic alloys in microgravity. The aim of these experiments is to deepen the quantitative understanding of the physical principles that govern solidification processes in cast alloys by directional solidification.

Prediction of La0.6Sr0.4Co0.2Fe0.8O3 cathode microstructures during sintering: Kinetic Monte Carlo (KMC) simulations calibrated by artificial neural networks

NASA Astrophysics Data System (ADS)

Yan, Zilin; Kim, Yongtae; Hara, Shotaro; Shikazono, Naoki

2017-04-01

The Potts Kinetic Monte Carlo (KMC) model, proven to be a robust tool to study all stages of sintering process, is an ideal tool to analyze the microstructure evolution of electrodes in solid oxide fuel cells (SOFCs). Due to the nature of this model, the input parameters of KMC simulations such as simulation temperatures and attempt frequencies are difficult to identify. We propose a rigorous and efficient approach to facilitate the input parameter calibration process using artificial neural networks (ANNs). The trained ANN reduces drastically the number of trial-and-error of KMC simulations. The KMC simulation using the calibrated input parameters predicts the microstructures of a La0.6Sr0.4Co0.2Fe0.8O3 cathode material during sintering, showing both qualitative and quantitative congruence with real 3D microstructures obtained by focused ion beam scanning electron microscopy (FIB-SEM) reconstruction.

Role of isostaticity and load-bearing microstructure in the elasticity of yielded colloidal gels.

PubMed

Hsiao, Lilian C; Newman, Richmond S; Glotzer, Sharon C; Solomon, Michael J

2012-10-02

We report a simple correlation between microstructure and strain-dependent elasticity in colloidal gels by visualizing the evolution of cluster structure in high strain-rate flows. We control the initial gel microstructure by inducing different levels of isotropic depletion attraction between particles suspended in refractive index matched solvents. Contrary to previous ideas from mode coupling and micromechanical treatments, our studies show that bond breakage occurs mainly due to the erosion of rigid clusters that persist far beyond the yield strain. This rigidity contributes to gel elasticity even when the sample is fully fluidized; the origin of the elasticity is the slow Brownian relaxation of rigid, hydrodynamically interacting clusters. We find a power-law scaling of the elastic modulus with the stress-bearing volume fraction that is valid over a range of volume fractions and gelation conditions. These results provide a conceptual framework to quantitatively connect the flow-induced microstructure of soft materials to their nonlinear rheology.

Materials Characterization of Additively Manufactured Components for Rocket Propulsion

NASA Technical Reports Server (NTRS)

Carter, Robert; Draper, Susan; Locci, Ivan; Lerch, Bradley; Ellis, David; Senick, Paul; Meyer, Michael; Free, James; Cooper, Ken; Jones, Zachary

2015-01-01

To advance Additive Manufacturing (AM) technologies for production of rocket propulsion components the NASA Glenn Research Center (GRC) is applying state of the art characterization techniques to interrogate microstructure and mechanical properties of AM materials and components at various steps in their processing. The materials being investigated for upper stage rocket engines include titanium, copper, and nickel alloys. Additive manufacturing processes include laser powder bed, electron beam powder bed, and electron beam wire fed processes. Various post build thermal treatments, including Hot Isostatic Pressure (HIP), have been studied to understand their influence on microstructure, mechanical properties, and build density. Micro-computed tomography, electron microscopy, and mechanical testing in relevant temperature environments has been performed to develop relationships between build quality, microstructure, and mechanical performance at temperature. A summary of GRC's Additive Manufacturing roles and experimental findings will be presented.

Material Characterization of Additively Manufactured Components for Rocket Propulsion

NASA Technical Reports Server (NTRS)

Carter, Robert; Draper, Susan; Locci, Ivan; Lerch, Bradley; Ellis, David; Senick, Paul; Meyer, Michael; Free, James; Cooper, Ken; Jones, Zachary

2015-01-01

To advance Additive Manufacturing (AM) technologies for production of rocket propulsion components the NASA Glenn Research Center (GRC) is applying state of the art characterization techniques to interrogate microstructure and mechanical properties of AM materials and components at various steps in their processing. The materials being investigated for upper stage rocket engines include titanium, copper, and nickel alloys. Additive manufacturing processes include laser powder bed, electron beam powder bed, and electron beam wire fed processes. Various post build thermal treatments, including Hot Isostatic Pressure (HIP), have been studied to understand their influence on microstructure, mechanical properties, and build density. Micro-computed tomography, electron microscopy, and mechanical testing in relevant temperature environments has been performed to develop relationships between build quality, microstructure, and mechanical performance at temperature. A summary of GRCs Additive Manufacturing roles and experimental findings will be presented.

Investigations on the Mechanical Properties of Conducting Polymer Coating-Substrate Structures and Their Influencing Factors

PubMed Central

Wang, Xi-Shu; Tang, Hua-Ping; Li, Xu-Dong; Hua, Xin

2009-01-01

This review covers recent advances and work on the microstructure features, mechanical properties and cracking processes of conducting polymer film/coating- substrate structures under different testing conditions. An attempt is made to characterize and quantify the relationships between mechanical properties and microstructure features. In addition, the film cracking mechanism on the micro scale and some influencing factors that play a significant role in the service of the film-substrate structure are presented. These investigations cover the conducting polymer film/coating nucleation process, microstructure-fracture characterization, translation of brittle-ductile fractures, and cracking processes near the largest inherent macromolecule defects under thermal-mechanical loadings, and were carried out using in situ scanning electron microscopy (SEM) observations, as a novel method for evaluation of interface strength and critical failure stress. PMID:20054470

Design and validation of diffusion MRI models of white matter

NASA Astrophysics Data System (ADS)

Jelescu, Ileana O.; Budde, Matthew D.

2017-11-01

Diffusion MRI is arguably the method of choice for characterizing white matter microstructure in vivo. Over the typical duration of diffusion encoding, the displacement of water molecules is conveniently on a length scale similar to that of the underlying cellular structures. Moreover, water molecules in white matter are largely compartmentalized which enables biologically-inspired compartmental diffusion models to characterize and quantify the true biological microstructure. A plethora of white matter models have been proposed. However, overparameterization and mathematical fitting complications encourage the introduction of simplifying assumptions that vary between different approaches. These choices impact the quantitative estimation of model parameters with potential detriments to their biological accuracy and promised specificity. First, we review biophysical white matter models in use and recapitulate their underlying assumptions and realms of applicability. Second, we present up-to-date efforts to validate parameters estimated from biophysical models. Simulations and dedicated phantoms are useful in assessing the performance of models when the ground truth is known. However, the biggest challenge remains the validation of the “biological accuracy” of estimated parameters. Complementary techniques such as microscopy of fixed tissue specimens have facilitated direct comparisons of estimates of white matter fiber orientation and densities. However, validation of compartmental diffusivities remains challenging, and complementary MRI-based techniques such as alternative diffusion encodings, compartment-specific contrast agents and metabolites have been used to validate diffusion models. Finally, white matter injury and disease pose additional challenges to modeling, which are also discussed. This review aims to provide an overview of the current state of models and their validation and to stimulate further research in the field to solve the remaining open questions and converge towards consensus.

Design and validation of diffusion MRI models of white matter

PubMed Central

Jelescu, Ileana O.; Budde, Matthew D.

2018-01-01

Diffusion MRI is arguably the method of choice for characterizing white matter microstructure in vivo. Over the typical duration of diffusion encoding, the displacement of water molecules is conveniently on a length scale similar to that of the underlying cellular structures. Moreover, water molecules in white matter are largely compartmentalized which enables biologically-inspired compartmental diffusion models to characterize and quantify the true biological microstructure. A plethora of white matter models have been proposed. However, overparameterization and mathematical fitting complications encourage the introduction of simplifying assumptions that vary between different approaches. These choices impact the quantitative estimation of model parameters with potential detriments to their biological accuracy and promised specificity. First, we review biophysical white matter models in use and recapitulate their underlying assumptions and realms of applicability. Second, we present up-to-date efforts to validate parameters estimated from biophysical models. Simulations and dedicated phantoms are useful in assessing the performance of models when the ground truth is known. However, the biggest challenge remains the validation of the “biological accuracy” of estimated parameters. Complementary techniques such as microscopy of fixed tissue specimens have facilitated direct comparisons of estimates of white matter fiber orientation and densities. However, validation of compartmental diffusivities remains challenging, and complementary MRI-based techniques such as alternative diffusion encodings, compartment-specific contrast agents and metabolites have been used to validate diffusion models. Finally, white matter injury and disease pose additional challenges to modeling, which are also discussed. This review aims to provide an overview of the current state of models and their validation and to stimulate further research in the field to solve the remaining open questions and converge towards consensus. PMID:29755979

Mechanical Characterization and Material Modeling of Diabetic Aortas in a Rabbit Model.

PubMed

Tong, Jianhua; Yang, F; Li, X; Xu, X; Wang, G X

2018-03-01

Diabetes has been recognized as a major risk factor to cause macrovascular diseases and plays a key role in aortic wall remodeling. However, the effects of diabetes on elastic properties of aortas remain largely unknown and quantitative mechanical data are lacking. Thirty adult rabbits (1.6-2.2 kg) were collected and the type 1 diabetic rabbit model was induced by injection of alloxan. A total of 15 control and 15 diabetic rabbit (abdominal) aortas were harvested. Uniaxial and biaxial tensile tests were performed to measure ultimate tensile strength and to characterize biaxial mechanical behaviors of the aortas. A material model was fitted to the biaxial experimental data to obtain constitutive parameters. Histological and mass fraction analyses were performed to investigate the underlying microstructure and dry weight percentages of elastin and collagen in the control and the diabetic aortas. No statistically significant difference was found in ultimate tensile strength between the control and the diabetic aortas. Regarding biaxial mechanical responses, the diabetic aortas exhibited significantly lower extensibility and significantly higher tissue stiffness than the control aortas. Notably, tissue stiffening occurred in both circumferential and axial directions for the diabetic aortas; however, mechanical anisotropy does not change significantly. The material model was able to fit biaxial experimental data very well. Histology showed that a number of isolated foam cells were embedded in the diabetic aortas and hyperplasia of collagen was identified. The dry weight percentages of collagen within the diabetic aortas increased significantly as compared to the control aortas, whereas no significant change was found for that of elastin. Our data suggest that the diabetes impairs elastic properties and alters microstructure of the aortas and consequently, these changes may further contribute to complex aortic wall remodeling.

3D Printing and Digital Rock Physics for Geomaterials

NASA Astrophysics Data System (ADS)

Martinez, M. J.; Yoon, H.; Dewers, T. A.

2015-12-01

Imaging techniques for the analysis of porous structures have revolutionized our ability to quantitatively characterize geomaterials. Digital representations of rock from CT images and physics modeling based on these pore structures provide the opportunity to further advance our quantitative understanding of fluid flow, geomechanics, and geochemistry, and the emergence of coupled behaviors. Additive manufacturing, commonly known as 3D printing, has revolutionized production of custom parts with complex internal geometries. For the geosciences, recent advances in 3D printing technology may be co-opted to print reproducible porous structures derived from CT-imaging of actual rocks for experimental testing. The use of 3D printed microstructure allows us to surmount typical problems associated with sample-to-sample heterogeneity that plague rock physics testing and to test material response independent from pore-structure variability. Together, imaging, digital rocks and 3D printing potentially enables a new workflow for understanding coupled geophysical processes in a real, but well-defined setting circumventing typical issues associated with reproducibility, enabling full characterization and thus connection of physical phenomena to structure. In this talk we will discuss the possibilities that these technologies can bring to geosciences and present early experiences with coupled multiscale experimental and numerical analysis using 3D printed fractured rock specimens. In particular, we discuss the processes of selection and printing of transparent fractured specimens based on 3D reconstruction of micro-fractured rock to study fluid flow characterization and manipulation. Micro-particle image velocimetry is used to directly visualize 3D single and multiphase flow velocity in 3D fracture networks. Sandia National Laboratories is a multi-program laboratory managed and operated by Sandia Corporation, a wholly owned subsidiary of Lockheed Martin Corporation, for the U.S. Department of Energy's National Nuclear Security Administration under contract DE-AC04-94AL85000.

Characterization of Plastic flow and Resulting Micro-Textures in a Friction Stir Weld

NASA Technical Reports Server (NTRS)

Schneider, J. A.; Nunes, A. C., Jr.

2003-01-01

The mechanically affected zone of a friction stir weld (FSW) cross section exhibits two distinct microstructural regions, possibly the residues of two distinct currents of metal in the FSW flow process. In this study the respective textures of these microstructural regions are investigated using orientation image mapping (OIM).

Characterization and modeling of mechanical behavior of single crystal titanium deformed by split-Hopkinson pressure bar

DOE PAGES

Morrow, B. M.; Lebensohn, R. A.; Trujillo, C. P.; ...

2016-03-28

Single crystal titanium samples were dynamically loaded using split-Hopkinson pressure bar (SHPB) and the resulting microstructures were examined. Characterization of the twins and dislocations present in the microstructure was conducted to understand the pathway for observed mechanical behavior. Electron backscatter diffraction (EBSD) was used to measure textures and quantify twinning. Microstructures were profusely twinned after loading, and twin variants and corresponding textures were different as a function of initial orientation. Focused ion beam (FIB) foils were created to analyze dislocation content using transmission electron microscopy (TEM). Large amounts of dislocations were present, indicating that plasticity was achieved through slip andmore » twinning together. Viscoplastic self-consistent (VPSC) modeling was used to confirm the complex order of operations during deformation. The activation of different mechanisms was highly dependent upon crystal orientation. For [0001] and View the MathML source[101¯1]-oriented crystals, compressive twinning was observed, followed by secondary tensile twinning. Furthermore, dislocations though prevalent in the microstructure, contributed to final texture far less than twinning.« less

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

Nanostructure formation during accumulative roll bonding of commercial purity titanium

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

Karimi, Mohsen, E-mail: m.karimi@shahroodut.ac.ir

2016-12-15

In this investigation, commercial purity titanium (CP–Ti) was subjected to accumulative roll bonding (ARB) process up to 8 cycles (equivalent strain of 6.4) at the ambient temperature. Transmission electron microscopy (TEM) and X–ray diffraction line profile analysis (XRDLPA) were utilized to investigate the microstructure and grain size evolution. Both characterization techniques could clarify the non–uniform microstructure in the early stages and the uniform microstructure in the final stages of the process. The effectiveness of ARB for the fabrication of the nano–grained structure in CP–Ti was revealed. It was found that the SFE is not the only factor affecting grain refinement,more » as compared with other studies on ARB of FCC materials. Influence of other factors such as the melting temperature and the crystalline structure of the material was determined on the grain refinement. - Highlights: •Nano–grained commercial purity titanium was produced by accumulative roll bonding. •TEM and XRDLPA were used for the characterization of the microstructure. •Important factors affecting the grain size of ARBed materials were discussed.« less

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

Metallographic Characterization of Wrought Depleted Uranium

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

Forsyth, Robert Thomas; Hill, Mary Ann

Metallographic characterization was performed on wrought depleted uranium (DU) samples taken from the longitudinal and transverse orientations from specific locations on two specimens. Characterization of the samples included general microstructure, inclusion analysis, grain size analysis, and microhardness testing. Comparisons of the characterization results were made to determine any differences based on specimen, sample orientation, or sample location. In addition, the characterization results for the wrought DU samples were also compared with data obtained from the metallographic characterization of cast DU samples previously characterized. No differences were observed in microstructure, inclusion size, morphology, and distribution, or grain size in regard tomore » specimen, location, or orientation for the wrought depleted uranium samples. However, a small difference was observed in average hardness with regard to orientation at the same locations within the same specimen. The longitudinal samples were slightly harder than the transverse samples from the same location of the same specimen. This was true for both wrought DU specimens. Comparing the wrought DU sample data with the previously characterized cast DU sample data, distinct differences in microstructure, inclusion size, morphology and distribution, grain size, and microhardness were observed. As expected, the microstructure of the wrought DU samples consisted of small recrystallized grains which were uniform, randomly oriented, and equiaxed with minimal twinning observed in only a few grains. In contrast, the cast DU microstructure consisted of large irregularly shaped grains with extensive twinning observed in most grains. Inclusions in the wrought DU samples were elongated, broken and cracked and light and dark phases were observed in some inclusions. The mean inclusion area percentage for the wrought DU samples ranged from 0.08% to 0.34% and the average density from all wrought DU samples was 1.62E+04/cm 2. Inclusions in the cast DU samples were equiaxed and intact with light and dark phases observed in some inclusions. The mean inclusion area percentage for the cast DU samples ranged from 0.93% to 1.00% and the average density from all wrought DU samples was 2.83E+04/cm 2. The average mean grain area from all wrought DU samples was 141 μm 2 while the average mean grain area from all cast DU samples was 1.7 mm2. The average Knoop microhardness from all wrought DU samples was 215 HK and the average Knoop microhardness from all cast DU samples was 264 HK.« less

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

Chen, Junfeng, E-mail: chenjunfeng@fzu.edu.cn; Zou, Linchi, E-mail: zoulinchi1201@163.com; Li, Qiang

The microstructure evolution of the 7050 Al alloy treated by age-forming was studied using a designed device which can simulate the age-forming process. The grain shape, grain boundary misorientation and grain orientation evolution of 7050 Al alloy during age-forming have been quantitatively characterized by electron backscattering diffraction technique. The results show that age-forming produced abundant low-angle boundaries and elongated grains, which attributed to stress induced dislocation movement and grain boundary migration during the age-forming process. On the other side, the stress along rolling direction caused some unstable orientation grains to rotate towards the Brass and S orientations during the age-formingmore » process. Hence, the intensity of the rolling texture orientation in age-formed samples is enhanced. But this effect decays gradually with increasing aging time, since stress decreases and precipitation hardening occurs during the age-forming process. - Highlights: • Quantitative analysis of grain evolution of 7050 Al alloys during age-forming • Stress induces some grain rotation of 7050 Al alloys during age-forming. • Creep leads to elongate grain of 7050 Al alloys during age-forming. • Obtains a trend on texture evolution during age-forming applied stress.« less

Calculation of grain boundary normals directly from 3D microstructure images

DOE PAGES

Lieberman, E. J.; Rollett, A. D.; Lebensohn, R. A.; ...

2015-03-11

The determination of grain boundary normals is an integral part of the characterization of grain boundaries in polycrystalline materials. These normal vectors are difficult to quantify due to the discretized nature of available microstructure characterization techniques. The most common method to determine grain boundary normals is by generating a surface mesh from an image of the microstructure, but this process can be slow, and is subject to smoothing issues. A new technique is proposed, utilizing first order Cartesian moments of binary indicator functions, to determine grain boundary normals directly from a voxelized microstructure image. In order to validate the accuracymore » of this technique, the surface normals obtained by the proposed method are compared to those generated by a surface meshing algorithm. Specifically, the local divergence between the surface normals obtained by different variants of the proposed technique and those generated from a surface mesh of a synthetic microstructure constructed using a marching cubes algorithm followed by Laplacian smoothing is quantified. Next, surface normals obtained with the proposed method from a measured 3D microstructure image of a Ni polycrystal are used to generate grain boundary character distributions (GBCD) for Σ3 and Σ9 boundaries, and compared to the GBCD generated using a surface mesh obtained from the same image. Finally, the results show that the proposed technique is an efficient and accurate method to determine voxelized fields of grain boundary normals.« less

Damage Mechanisms and Mechanical Properties of High-Strength Multiphase Steels.

PubMed

Heibel, Sebastian; Dettinger, Thomas; Nester, Winfried; Clausmeyer, Till; Tekkaya, A Erman

2018-05-09

The usage of high-strength steels for structural components and reinforcement parts is inevitable for modern car-body manufacture in reaching lightweight design as well as increasing passive safety. Depending on their microstructure these steels show differing damage mechanisms and various mechanical properties which cannot be classified comprehensively via classical uniaxial tensile testing. In this research, damage initiation, evolution and final material failure are characterized for commercially produced complex-phase (CP) and dual-phase (DP) steels in a strength range between 600 and 1000 MPa. Based on these investigations CP steels with their homogeneous microstructure are characterized as damage tolerant and hence less edge-crack sensitive than DP steels. As final fracture occurs after a combination of ductile damage evolution and local shear band localization in ferrite grains at a characteristic thickness strain, this strain measure is introduced as a new parameter for local formability. In terms of global formability DP steels display advantages because of their microstructural composition of soft ferrite matrix including hard martensite particles. Combining true uniform elongation as a measure for global formability with the true thickness strain at fracture for local formability the mechanical material response can be assessed on basis of uniaxial tensile testing incorporating all microstructural characteristics on a macroscopic scale. Based on these findings a new classification scheme for the recently developed high-strength multiphase steels with significantly better formability resulting of complex underlying microstructures is introduced. The scheme overcomes the steel designations using microstructural concepts, which provide no information about design and production properties.

Damage Evolution in Complex-Phase and Dual-Phase Steels during Edge Stretching.

PubMed

Pathak, Nikky; Butcher, Cliff; Worswick, Michael James; Bellhouse, Erika; Gao, Jeff

2017-03-27

The role of microstructural damage in controlling the edge stretchability of Complex-Phase (CP) and Dual-Phase (DP) steels was evaluated using hole tension experiments. The experiments considered a tensile specimen with a hole at the center of specimen that is either sheared (sheared edge condition) or drilled and then reamed (reamed edge condition). The damage mechanism and accumulation in the CP and DP steels were systematically characterized by interrupting the hole tension tests at different strain levels using scanning electron microscope (SEM) analysis and optical microscopy. Martensite cracking and decohesion of ferrite-martensite interfaces are the dominant nucleation mechanisms in the DP780. The primary source of void nucleation in the CP800 is nucleation at TiN particles, with secondary void formation at martensite/bainite interfaces near the failure strain. The rate of damage evolution is considerably higher for the sheared edge in contrast with the reamed edge since the shearing process alters the microstructure in the shear affected zone (SAZ) by introducing work-hardening and initial damage behind the sheared edge. The CP microstructures were shown to be less prone to shear-induced damage than the DP materials resulting in much higher sheared edge formability. Microstructural damage in the CP and DP steels was characterized to understand the interaction between microstructure, damage evolution and edge formability during edge stretching. An analytical model for void evolution and coalescence was developed and applied to predict the damage rate in these rather diverse microstructures.

Microstructured bicontinuous phase formulations: their characterization and application in dermal and transdermal drug delivery.

PubMed

Lapteva, Maria; Kalia, Yogeshvar N

2013-08-01

The development of approaches to increase drug solubility and partitioning into the skin is an active area of research in topical and transdermal delivery. In addition to forming spherical aggregates, e.g., conventional oil in water or water in oil microemulsions, the combination of an oil, surfactant and water can create bicontinuous structures where the self-assembly properties of surfactants mean that the boundaries between oil and water are no longer random. This leads to the formation of specific microstructures whose intrinsic properties and interactions with the drug will determine the ability to formulate a given drug, its stability once formulated and its subsequent delivery. The review explores the relationship between the microstructure of biphasic formulations, present in microemulsions and liquid crystalline phases, and drug delivery into the skin. An overview of possible internal microstructures is followed by a summary of the methods used for structure characterization. The final section presents the work to-date and discusses the efficacy of such vehicles in enhancing dermal and transdermal delivery. The combination of water, surface agent and oil generates a broad range of three dimensional structures differing in both chemical and physical proprieties. Knowledge of the microstructure is important in understanding the behavior of a formulation and its effect on drug delivery into the skin. Microstructure complexity, interactions between the drug and the vehicle (i.e., location and mobility) and those between the vehicle and the skin are key determinants of drug delivery.

Damage Evolution in Complex-Phase and Dual-Phase Steels during Edge Stretching

PubMed Central

Pathak, Nikky; Butcher, Cliff; Worswick, Michael James; Bellhouse, Erika; Gao, Jeff

2017-01-01

The role of microstructural damage in controlling the edge stretchability of Complex-Phase (CP) and Dual-Phase (DP) steels was evaluated using hole tension experiments. The experiments considered a tensile specimen with a hole at the center of specimen that is either sheared (sheared edge condition) or drilled and then reamed (reamed edge condition). The damage mechanism and accumulation in the CP and DP steels were systematically characterized by interrupting the hole tension tests at different strain levels using scanning electron microscope (SEM) analysis and optical microscopy. Martensite cracking and decohesion of ferrite-martensite interfaces are the dominant nucleation mechanisms in the DP780. The primary source of void nucleation in the CP800 is nucleation at TiN particles, with secondary void formation at martensite/bainite interfaces near the failure strain. The rate of damage evolution is considerably higher for the sheared edge in contrast with the reamed edge since the shearing process alters the microstructure in the shear affected zone (SAZ) by introducing work-hardening and initial damage behind the sheared edge. The CP microstructures were shown to be less prone to shear-induced damage than the DP materials resulting in much higher sheared edge formability. Microstructural damage in the CP and DP steels was characterized to understand the interaction between microstructure, damage evolution and edge formability during edge stretching. An analytical model for void evolution and coalescence was developed and applied to predict the damage rate in these rather diverse microstructures. PMID:28772707

Microstructure selection in thin-sample directional solidification of an Al-Cu alloy: In situ X-ray imaging and phase-field simulations

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

Clarke, A. J.; Tourret, D.; Song, Y.

We study microstructure selection during during directional solidification of a thin metallic sample. We combine in situ X-ray radiography of a dilute Al-Cu alloy solidification experiments with three-dimensional phase-field simulations. Here we explore a range of temperature gradient G and growth velocity V and build a microstructure selection map for this alloy. We investigate the selection of the primary dendritic spacing Λ and tip radius ρ. While ρ shows a good agreement between experimental measurements and dendrite growth theory, with ρ~V $-$1/2, Λ is observed to increase with V (∂Λ/∂V > 0), in apparent disagreement with classical scaling laws formore » primary dendritic spacing, which predict that ∂Λ/∂V<0. We show through simulations that this trend inversion for Λ(V) is due to liquid convection in our experiments, despite the thin sample configuration. We use a classical diffusion boundary-layer approximation to semi-quantitatively incorporate the effect of liquid convection into phase-field simulations. This approximation is implemented by assuming complete solute mixing outside a purely diffusive zone of constant thickness that surrounds the solid-liquid interface. This simple method enables us to quantitatively match experimental measurements of the planar morphological instability threshold and primary spacings over an order of magnitude in V. Lastly, we explain the observed inversion of ∂Λ/∂V by a combination of slow transient dynamics of microstructural homogenization and the influence of the sample thickness.« less

Microstructure selection in thin-sample directional solidification of an Al-Cu alloy: In situ X-ray imaging and phase-field simulations

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

Clarke, A. J.; Tourret, D.; Song, Y.

We study microstructure selection during directional solidification of a thin metallic sample. We combine in situ X-ray radiography of a dilute Al-Cu alloy solidification experiments with three-dimensional phase-field simulations. We explore a range of temperature gradient G and growth velocity V and build a microstructure selection map for this alloy. We investigate the selection of the primary dendritic spacing Lambda and tip radius rho. While rho shows a good agreement between experimental measurements and dendrite growth theory, with rho similar to V-1/2, Lambda is observed to increase with V (partial derivative Lambda/partial derivative V > 0), in apparent disagreement withmore » classical scaling laws for primary dendritic spacing, which predict that partial derivative Lambda/partial derivative V <0. We show through simulations that this trend inversion for Lambda(V) is due to liquid convection in our experiments, despite the thin sample configuration. We use a classical diffusion boundary-layer approximation to semi-quantitatively incorporate the effect of liquid convection into phase-field simulations. This approximation is implemented by assuming complete solute mixing outside a purely diffusive zone of constant thickness that surrounds the solid-liquid interface. This simple method enables us to quantitatively match experimental measurements of the planar morphological instability threshold and primary spacings over an order of magnitude in V. We explain the observed inversion of partial derivative Lambda/partial derivative V by a combination of slow transient dynamics of microstructural homogenization and the influence of the sample thickness.« less

Microstructure selection in thin-sample directional solidification of an Al-Cu alloy: In situ X-ray imaging and phase-field simulations

DOE PAGES

Clarke, A. J.; Tourret, D.; Song, Y.; ...

2017-05-01

We study microstructure selection during during directional solidification of a thin metallic sample. We combine in situ X-ray radiography of a dilute Al-Cu alloy solidification experiments with three-dimensional phase-field simulations. Here we explore a range of temperature gradient G and growth velocity V and build a microstructure selection map for this alloy. We investigate the selection of the primary dendritic spacing Λ and tip radius ρ. While ρ shows a good agreement between experimental measurements and dendrite growth theory, with ρ~V $-$1/2, Λ is observed to increase with V (∂Λ/∂V > 0), in apparent disagreement with classical scaling laws formore » primary dendritic spacing, which predict that ∂Λ/∂V<0. We show through simulations that this trend inversion for Λ(V) is due to liquid convection in our experiments, despite the thin sample configuration. We use a classical diffusion boundary-layer approximation to semi-quantitatively incorporate the effect of liquid convection into phase-field simulations. This approximation is implemented by assuming complete solute mixing outside a purely diffusive zone of constant thickness that surrounds the solid-liquid interface. This simple method enables us to quantitatively match experimental measurements of the planar morphological instability threshold and primary spacings over an order of magnitude in V. Lastly, we explain the observed inversion of ∂Λ/∂V by a combination of slow transient dynamics of microstructural homogenization and the influence of the sample thickness.« less

Quantitative XRD analysis of {110} twin density in biotic aragonites.

PubMed

Suzuki, Michio; Kim, Hyejin; Mukai, Hiroki; Nagasawa, Hiromichi; Kogure, Toshihiro

2012-12-01

{110} Twin densities in biotic aragonite have been estimated quantitatively from the peak widths of specific reflections in powder X-ray diffraction (XRD) patterns, as well as direct confirmation of the twins using transmission electron microscopy (TEM). Influence of the twin density on the peak widths in the XRD pattern was simulated using DIFFaX program, regarding (110) twin as interstratification of two types of aragonite unit layers with mirrored relationship. The simulation suggested that the twin density can be estimated from the difference of the peak widths between 111 and 021, or between 221 and 211 reflections. Biotic aragonite in the crossed-lamellar microstructure (three species) and nacreous microstructure (four species) of molluscan shells, fish otoliths (two species), and a coral were investigated. The XRD analyses indicated that aragonite crystals in the crossed-lamellar microstructure of the three species contain high density of the twins, which is consistent with the TEM examination. On the other hand, aragonite in the nacre of the four species showed almost no difference of the peak widths between the paired reflections, indicating low twin densities. The results for the fish otoliths were varied between the species. Such variation of the twin density in biotic aragonites may reflect different schemes of crystal growth in biomineralization. Copyright © 2012 Elsevier Inc. All rights reserved.

Fast Realistic MRI Simulations Based on Generalized Multi-Pool Exchange Tissue Model.

PubMed

Liu, Fang; Velikina, Julia V; Block, Walter F; Kijowski, Richard; Samsonov, Alexey A

2017-02-01

We present MRiLab, a new comprehensive simulator for large-scale realistic MRI simulations on a regular PC equipped with a modern graphical processing unit (GPU). MRiLab combines realistic tissue modeling with numerical virtualization of an MRI system and scanning experiment to enable assessment of a broad range of MRI approaches including advanced quantitative MRI methods inferring microstructure on a sub-voxel level. A flexible representation of tissue microstructure is achieved in MRiLab by employing the generalized tissue model with multiple exchanging water and macromolecular proton pools rather than a system of independent proton isochromats typically used in previous simulators. The computational power needed for simulation of the biologically relevant tissue models in large 3D objects is gained using parallelized execution on GPU. Three simulated and one actual MRI experiments were performed to demonstrate the ability of the new simulator to accommodate a wide variety of voxel composition scenarios and demonstrate detrimental effects of simplified treatment of tissue micro-organization adapted in previous simulators. GPU execution allowed  ∼ 200× improvement in computational speed over standard CPU. As a cross-platform, open-source, extensible environment for customizing virtual MRI experiments, MRiLab streamlines the development of new MRI methods, especially those aiming to infer quantitatively tissue composition and microstructure.

Fast Realistic MRI Simulations Based on Generalized Multi-Pool Exchange Tissue Model

PubMed Central

Velikina, Julia V.; Block, Walter F.; Kijowski, Richard; Samsonov, Alexey A.

2017-01-01

We present MRiLab, a new comprehensive simulator for large-scale realistic MRI simulations on a regular PC equipped with a modern graphical processing unit (GPU). MRiLab combines realistic tissue modeling with numerical virtualization of an MRI system and scanning experiment to enable assessment of a broad range of MRI approaches including advanced quantitative MRI methods inferring microstructure on a sub-voxel level. A flexibl representation of tissue microstructure is achieved in MRiLab by employing the generalized tissue model with multiple exchanging water and macromolecular proton pools rather than a system of independent proton isochromats typically used in previous simulators. The computational power needed for simulation of the biologically relevant tissue models in large 3D objects is gained using parallelized execution on GPU. Three simulated and one actual MRI experiments were performed to demonstrate the ability of the new simulator to accommodate a wide variety of voxel composition scenarios and demonstrate detrimental effects of simplifie treatment of tissue micro-organization adapted in previous simulators. GPU execution allowed ∼200× improvement in computational speed over standard CPU. As a cross-platform, open-source, extensible environment for customizing virtual MRI experiments, MRiLab streamlines the development of new MRI methods, especially those aiming to infer quantitatively tissue composition and microstructure. PMID:28113746

Effects of Thermomechanical History on the Tensile Behavior of Nitinol Ribbon

NASA Technical Reports Server (NTRS)

Lach, Cynthia L.; Turner, Travis L.; Taminger, Karen M.; Shenoy, Ravi N.

2002-01-01

Shape memory alloys (SMAs) have enormous potential for a wide variety of applications. A large body of work exists on the characterization of the microstructure and stress-strain behavior of these alloys, Nitinol (NiTi) in particular. However, many attributes of these materials are yet to be fully understood. Previous work at NASA Langley Research Center (LaRC) has included fabrication of hybrid composite specimens with embedded Nitinol actuators and modeling of their thermomechanical behavior. An intensive characterization effort has been undertaken to facilitate fundamental understanding of this alloy and to promote implementation of Nitinol in aerospace applications. Previous work revealed attributes of the Nitinol ribbon that were not easily rationalized with existing data in the literature. In particular, tensile behavior at ambient temperature showed significant dependence on the thermomechanical history prior to testing. The present work is focused on characterizing differences in the microstructure of Nitinol ribbons exposed to four different thermomechanical histories and correlation of the microstructure with tensile properties. Differential scanning calorimetry (DSC) and x-ray diffraction (XRD) analysis were employed to rationalize the microstructures present after exposure to various thermomechanical histories. Three of the Nitinol ribbon conditions were reversible upon heating (in the DSC) through the reverse transformation temperature (A(sub f) to transform the microstructure to austenite. However, the prior thermomechanical conditioning for the Nitinol ribbon that reflected the entire fabrication procedure (4% thermal cycle condition) was found to have an irreversible effect on the microstructure, as it remained unchanged after repeated complete thermal cycles. Tensile tests were conducted to determine the effect of prior thermomechancal conditioning on both the tensile behavior of the Nitinol ribbons and the stress state of the microstructure. The stress-strain behavior of the Nitinol actuators appears to be governed by the interplay between two major variables: namely, microstructural constituents such as the R-phase and the martensite; and the stress state of these constituents (whether twinned with low residual stresses, or detwinned with high residual stresses). The most significant difference in the stress-strain behavior of the four conditions, the critical stress required to achieve an initial stress plateau, was found to depend on both the amount and stress state (twinned or detwinned) of R-phase present in the initial microstructure. Thus, the effect of prior thermomechanical processing is critical to the resulting tensile behavior of the Nitinol actuator. For numerical modeling inputs one must take into account the entire fabrication process on the Nitinol actuator.

Portable vibro-acoustic testing system for in situ microstructure characterization and metrology

NASA Astrophysics Data System (ADS)

Smith, James A.; Nichol, Corrie I.; Zuck, Larry D.; Fatemi, Mostafa

2018-04-01

There is a need in research reactors like the one at INL to inspect irradiated materials and structures. The goal of this work is to develop a portable scanning infrastructure for a material characterization technique called vibro-acoustography (VA) that has been developed by the Idaho National laboratory for nuclear applications to characterize fuel, cladding materials, and structures. The proposed VA technology is based on ultrasound and acoustic waves; however, it provides information beyond what is available from the traditional ultrasound techniques and can expand the knowledge on nuclear material characterization and microstructure evolution. This paper will report on the development of a portable scanning system that will be set up to characterize materials and components in open water reactors and canals in situ. We will show some initial laboratory results of images generated by vibro-acoustics of surrogate fuel plates and graphite structures and discuss the design of the portable system.

Microstructures and properties of rapidly solidified alloys

NASA Technical Reports Server (NTRS)

Shechtman, D.; Horowitz, E.

1984-01-01

The microstructure and properties of rapidly solidified aluminum alloys were researched. The effects of powder and flake chemistry and morphology and alternative consolidation processing parameters are being conducted. Samples of the powders being utilized were obtained for comprehensive metallurgical characterization. Seven aluminum alloys in the form of thin foils were studied by a variety of techniques including optical metallography, scanning electron microscope, and transmission electron microscope. Details of the microstructural characteristics are presented along with a discussion of the solidification process. A better understanding of the microstructure of the rapidly solidified aluminum alloys prepared by a variety of techniques such as roller quenching, the vacuum atomized procedure, ultrasonically atomized in inert atmospheres, and atomized in flue gas was provided.

Artificial Microstructures to Investigate Microstructure-Property Relationships in Metallic Glasses

NASA Astrophysics Data System (ADS)

Sarac, Baran

Technology has evolved rapidly within the last decade, and the demand for higher performance materials has risen exponentially. To meet this demand, novel materials with advanced microstructures have been developed and are currently in use. However, the already complex microstructure of technological relevant materials imposes a limit for currently used development strategies for materials with optimized properties. For this reason, a strategy to correlate microstructure features with properties is still lacking. Computer simulations are challenged due to the computing size required to analyze multi-scale characteristics of complex materials, which is orders of magnitude higher than today's state of the art. To address these challenges, we introduced a novel strategy to investigate microstructure-property relationships. We call this strategy "artificial microstructure approach", which allows us to individually and independently control microstructural features. By this approach, we defined a new way of analyzing complex microstructures, where microstructural second phase features were precisely varied over a wide range. The artificial microstructures were fabricated by the combination of lithography and thermoplastic forming (TPF), and subsequently characterized under different loading conditions. Because of the suitability and interesting properties of metallic glasses, we proposed to use this toolbox to investigate the different deformation modes in cellular structures and toughening mechanism in metallic glass (MG) composites. This study helped us understand how to combine the unique properties of metallic glasses such as high strength, elasticity, and thermoplastic processing ability with plasticity generated from heterostructures of metallic glasses. It has been widely accepted that metallic glass composites are very complex, and a broad range of contributions have been suggested to explain the toughening mechanism. This includes the shear modulus, morphology, size, spacing, volume fraction of the second phase, and strength and toughness of the interface. Previous studies suggest these contributions, however, do not provide quantitative experimental evidence. Within this thesis, we paid tribute to the complexity of the toughening mechanism by revealing the correlation between plastic zone size (Rp) and second phase spacing (s ), and the results guided us how to design elasticity through the second phase morphology (AB pore stacking) in MG heterostructures. The second phase elasticity and shear modulus were also found to be contributing to the overall elasticity. We identified the pores' ratio of diameter to spacing (d/s) as one of the major factors controlling the mechanical properties of MG hetero structures, which is most efficient when d/s ≈ 1. Effectiveness of MG heterostructures also depends on the size of the sample, w, in comparison to s. Our experimental findings illuminate the complexity in MG composites, which can be resolved with our artificial microstructure approach. Another subject where we use artificial microstructures is to identify the effect of length scales on structural properties of MG heterostructures. MG structures can be fabricated over 7 orders of magnitude length scale (nm to cm), where the effect of the feature size determines whether the deformation will be homogenous throughout the sample, it will be localized into shear bands, or it will not show any shear bands (no plasticity) during bending and tension. We investigated the deformation modes of Zr-based MGs in hexagonal cellular structures controlled by the relative density, and revealed three distinctive deformation regions: collective buckling, local failure, and global failure which originate from size effects in metallic glasses. The relative density of ˜25.0% was determined as the ideal relative density for energy absorption, strength and plasticity in MG cellular structures. Besides two specific examples studied in detail here, the artificial microstructure concept can be applied to a wide range of problems in microstructures and micro structural architectures of porous and natural materials. Furthermore, it can be used to determine the flaw tolerance, and to investigate the sensitivity of microstructures to imperfections. For example, a mechanistic understanding of shear localization would help address the major shortcoming of metallic glasses and enable predictive models to be developed which would permit one to intelligently design microstructures to exhibit desirable properties.

Ultrasonic characterization of microstructure in powder metal alloy

NASA Technical Reports Server (NTRS)

Tittmann, B. R.; Ahlberg, L. A.; Fertig, K.

1986-01-01

The ultrasonic wave propagation characteristics were measured for IN-100, a powder metallurgy alloy used for aircraft engine components. This material was as a model system for testing the feasibility of characterizing the microstructure of a variety of inhomogeneous media including powder metals, ceramics, castings and components. The data were obtained for a frequency range from about 2 to 20 MHz and were statistically averaged over numerous volume elements of the samples. Micrographical examination provided size and number distributions for grain and pore structure. The results showed that the predominant source for the ultrasonic attenuation and backscatter was a dense (approx. 100/cubic mm) distribution of small micropores (approx. 10 micron radius). Two samples with different micropore densities were studied in detail to test the feasibility of calculating from observed microstructural parameters the frequency dependence of the microstructural backscatter in the regime for which the wavelength is much larger than the size of the individual scattering centers. Excellent agreement was found between predicted and observed values so as to demonstrate the feasibility of solving the forward problem. The results suggest a way towards the nondestructive detection and characterization of anomalous distributions of micropores when conventional ultrasonic imaging is difficult. The findings are potentially significant toward the application of the early detection of porosity during the materials fabrication process and after manufacturing of potential sites for stress induced void coalescence leading to crack initiation and subsequent failure.

Effects of irradiation on the microstructure of U-7Mo dispersion fuel with Al-2Si matrix

NASA Astrophysics Data System (ADS)

Keiser, Dennis D.; Jue, Jan-Fong; Robinson, Adam B.; Medvedev, Pavel; Gan, Jian; Miller, Brandon D.; Wachs, Daniel M.; Moore, Glenn A.; Clark, Curtis R.; Meyer, Mitchell K.; Ross Finlay, M.

2012-06-01

The Reduced Enrichment for Research and Test Reactor (RERTR) program is developing low-enriched uranium U-Mo dispersion fuels for application in research and test reactors around the world. As part of this development, fuel plates have been irradiated in the Advanced Test Reactor and then characterized using optical metallography (OM) and scanning electron microscopy (SEM) to determine the as-irradiated microstructure. To demonstrate the irradiation performance of U-7Mo dispersion fuel plates with 2 wt.% Si added to the matrix, fuel plates were tested to moderate burnups at intermediate fission rates as part of the RERTR-6 experiment. Further testing was performed to higher fission rates as part of the RERTR-7A experiment, and very aggressive testing (high temperature, high fission density, and high fission rate) was performed in the RERTR-9A, RERTR-9B, and AFIP-1 experiments. As-irradiated microstructures were compared to those observed after fabrication to determine the effects of irradiation on the microstructure. Based on comparison of the microstructural characterization results for each irradiated sample, some general conclusions can be drawn about how the microstructure evolves during irradiation: there is growth during irradiation of the fuel/matrix interaction (FMI) layer created during fabrication; Si diffuses from the FMI layer to deeper depths in the U-7Mo particles as the irradiation conditions are made more aggressive; lowering of the Si content in the FMI layer results in an increase in the size of the fission gas bubbles; as the FMI layer grows during irradiation, more Si diffuses from the matrix to the FMI layer/matrix interface; and interlinking of fission gas bubbles in the fuel plate microstructure that may indicate breakaway swelling is not observed.

Microstructural Characterization of Irradiated U0.7ZrH1.6 Using Ultrasonic Techniques

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

Ramuhalli, Pradeep; Jacob, Richard E.; MacFarlan, Paul J.

In recent years, there has been an increased level of effort to understand the changes in microstructure that occur due to irradiation of nuclear fuel. The primary driver for this increased effort is the potential for designing new fuels that are safer and more reliable, in turn enabling new and improved reactor technologies. Much of the data on microstructural change in irradiated fuels is generated through a host of post irradiation examination techniques such as optical microscopy (OM), scanning electron microscopy (SEM), and transmission electron microscopy (TEM) to determine grain structure, porosity, crack geometry, etc. in irradiated fuels. Such “traditional”more » examination techniques were recently used to characterize a novel new fuel consisting of U0.17ZrH1.6 pellets bonded to zircaloy-2 cladded with lead-bismuth eutectic before and after irradiation. However, alternative methods such as ultrasonic inspection can provide an opportunity for nondestructively assessing microstructure in both in-pile and post-irradiation examinations. In this paper, we briefly describe initial results of ultrasonic examination of the U0.17ZrH1.6 pellets (unirradiated and irradiated), in a post-irradiation examination study. Data indicate some correlation with microstructural changes due to irradiation; however, it is not clear what the specific microstructural changes are that are influencing the ultrasonic measurements. Interestingly, specimens with nominally identical burnup show differences in ultrasonic signatures, indicating apparent microstructural differences between these specimens. A summary of the experimental study, preliminary data and findings are presented in this short paper. Additional details of the analysis will be included in the presentation.« less

Biomass particle models with realistic morphology and resolved microstructure for simulations of intraparticle transport phenomena

DOE PAGES

Ciesielski, Peter N.; Crowley, Michael F.; Nimlos, Mark R.; ...

2014-12-09

Biomass exhibits a complex microstructure of directional pores that impact how heat and mass are transferred within biomass particles during conversion processes. However, models of biomass particles used in simulations of conversion processes typically employ oversimplified geometries such as spheres and cylinders and neglect intraparticle microstructure. In this study, we develop 3D models of biomass particles with size, morphology, and microstructure based on parameters obtained from quantitative image analysis. We obtain measurements of particle size and morphology by analyzing large ensembles of particles that result from typical size reduction methods, and we delineate several representative size classes. Microstructural parameters, includingmore » cell wall thickness and cell lumen dimensions, are measured directly from micrographs of sectioned biomass. A general constructive solid geometry algorithm is presented that produces models of biomass particles based on these measurements. Next, we employ the parameters obtained from image analysis to construct models of three different particle size classes from two different feedstocks representing a hardwood poplar species ( Populus tremuloides, quaking aspen) and a softwood pine ( Pinus taeda, loblolly pine). Finally, we demonstrate the utility of the models and the effects explicit microstructure by performing finite-element simulations of intraparticle heat and mass transfer, and the results are compared to similar simulations using traditional simplified geometries. In conclusion, we show how the behavior of particle models with more realistic morphology and explicit microstructure departs from that of spherical models in simulations of transport phenomena and that species-dependent differences in microstructure impact simulation results in some cases.« less

Modification of the Stress-Strain Curve for High-Strength Line Pipe Steel

NASA Astrophysics Data System (ADS)

Jonsson, Katherine

2013-01-01

This thesis presents work performed to improve the work hardening behaviour of an X80 microalloyed steel through various Interrupted Thermal Treatments (ITT). The aim of this work was to determine the relationships between thermal history, microstructure and mechanical properties through both qualitative and quantitative measures. Prior to the ITT experiments, a continuous cooling transformation (CCT) diagram was constructed under no-strain conditions to identify the transformation temperatures and products that are achievable in X80 steel. The thermal treatments were applied using a Gleeble thermal-mechanical simulator to generate a variety of microstructures in various fractions and morphologies. Scanning electron microscopy (SEM) and transmission electron microscopy (TEM) were used to investigate and quantify the microstructures in terms of phase fraction and grain size. The ITT experiments successfully generated microstructures comprised of ferrite, bainitic ferrite, martensite and martensite-austenite (M-A) without the addition of strain. The effect of cooling rates, interrupt temperature, re-heat temperature and hold times were investigated and the mechanical performance was correlated with the quantified microstructures. Although the ITT experiments did not improve the strength relative to a continuously cooled sample, the work hardening coefficient was increased as a result of the interrupted thermal treatments.

The Effects of Helium Bubble Microstructure on Ductility in Annealed and HERF 21Cr-6Ni-9Mn Stainless Steel

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

Tosten, M.H.; Morgan, M.J.

1998-01-01

This study examined the effects of microstructure on the ambient temperature embrittlement from hydrogen isotopes and decay helium in 21Cr-6Ni-9Mn stainless steel. Hydrogen and tritium-exposed 21Cr-6Ni-9Mn stainless steel tensile samples were pulled to failure and then characterized by transmission electron microscopy (TEM) and optical microscopy. This study determined that ductility differences between annealed and high-energy-rate-forged (HERF) stainless steel containing tritium and its decay product, helium, could be related to differences in the helium bubble microstructures. The HERF microstructures were more resistant to tritium-induced embrittlement than annealed microstructures because the high number density of helium bubbles on dislocations trap tritium withinmore » the matrix and away from the grain boundaries.« less

Heat-affected zone microstructure and mechanical properties evolution for laser remanufacturing 35CrMoA axle steel

NASA Astrophysics Data System (ADS)

Feng, Xiangyi; Dong, Shiyun; Yan, Shixing; Liu, Xiaoting; Xu, Binshi; Pan, Fusheng

2018-03-01

In this article, by using orthogonal test the technological test was conducted and the optimum processing of the remanufacturing35CrMoA axle were obtained. The evolution of microstructure and mechanical property of HAZ were investigated. The microstructure of HAZ was characterized by means of OM and SEM. Meanwhile hardness distribution in HAZ and tensile property of cladding-HAZ-substrate samples were measured. The microstructure of cladding and HAZ were observed. The microsturcture evoltion and the mechanism of harden in the HAZ was discussed and revealed. The results indicated that the remanufacturing part has excellent strength due to grain refining and dispersive distribution of nanoscale cementite. The remanufacturing part will have uniform microstructure and hardness matching with that of 35CrMoA axle by using stress-relieving annealing at 580°.

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.

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

PubMed

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

2013-02-01

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

Collagen Organization in Facet Capsular Ligaments Varies With Spinal Region and With Ligament Deformation.

PubMed

Ban, Ehsan; Zhang, Sijia; Zarei, Vahhab; Barocas, Victor H; Winkelstein, Beth A; Picu, Catalin R

2017-07-01

The spinal facet capsular ligament (FCL) is primarily comprised of heterogeneous arrangements of collagen fibers. This complex fibrous structure and its evolution under loading play a critical role in determining the mechanical behavior of the FCL. A lack of analytical tools to characterize the spatial anisotropy and heterogeneity of the FCL's microstructure has limited the current understanding of its structure-function relationships. Here, the collagen organization was characterized using spatial correlation analysis of the FCL's optically obtained fiber orientation field. FCLs from the cervical and lumbar spinal regions were characterized in terms of their structure, as was the reorganization of collagen in stretched cervical FCLs. Higher degrees of intra- and intersample heterogeneity were found in cervical FCLs than in lumbar specimens. In the cervical FCLs, heterogeneity was manifested in the form of curvy patterns formed by collections of collagen fibers or fiber bundles. Tensile stretch, a common injury mechanism for the cervical FCL, significantly increased the spatial correlation length in the stretch direction, indicating an elongation of the observed structural features. Finally, an affine estimation for the change of correlation length under loading was performed which gave predictions very similar to the actual values. These findings provide structural insights for multiscale mechanical analyses of the FCLs from various spinal regions and also suggest methods for quantitative characterization of complex tissue patterns.

Structural characterization of the packings of granular regular polygons.

PubMed

Wang, Chuncheng; Dong, Kejun; Yu, Aibing

2015-12-01

By using a recently developed method for discrete modeling of nonspherical particles, we simulate the random packings of granular regular polygons with three to 11 edges under gravity. The effects of shape and friction on the packing structures are investigated by various structural parameters, including packing fraction, the radial distribution function, coordination number, Voronoi tessellation, and bond-orientational order. We find that packing fraction is generally higher for geometrically nonfrustrated regular polygons, and can be increased by the increase of edge number and decrease of friction. The changes of packing fraction are linked with those of the microstructures, such as the variations of the translational and orientational orders and local configurations. In particular, the free areas of Voronoi tessellations (which are related to local packing fractions) can be described by log-normal distributions for all polygons. The quantitative analyses establish a clearer picture for the packings of regular polygons.

Study of the influence of volume fraction of ceramic inclusions in NiCr-TiC composite with columnar structure on its mechanical behavior

NASA Astrophysics Data System (ADS)

Eremina, Galina M.; Smolin, Alexey Yu.; Shilko, Evgeny V.

2017-12-01

Metal-ceramic materials are characterized by high mechanical and tribological properties. The surface treatment of the composite by an electron beam in inert gas plasma leads to a qualitative and quantitative change in its microstructure as well as to a change in mechanical properties of the components: a columnar structure forms in the modified layer. Different treatment regimes result in different concentrations of inclusions in the surface layer. In this paper, the effect of the volume concentration of inclusions on the integral mechanical properties of a dispersion-strengthened NiCr-TiC composite is studied on the basis of 3D numerical simulation. The results of computer simulation show that the change in concentration significantly affects the integral mechanical characteristics of the composite material as well as the nature of the nucleation and development of damages in it.

Hierarchical microstructures in CZT

NASA Astrophysics Data System (ADS)

Sundaram, S. K.; Henager, C. H.; Edwards, D. J.; Schemer-Kohrn, A. L.; Bliss, M.; Riley, B. R.; Toloczko, M. B.; Lynn, K. G.

2011-10-01

Advanced characterization tools, such as electron backscatter diffraction and transmitted IR microscopy, are being applied to study critical microstructural features and orientation relations in as-grown CZT crystals to aid in understanding the relation between structure and properties in radiation detectors. Even carefully prepared single crystals of CZT contain regions of slight misorientation, Te-particles, and dislocation networks that must be understood for more accurate models of detector response. This paper describes initial research at PNNL into the hierarchy of microstructures observed in CZT grown via the vertical gradient freeze or vertical Bridgman method at PNNL and WSU.

Nonequilibrium synthesis of NbAl3 and Nb-Al-V alloys by laser cladding. I - Microstructure evolution

NASA Technical Reports Server (NTRS)

Sircar, S.; Chattopadhyay, K.; Mazumder, J.

1992-01-01

The evolution of the microstructure in NbAl3 synthesized by a laser cladding technique (a rapid solidification process, with cooling rates up to 10 exp 6 C/sec) is investigated, and the phases are identified using convergent beam electron diffraction. Two new metastable phases were identified and characterized in detail. The effect of adding V on the final microstructure was also investigated, and the various phase chemistries and the partitioning of different elements into different phases were studied.

Transport efficiency in transdermal drug delivery: What is the role of fluid microstructure?

PubMed

Liuzzi, Roberta; Carciati, Antonio; Guido, Stefano; Caserta, Sergio

2016-03-01

Interaction of microstructured fluids with skin is ubiquitous in everyday life, from the use of cosmetics, lotions, and drugs, to personal care with detergents or soaps. The formulation of microstructured fluids is crucial for the control of the transdermal transport. In biomedical applications transdermal delivery is an efficient approach, alternative to traditional routes like oral and parenteral administration, for local release of drugs. Poor skin permeability, mainly due to its outer layer, which acts as the first barrier against the entry of external compounds, greatly limits the applicability of transdermal delivery. In this review, we focus on recent studies on the improvement of skin transport efficiency by using microemulsions (ME). Quantitative techniques, which are able to investigate both skin morphology and penetration processes, are also reviewed. ME are increasingly used as transdermal systems due to their low preparation cost, stability and high bioavailability. ME may act as penetration enhancers for many active principles, but ME microstructure should be chosen appropriately considering several factors such as ratio and type of ingredients and physic-chemical properties of the active components. ME microstructure is strongly affected by the flow conditions applied during processing, or during spreading and rubbing onto skin. Although the role played by ME microstructure has been generally recognized, the skin transport mechanisms associated with different ME microstructures are still to be elucidated and further investigations are required to fully exploit the potential of ME in transdermal delivery. Copyright © 2015 Elsevier B.V. All rights reserved.

Effect of low-dose CT and iterative reconstruction on trabecular bone microstructure assessment

NASA Astrophysics Data System (ADS)

Kopp, Felix K.; Baum, Thomas; Nasirudin, Radin A.; Mei, Kai; Garcia, Eduardo G.; Burgkart, Rainer; Rummeny, Ernst J.; Bauer, Jan S.; Noël, Peter B.

2016-03-01

The trabecular bone microstructure is an important factor in the development of osteoporosis. It is well known that its deterioration is one effect when osteoporosis occurs. Previous research showed that the analysis of trabecular bone microstructure enables more precise diagnoses of osteoporosis compared to a sole measurement of the mineral density. Microstructure parameters are assessed on volumetric images of the bone acquired either with high-resolution magnetic resonance imaging, high-resolution peripheral quantitative computed tomography or high-resolution computed tomography (CT), with only CT being applicable to the spine, which is one of clinically most relevant fracture sites. However, due to the high radiation exposure for imaging the whole spine these measurements are not applicable in current clinical routine. In this work, twelve vertebrae from three different donors were scanned with standard and low radiation dose. Trabecular bone microstructure parameters were assessed for CT images reconstructed with statistical iterative reconstruction (SIR) and analytical filtered backprojection (FBP). The resulting structure parameters were correlated to the biomechanically determined fracture load of each vertebra. Microstructure parameters assessed for low-dose data reconstructed with SIR significantly correlated with fracture loads as well as parameters assessed for standard-dose data reconstructed with FBP. Ideal results were achieved with low to zero regularization strength yielding microstructure parameters not significantly different from those assessed for standard-dose FPB data. Moreover, in comparison to other approaches, superior noise-resolution trade-offs can be found with the proposed methods.

Interface Pattern Selection in Directional Solidification

NASA Technical Reports Server (NTRS)

Trivedi, Rohit; Tewari, Surendra N.

2001-01-01

The central focus of this research is to establish key scientific concepts that govern the selection of cellular and dendritic patterns during the directional solidification of alloys. Ground-based studies have established that the conditions under which cellular and dendritic microstructures form are precisely where convection effects are dominant in bulk samples. Thus, experimental data can not be obtained terrestrially under pure diffusive regime. Furthermore, reliable theoretical models are not yet possible which can quantitatively incorporate fluid flow in the pattern selection criterion. Consequently, microgravity experiments on cellular and dendritic growth are designed to obtain benchmark data under diffusive growth conditions that can be quantitatively analyzed and compared with the rigorous theoretical model to establish the fundamental principles that govern the selection of specific microstructure and its length scales. In the cellular structure, different cells in an array are strongly coupled so that the cellular pattern evolution is controlled by complex interactions between thermal diffusion, solute diffusion and interface effects. These interactions give infinity of solutions, and the system selects only a narrow band of solutions. The aim of this investigation is to obtain benchmark data and develop a rigorous theoretical model that will allow us to quantitatively establish the physics of this selection process.

A study on the influence of microstructure on small fatigue cracks

NASA Astrophysics Data System (ADS)

Castelluccio, Gustavo M.

In spite of its significance in industrial applications, the prediction of the influence of microstructure on the early stages of crack formation and growth in engineering alloys remains underdeveloped. The formation and early growth of fatigue cracks in the high cycle fatigue regime lasts for much of the fatigue life, and it is strongly influenced by microstructural features such as grain size, twins and morphological and crystallographic texture. However, most fatigue models do not predict the in uence of the microstructure on early stages of crack formation, or they employ parameters that should be calibrated with experimental data from specimens with microstructures of interest. These post facto strategies are adequate to characterize materials, but they are not fully appropriate to aid in the design of fatigue-resistant engineering alloys. This thesis considers finite element computational models that explicitly render the microstructure of selected FCC metallic systems and introduces a fatigue methodology that estimates transgranular and intergranular fatigue growth for microstructurally small cracks. The driving forces for both failure modes are assessed by means of fatigue indicators, which are used along with life correlations to estimate the fatigue life. Furthermore, cracks with meandering paths are modeled by considering crack growth on a grain-by-grain basis with a damage model embedded analytically to account for stress and strain redistribution as the cracks extend. The methodology is implemented using a crystal plasticity constitutive model calibrated for studying the effect of microstructure on early fatigue life of a powder processed Ni-base RR1000 superalloy at elevated temperature under high cycle fatigue conditions. This alloy is employed for aircraft turbine engine disks, which undergo a thermomechanical production process to produce a controlled bimodal grain size distribution. The prediction of the fatigue life for this complex microstructure presents particular challenges that are discussed and addressed. The conclusions of this work describe the mechanistic of microstructural small crack. In particular, the fatigue crack growth driving force has been characterized as it evolves within grains and crosses to other grains. Furthermore, the computational models serve as a tool to assess the effects of microstructural features on early stages of fatigue crack formation and growth, such as distributions of grain size and twins.

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.

Influence of coarsened and rafted microstructures on the thermomechanical fatigue of a Ni-base superalloy

DOE PAGES

Kirka, M. M.; Brindley, K. A.; Neu, R. W.; ...

2015-08-17

The aging of the microstructure of Ni-base superalloys during service is mainly characterized by coarsening and rafting of the γ' precipitates. The influence of these different aged microstructures on thermomechanical fatigue (TMF) under either continuously cycled (CC) and creep-fatigue (CF) was investigated. Three different aged microstructures, generated through accelerated aging and pre-creep treatments, were studied: stress-free coarsened γ', rafted with orientation perpendicular to loading direction (N-raft), and rafted with orientation parallel to loading direction (P-raft). Under most conditions, the aged microstructures were less resistant to TMF than the virgin microstructure; however, there were exceptions. Both stress-free coarsened and N-raft microstructuresmore » resulted in a reduction in TMF life under both CC and CF conditions in comparison to the virgin material. P-raft microstructure also resulted in reduction in TMF life under CC conditions; however, an increase in life over that of the virgin material was observed under CF conditions. Finally, these differences are discussed and hypothesized to be related to the interactions of the dislocations in the γ channels with γ' precipitates.« less

Analysis of the Microstructure of Titles in the INSPEC Data-Base

ERIC Educational Resources Information Center

And Others; Lynch, Michael F.

1973-01-01

A high degree of constancy has been found in the microstructure of titles of samples of the INSPEC data base taken over a three-year period. Character and digram frequencies are relatively stable, while variable-length character-strings characterizing samples separated by three years in time show close similarities. (2 references) (Author/SJ)

Effect of Isothermal Hold on the Microstructural Evolution of the Stainless Steel 304L/Zircaloy-4 Interface

NASA Astrophysics Data System (ADS)

Lebaili, A.; Taouinet, M.; Nibou, D.; Lebaili, S.; Hodaj, F.

2017-07-01

The transition from solid-state bonding of the stainless steel 304L/Zircaloy-4 diffusion couple to a partial liquid-phase bonding is important for the bonding process at temperatures ranging from 950 to 1050 °C. In this study, the temperature at which a melting process occurs at the interface after 45 min of isothermal holdings is determined experimentally. This melting process leads to a drastic change in the thickness of the reaction products zone (RPZ) as well as on its microstructure. Diffusion couples were characterized by SEM-EDS, and quantitative chemical analyses of different phases are performed by EPMA. The RPZ consists of three layers: the (α-Fe-Cr) phase layer and two layers consisting of Zr(Fe,Cr)2 (ɛ), Zr2(Fe,Ni) and (α-Zr) phases. The thickness of these layers strongly depends on the holding temperature. The analysis allowed the description of the physicochemical phenomena occurring during isothermal holding as well as during cooling. The solidification paths are determined at 1000, 1020 and 1050 °C. Hardness tests are performed on the bonded samples in order to qualify the mechanical properties of different phases of the RPZ. This study leads to a better understanding of the complex phenomena intervening in the joining process which is very useful for applications in industrial scale.

Detecting and modelling structures on the micro and the macro scales: Assessing their effects on solute transport behaviour

NASA Astrophysics Data System (ADS)

Haslauer, C. P.; Bárdossy, A.; Sudicky, E. A.

2017-09-01

This paper demonstrates quantitative reasoning to separate the dataset of spatially distributed variables into different entities and subsequently characterize their geostatistical properties, properly. The main contribution of the paper is a statistical based algorithm that matches the manual distinction results. This algorithm is based on measured data and is generally applicable. In this paper, it is successfully applied at two datasets of saturated hydraulic conductivity (K) measured at the Borden (Canada) and the Lauswiesen (Germany) aquifers. The boundary layer was successfully delineated at Borden despite its only mild heterogeneity and only small statistical differences between the divided units. The methods are verified with the more heterogeneous Lauswiesen aquifer K data-set, where a boundary layer has previously been delineated. The effects of the macro- and the microstructure on solute transport behaviour are evaluated using numerical solute tracer experiments. Within the microscale structure, both Gaussian and non-Gaussian models of spatial dependence of K are evaluated. The effects of heterogeneity both on the macro- and the microscale are analysed using numerical tracer experiments based on four scenarios: including or not including the macroscale structures and optimally fitting a Gaussian or a non-Gaussian model for the spatial dependence in the micro-structure. The paper shows that both micro- and macro-scale structures are important, as in each of the four possible geostatistical scenarios solute transport behaviour differs meaningfully.

Additive Manufacturing of Single-Crystal Superalloy CMSX-4 Through Scanning Laser Epitaxy: Computational Modeling, Experimental Process Development, and Process Parameter Optimization

NASA Astrophysics Data System (ADS)

Basak, Amrita; Acharya, Ranadip; Das, Suman

2016-08-01

This paper focuses on additive manufacturing (AM) of single-crystal (SX) nickel-based superalloy CMSX-4 through scanning laser epitaxy (SLE). SLE, a powder bed fusion-based AM process was explored for the purpose of producing crack-free, dense deposits of CMSX-4 on top of similar chemistry investment-cast substrates. Optical microscopy and scanning electron microscopy (SEM) investigations revealed the presence of dendritic microstructures that consisted of fine γ' precipitates within the γ matrix in the deposit region. Computational fluid dynamics (CFD)-based process modeling, statistical design of experiments (DoE), and microstructural characterization techniques were combined to produce metallurgically bonded single-crystal deposits of more than 500 μm height in a single pass along the entire length of the substrate. A customized quantitative metallography based image analysis technique was employed for automatic extraction of various deposit quality metrics from the digital cross-sectional micrographs. The processing parameters were varied, and optimal processing windows were identified to obtain good quality deposits. The results reported here represent one of the few successes obtained in producing single-crystal epitaxial deposits through a powder bed fusion-based metal AM process and thus demonstrate the potential of SLE to repair and manufacture single-crystal hot section components of gas turbine systems from nickel-based superalloy powders.

Laser engineered net shaping of quasi-continuous network microstructural TiB reinforced titanium matrix bulk composites: Microstructure and wear performance

NASA Astrophysics Data System (ADS)

Hu, Yingbin; Ning, Fuda; Wang, Hui; Cong, Weilong; Zhao, Bo

2018-02-01

Titanium (Ti) and its alloys have been successfully applied to the aeronautical and biomedical industries. However, their poor tribological properties restrict their fields of applications under severe wear conditions. Facing to these challenges, this study investigated TiB reinforced Ti matrix composites (TiB-TMCs), fabricated by in-situ laser engineered net shaping (LENS) process, through analyzing parts quality, microstructure formation mechanisms, microstructure characterizations, and workpiece wear performance. At high B content areas (original B particle locations), reaction between Ti and B particles took place, generating flower-like microstructure. At low B content areas, eutectic TiB nanofibers contacted with each other with the formation of crosslinking microstructure. The crosslinking microstructural TiB aggregated and connected at the boundaries of Ti grains, forming a three-dimensional quasi-continuous network microstructure. The results show that compared with commercially pure Ti bulk parts, the TiB-TMCs exhibited superior wear performance (i.e. indentation wear resistance and friction wear resistance) due to the present of TiB reinforcement and the innovative microstructures formed inside TiB-TMCs. In addition, the qualities of the fabricated parts were improved with fewer interior defects by optimizing laser power, thus rendering better wear performance.

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

Dynamic mechanical properties of hydroxyapatite/polyethylene oxide nanocomposites: characterizing isotropic and post-processing microstructures

NASA Astrophysics Data System (ADS)

Shofner, Meisha; Lee, Ji Hoon

2012-02-01

Compatible component interfaces in polymer nanocomposites can be used to facilitate a dispersed morphology and improved physical properties as has been shown extensively in experimental results concerning amorphous matrix nanocomposites. In this research, a block copolymer compatibilized interface is employed in a semi-crystalline matrix to prevent large scale nanoparticle clustering and enable microstructure construction with post-processing drawing. The specific materials used are hydroxyapatite nanoparticles coated with a polyethylene oxide-b-polymethacrylic acid block copolymer and a polyethylene oxide matrix. Two particle shapes are used: spherical and needle-shaped. Characterization of the dynamic mechanical properties indicated that the two nanoparticle systems provided similar levels of reinforcement to the matrix. For the needle-shaped nanoparticles, the post-processing step increased matrix crystallinity and changed the thermomechanical reinforcement trends. These results will be used to further refine the post-processing parameters to achieve a nanocomposite microstructure with triangulated arrays of nanoparticles.

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.

Microstructural Evolution of HSLA ISO 3183 X80M (API 5L X80) Friction Stir Welded Joints

NASA Astrophysics Data System (ADS)

Hermenegildo, Tahiana F. C.; Santos, Tiago F. A.; Torres, Edwar A.; Afonso, Conrado R. M.; Ramirez, Antonio J.

2018-03-01

Evaluation was made of friction stir welded joints, identifying conditions that resulted in satisfactory welded joints free from defects and with microstructural characteristics that provided good mechanical properties. Microstructural characterization and cooling curve analysis of the joints with lower and higher heat inputs evidenced deformation below and above the non-recrystallization temperature (Tnr) and dynamic recrystallization during microstructural evolution. Microscopy analyses showed acicular ferrite, bainitic ferrite, and coalesced bainite microstructures in the stir zone of the cold weld (lower heat input), while the stir zone of the hot weld (higher heat input) contained bainitic ferrite, acicular ferrite, coalesced bainite, martensite, and dispersed carbides. Granular bainite and dispersed carbides were observed in all the heat affected zones. Analysis of the microstructural transformations, together with the thermal history of the joints, showed that the variable that had the greatest influence on the morphology of the bainite (granular bainite/bainitic ferrite) was the deformation temperature.

PVA/NaCl/MgO nanocomposites-microstructural analysis by whole pattern fitting method

NASA Astrophysics Data System (ADS)

Prashanth, K. S.; Mahesh, S. S.; Prakash, M. B. Nanda; Somashekar, R.; Nagabhushana, B. M.

2018-04-01

The nanofillers in the macromolecular matrix have displayed noteworthy changes in the structure and reactivity of the polymer nanocomposites. Novel functional materials usually consist of defects and are largely disordered. The intriguing properties of these materials are often attributed to defects. X-ray line profiles from powder diffraction reveal the quantitative information about size distribution and shape of diffracting domains which governs the contribution from small conventional X-ray diffraction (XRD) techniques to enumerate the microstructural information. In this study the MgO nanoparticles were prepared by solution combustion method and PVA/NaCl/MgO nanocomposite films were synthesized by the solvent cast method. Microstructural parameters viz crystal defects like stacking faults and twin faults, compositional inhomogeneity, crystallite size and lattice strain (g in %), were extracted using whole pattern fitting method.

MRI tools for assessment of microstructure and nephron function of the kidney.

PubMed

Xie, Luke; Bennett, Kevin M; Liu, Chunlei; Johnson, G Allan; Zhang, Jeff Lei; Lee, Vivian S

2016-12-01

MRI can provide excellent detail of renal structure and function. Recently, novel MR contrast mechanisms and imaging tools have been developed to evaluate microscopic kidney structures including the tubules and glomeruli. Quantitative MRI can assess local tubular function and is able to determine the concentrating mechanism of the kidney noninvasively in real time. Measuring single nephron function is now a near possibility. In parallel to advancing imaging techniques for kidney microstructure is a need to carefully understand the relationship between the local source of MRI contrast and the underlying physiological change. The development of these imaging markers can impact the accurate diagnosis and treatment of kidney disease. This study reviews the novel tools to examine kidney microstructure and local function and demonstrates the application of these methods in renal pathophysiology. Copyright © 2016 the American Physiological Society.

Processing of MnBi bulk magnets with enhanced energy product

DOE PAGES

Poudyal, Narayan; Liu, Xubo; Wang, Wei; ...

2016-02-23

Here, we report magnetic properties and microstructure of high energy-product MnBi bulk magnets fabricated by low-temperature ball-milling and warm compaction technique. A maximum energy product (BH) max of 8.4 MGOe and a coercivity of 6.2 kOe were obtained in the bulk MnBi magnet at room temperature. Magnetic characterization at elevated temperatures showed an increase in coercivity to 16.2 kOe while (BH) max value decreased to 6.8 MGOe at 400 K. Microstructure characterization revealed that the bulk magnets consist of oriented uniform nanoscale grains with average size about 50 nm.

Analytical Ultrasonics in Materials Research and Testing

NASA Technical Reports Server (NTRS)

Vary, A.

1986-01-01

Research results in analytical ultrasonics for characterizing structural materials from metals and ceramics to composites are presented. General topics covered by the conference included: status and advances in analytical ultrasonics for characterizing material microstructures and mechanical properties; status and prospects for ultrasonic measurements of microdamage, degradation, and underlying morphological factors; status and problems in precision measurements of frequency-dependent velocity and attenuation for materials analysis; procedures and requirements for automated, digital signal acquisition, processing, analysis, and interpretation; incentives for analytical ultrasonics in materials research and materials processing, testing, and inspection; and examples of progress in ultrasonics for interrelating microstructure, mechanical properites, and dynamic response.

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

Pore- and micro-structural characterization of a novel structural binder based on iron carbonation

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

Das, Sumanta, E-mail: Sumanta.Das@asu.edu; Stone, David, E-mail: dajstone@gmail.com; Convey, Diana, E-mail: Diana.Convey@asu.edu

2014-12-15

The pore- and micro-structural features of a novel binding material based on the carbonation of waste metallic iron powder are reported in this paper. The binder contains metallic iron powder as the major ingredient, followed by additives containing silica and alumina to facilitate favorable reaction product formation. Compressive strengths sufficient for a majority of concrete applications are attained. The material pore structure is investigated primarily through mercury intrusion porosimetry whereas electron microscopy is used for microstructural characterization. Reduction in the overall porosity and the average pore size with an increase in carbonation duration from 1 day to 4 days ismore » noticed. The pore structure features are used in predictive models for gas and moisture transport (water vapor diffusivity and moisture permeability) through the porous medium which dictates its long-term durability when used in structural applications. Comparisons of the pore structure with those of a Portland cement paste are also provided. The morphology of the reaction products in the iron-based binder, and the distribution of constituent elements in the microstructure are also reported. - Highlights: • Carbonation of iron produces a dense microstructure. • Pore volume in iron carbonate lower, critical size higher than those in OPC pastes • Reaction product contains iron, carbon, silicon, aluminum and calcium. • Power-law for porosity-moisture permeability relationship was established.« less

Damage Mechanisms and Mechanical Properties of High-Strength Multiphase Steels

PubMed Central

Heibel, Sebastian; Dettinger, Thomas; Nester, Winfried; Tekkaya, A. Erman

2018-01-01

The usage of high-strength steels for structural components and reinforcement parts is inevitable for modern car-body manufacture in reaching lightweight design as well as increasing passive safety. Depending on their microstructure these steels show differing damage mechanisms and various mechanical properties which cannot be classified comprehensively via classical uniaxial tensile testing. In this research, damage initiation, evolution and final material failure are characterized for commercially produced complex-phase (CP) and dual-phase (DP) steels in a strength range between 600 and 1000 MPa. Based on these investigations CP steels with their homogeneous microstructure are characterized as damage tolerant and hence less edge-crack sensitive than DP steels. As final fracture occurs after a combination of ductile damage evolution and local shear band localization in ferrite grains at a characteristic thickness strain, this strain measure is introduced as a new parameter for local formability. In terms of global formability DP steels display advantages because of their microstructural composition of soft ferrite matrix including hard martensite particles. Combining true uniform elongation as a measure for global formability with the true thickness strain at fracture for local formability the mechanical material response can be assessed on basis of uniaxial tensile testing incorporating all microstructural characteristics on a macroscopic scale. Based on these findings a new classification scheme for the recently developed high-strength multiphase steels with significantly better formability resulting of complex underlying microstructures is introduced. The scheme overcomes the steel designations using microstructural concepts, which provide no information about design and production properties. PMID:29747417

Microstructure and yield strength effects on hydrogen and tritium induced cracking in HERF (high-energy-rate-forged) stainless steel

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

Morgan, M J; Tosten, M H

1989-01-01

Rising-load J-integral measurements and falling-load threshold stress intensity measurements were used to characterize hydrogen and tritium induced cracking in high-energy-rate-forged (HERF) 21-6-9 stainless steel. Samples having yield strengths in the range 517--930 MPa were thermally charged with either hydrogen or tritium and tested at room temperature in either air or high-pressure hydrogen gas. In general, the hydrogen isotopes reduced the fracture toughness by affecting the fracture process. Static recrystallization in the HERF microstructures affected the material's fracture toughness and its relative susceptibility to hydrogen and tritium induced fracture. In hydrogen-exposed samples, the reduction in fracture toughness was primarily dependent onmore » the susceptibility of the microstructure to intergranular fracture and only secondarily affected by strength in the range of 660 to 930 MPa. Transmission-electron microscopy observations revealed that the microstructures least susceptible to hydrogen-induced intergranular cracking contained patches of fully recrystallized grains. These grains are surrounded by highly deformed regions containing a high number density of dislocations. The microstructure can best be characterized as duplex'', with soft recrystallized grains embedded in a hard, deformed matrix. The microstructures most susceptible to hydrogen-induced intergranular fracture showed no well-developed recrystallized grains. The patches of recrystallized grains seemed to act as crack barriers to hydrogen-induced intergranular fracture. In tritium-exposed-and-aged samples, the amount of static recrystallization also affected the fracture toughness properties but to a lesser degree. 7 refs., 25 figs.« less

In situ, 3D characterization of the deformation mechanics of a superelastic NiTi shape memory alloy single crystal under multiscale constraint

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

Paranjape, Harshad M.; Paul, Partha P.; Amin-Ahmadi, Behnam

Microstructural elements in NiTi shape memory alloys (SMAs) – precipitates, phase boundaries, inclusions, grain boundaries – can be viewed as sources of multiscale constraint that influence their deformation response. In this paper, we characterized in situ, and in 3D, the deformation and the evolution of microstructure during a tension test in a superelastic NiTi specimen containing some of these sources of constraint. The method used was far-field high-energy X-ray diffraction microscopy (ff-HEDM), complemented by electron microscopy. We simulated the local stress state in the specimen using a microstructural model informed by the experimental data. Using these combined microstructure, deformation, andmore » stress data, we report three phenomena, and relate them to specific sources of constraint. During initial elastic loading, axial lattice strain in austenite increased monotonically. On partial stress-induced phase transformation to martensite, the stress redistributed to both phases leading to a stress relaxation in austenite. The specimen contained a dense distribution of inclusions, which led to the activation of martensite habit plane variants that produce less than theoretical maximum transformation strain. Large Ni 4Ti 3 precipitates potentially contributed to the poor transformation response. Under load, proportional gradients in local rotation and elastic stretch developed in the martensite phase, because of the constraint at phase interfaces. Finally, this combined ff-HEDM, electron microscopy, microstructural simulation toolbox provides a versatile method to understand the effect of constraint on inelastic deformation in other alloys with hierarchical microstructure.« less

In situ, 3D characterization of the deformation mechanics of a superelastic NiTi shape memory alloy single crystal under multiscale constraint

DOE PAGES

Paranjape, Harshad M.; Paul, Partha P.; Amin-Ahmadi, Behnam; ...

2017-11-20

Microstructural elements in NiTi shape memory alloys (SMAs) – precipitates, phase boundaries, inclusions, grain boundaries – can be viewed as sources of multiscale constraint that influence their deformation response. In this paper, we characterized in situ, and in 3D, the deformation and the evolution of microstructure during a tension test in a superelastic NiTi specimen containing some of these sources of constraint. The method used was far-field high-energy X-ray diffraction microscopy (ff-HEDM), complemented by electron microscopy. We simulated the local stress state in the specimen using a microstructural model informed by the experimental data. Using these combined microstructure, deformation, andmore » stress data, we report three phenomena, and relate them to specific sources of constraint. During initial elastic loading, axial lattice strain in austenite increased monotonically. On partial stress-induced phase transformation to martensite, the stress redistributed to both phases leading to a stress relaxation in austenite. The specimen contained a dense distribution of inclusions, which led to the activation of martensite habit plane variants that produce less than theoretical maximum transformation strain. Large Ni 4Ti 3 precipitates potentially contributed to the poor transformation response. Under load, proportional gradients in local rotation and elastic stretch developed in the martensite phase, because of the constraint at phase interfaces. Finally, this combined ff-HEDM, electron microscopy, microstructural simulation toolbox provides a versatile method to understand the effect of constraint on inelastic deformation in other alloys with hierarchical microstructure.« less

C-Coupon Studies of CMCS: Fracture Behavior and Microstructural Characterization

NASA Technical Reports Server (NTRS)

Hurwitz, Frances I.; Calomino, Anthony M.; McCue, Terry R.; Abdul-Aziz, Ali

2001-01-01

A curved beam 'C-coupon' was used to assess fracture behavior in a Sylramic(tm)/melt infiltration (MI) SiC matrix composite. Failure stresses and fracture mechanisms, as determined by optical and scanning electron microstructural analysis, are compared with finite element stress calculations to analyze failure modes. Material microstructure was found to have a strong influence on mechanical behavior. Fracture occurs in interlaminar tension (ILT), provided that the ratio of ILT to tensile strength for the material is less than the ratio of radial to hoop stresses for the C-coupon geometry. Utilization of 3D architectures to improve interlaminar strength requires significant development efforts to incorporate through thickness fibers in regions with high curvatures while maintaining uniform thickness, radius, and microstructure.

Mechanical and Microstructural Effects of Thermal Aging on Cast Duplex Stainless Steels by Experiment and Finite Element Method

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

Schwarm, Samuel C.; Mburu, Sarah N.; Kolli, Ratna P.

Cast duplex stainless steel piping in light water nuclear reactors expe- rience thermal aging embrittlement during operational service. Interest in extending the operational life to 80 years requires an increased understanding of the microstructural evolution and corresponding changes in mechanical behavior. We analyze the evolution of the microstructure during thermal aging of cast CF-3 and CF-8 stainless steels using electron microscopy and atom probe tomography. The evolution of the mechanical properties is measured concurrently by mechanical methods such as tensile tests, Charpy V-notch tests, and instrumented nanoinden- tation. A microstructure-based finite element method model is developed and uti- lized inmore » conjunction with the characterization results in order to correlate the local stress-strain effects in the microstructure with the bulk measurements. This work is supported by the DOE Nuclear Energy University Programs (NEUP), contract number DE-NE0000724.« less

Microstructural characterization of Ti-6Al-4V metal chips by focused ion beam (FIB) and transmission electron microscopy (TEM)

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

Schneider, Judy; Dong, Lei; Howe, Jane Y

2011-01-01

The microstructure of the secondary deformation zone (SDZ) near the cutting surface in metal chips of Ti-6Al-4V formed during machining was investigated using focused ion beam (FIB) specimen preparation and transmission electron microscopy (TEM) imaging. Use of the FIB allowed precise extraction of the specimen across this region to reveal its inhomogeneous microstructure resulting from the non-uniform distribution of strain, strain rate, and temperature generated during the cutting process. Initial imaging from conventional TEM foil preparation revealed microstructures ranging from heavily textured to regions of fine grains. Using FIB preparation, the transverse microstructure could be interpreted as fine grains nearmore » the cutting surface which transitioned to coarse grains toward the free surface. At the cutting surface a 10 nm thick recrystallized layer was observed capping a 20 nm thick amorphous layer.« 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.

Three-Dimensional Characterization and Modeling of Microstructural Weak Links for Spall Damage in FCC Metals

DOE PAGES

Krishnan, Kapil; Brown, Andrew; Wayne, Leda; ...

2014-11-25

Local microstructural weak links for spall damage were investigated using three-dimensional (3-D) characterization in multicrystalline copper samples (grain size ≈ 450 µm) shocked with laser-driven plates at low pressures (2 to 4 GPa). The thickness of samples and flyer plates, approximately 1000 and 500 µm respectively, led to short pressure pulses that allowed isolating microstructure effects on local damage characteristics. Electron Backscattering Diffraction and optical microscopy were used to relate the presence, size, and shape of porosity to local microstructure. The experiments were complemented with 3-D finite element simulations of individual grain boundaries (GBs) that resulted in large damage volumesmore » using crystal plasticity coupled with a void nucleation and growth model. Results from analysis of these damage sites show that the presence of a GB-affected zone, where strain concentration occurs next to a GB, correlates strongly with damage localization at these sites, most likely due to the inability of maintaining strain compatibility across these interfaces, with additional effects due to the inclination of the GB with respect to the shock. Results indicate that strain compatibility plays an important role on intergranular spall damage in metallic materials.« less

Microstructural characterization of dissimilar welds between Incoloy 800H and 321 Austenitic Stainless Steel

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

Sayiram, G., E-mail: sayiram.g@vit.ac.in; Arivazhagan, N.

2015-04-15

In this work, the microstructural character of dissimilar welds between Incoloy 800H and 321 Stainless Steel has been discussed. The microscopic examination of the base metals, fusion zones and interfaces was characterized using an optical microscope and scanning electron microscopy. The results revealed precipitates of Ti (C, N) in the austenitic matrix along the grain boundaries of the base metals. Migration of grain boundaries in the Inconel 82 weld metal was very extensive when compared to Inconel 617 weldment. Epitaxial growth was observed in the 617 weldment which increases the strength and ductility of the weld metal. Unmixed zone nearmore » the fusion line between 321 Stainless Steel and Inconel 82 weld metal was identified. From the results, it has been concluded that Inconel 617 filler metal is a preferable choice for the joint between Incoloy 800H and 321 Stainless Steel. - Highlights: • Failure mechanisms produced by dissimilar welding of Incoloy 800H to AISI 321SS • Influence of filler wire on microstructure properties • Contemplative comparisons of metallurgical aspects of these weldments • Microstructure and chemical studies including metallography, SEM–EDS • EDS-line scan study at interface.« less

A diffusion model-free framework with echo time dependence for free-water elimination and brain tissue microstructure characterization.

PubMed

Molina-Romero, Miguel; Gómez, Pedro A; Sperl, Jonathan I; Czisch, Michael; Sämann, Philipp G; Jones, Derek K; Menzel, Marion I; Menze, Bjoern H

2018-03-23

The compartmental nature of brain tissue microstructure is typically studied by diffusion MRI, MR relaxometry or their correlation. Diffusion MRI relies on signal representations or biophysical models, while MR relaxometry and correlation studies are based on regularized inverse Laplace transforms (ILTs). Here we introduce a general framework for characterizing microstructure that does not depend on diffusion modeling and replaces ill-posed ILTs with blind source separation (BSS). This framework yields proton density, relaxation times, volume fractions, and signal disentanglement, allowing for separation of the free-water component. Diffusion experiments repeated for several different echo times, contain entangled diffusion and relaxation compartmental information. These can be disentangled by BSS using a physically constrained nonnegative matrix factorization. Computer simulations, phantom studies, together with repeatability and reproducibility experiments demonstrated that BSS is capable of estimating proton density, compartmental volume fractions and transversal relaxations. In vivo results proved its potential to correct for free-water contamination and to estimate tissue parameters. Formulation of the diffusion-relaxation dependence as a BSS problem introduces a new framework for studying microstructure compartmentalization, and a novel tool for free-water elimination. © 2018 International Society for Magnetic Resonance in Medicine.

TEM Characterization of High Burn-up Microstructure of U-7Mo Alloy

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

Jian Gan; Brandon Miller; Dennis Keiser

2014-04-01

As an essential part of global nuclear non-proliferation effort, the RERTR program is developing low enriched U-Mo fuels (< 20% U-235) for use in research and test reactors that currently employ highly enriched uranium fuels. One type of fuel being developed is a dispersion fuel plate comprised of U-7Mo particles dispersed in Al alloy matrix. Recent TEM characterizations of the ATR irradiated U-7Mo dispersion fuel plates include the samples with a local fission densities of 4.5, 5.2, 5.6 and 6.3 E+21 fissions/cm3 and irradiation temperatures of 101-136?C. The development of the irradiated microstructure of the U-7Mo fuel particles consists ofmore » fission gas bubble superlattice, large gas bubbles, solid fission product precipitates and their association to the large gas bubbles, grain subdivision to tens or hundreds of nanometer size, collapse of bubble superlattice, and amorphisation. This presentation will describe the observed microstructures specifically focusing on the U-7Mo fuel particles. The impact of the observed microstructure on the fuel performance and the comparison of the relevant features with that of the high burn-up UO2 fuels will be discussed.« less

Brain tissues atrophy is not always the best structural biomarker of physiological aging: A multimodal cross-sectional study.

PubMed

Cherubini, Andrea; Caligiuri, Maria Eugenia; Péran, Patrice; Sabatini, Umberto; Cosentino, Carlo; Amato, Francesco

2015-01-01

This study presents a voxel-based multiple regression analysis of different magnetic resonance image modalities, including anatomical T1-weighted, T2* relaxometry, and diffusion tensor imaging. Quantitative parameters sensitive to complementary brain tissue alterations, including morphometric atrophy, mineralization, microstructural damage, and anisotropy loss, were compared in a linear physiological aging model in 140 healthy subjects (range 20-74 years). The performance of different predictors and the identification of the best biomarker of age-induced structural variation were compared without a priori anatomical knowledge. The best quantitative predictors in several brain regions were iron deposition and microstructural damage, rather than macroscopic tissue atrophy. Age variations were best resolved with a combination of markers, suggesting that multiple predictors better capture age-induced tissue alterations. These findings highlight the importance of a combined evaluation of multimodal biomarkers for the study of aging and point to a number of novel applications for the method described.

Characterization of a Messer – The late-Medieval single-edged sword of Central Europe

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

Fajfar, Peter; Medved, Jožef; Klančnik, Grega

2013-12-15

Metallurgical characterization of a sword blade fragments dating from the second half of the 15th century found in central Slovenia was performed in order to determine its chemical composition, microstructure, microhardness, and to obtain insight into the methods of manufacture of a late-medieval Messer sword. As the artefact was broken, examinations were limited to six very small fragments that were allowed to be removed from the cutting edge, core and the back of the blade. Light optical microscopy, scanning electron microscopy, energy dispersive X-ray spectroscopy, energy dispersive X-ray fluorescence spectrometry, differential scanning calorimetry, thermodynamics approach and Vickers micro-hardness tests weremore » employed to analyze the microstructure and mechanical properties. The results show that the sword was manufactured from a single wrought iron billet. The surface of the sword was carburized. No evidence of quenching was found. The ferritic microstructure is concentrated in the core, and the pearlitic in the outer layer of the blade. All metal fragments contained non-metallic inclusions that were derived mostly from slag and some from hammer scale. - Highlights: • A metallurgical characterization of a medieval sword blade has been performed. • The carbon content decreased from the surface to the core of the blade. • The dominant microstructure in the outer layer is pearlite and in the core is ferrite. • The presence of lump shaped and elongated non-metallic inclusions was observed. • The sword was manufactured from a single wrought iron billet.« less

Microstructural effect on radiative scattering coefficient and asymmetry factor of anisotropic thermal barrier coatings

NASA Astrophysics Data System (ADS)

Chen, X. W.; Zhao, C. Y.; Wang, B. X.

2018-05-01

Thermal barrier coatings are common porous materials coated on the surface of devices operating under high temperatures and designed for heat insulation. This study presents a comprehensive investigation on the microstructural effect on radiative scattering coefficient and asymmetry factor of anisotropic thermal barrier coatings. Based on the quartet structure generation set algorithm, the finite-difference-time-domain method is applied to calculate angular scattering intensity distribution of complicated random microstructure, which takes wave nature into account. Combining Monte Carlo method with Particle Swarm Optimization, asymmetry factor, scattering coefficient and absorption coefficient are retrieved simultaneously. The retrieved radiative properties are identified with the angular scattering intensity distribution under different pore shapes, which takes dependent scattering and anisotropic pore shape into account implicitly. It has been found that microstructure significantly affects the radiative properties in thermal barrier coatings. Compared with spherical shape, irregular anisotropic pore shape reduces the forward scattering peak. The method used in this paper can also be applied to other porous media, which designs a frame work for further quantitative study on porous media.

Small strain multiphase-field model accounting for configurational forces and mechanical jump conditions

NASA Astrophysics Data System (ADS)

Schneider, Daniel; Schoof, Ephraim; Tschukin, Oleg; Reiter, Andreas; Herrmann, Christoph; Schwab, Felix; Selzer, Michael; Nestler, Britta

2018-03-01

Computational models based on the phase-field method have become an essential tool in material science and physics in order to investigate materials with complex microstructures. The models typically operate on a mesoscopic length scale resolving structural changes of the material and provide valuable information about the evolution of microstructures and mechanical property relations. For many interesting and important phenomena, such as martensitic phase transformation, mechanical driving forces play an important role in the evolution of microstructures. In order to investigate such physical processes, an accurate calculation of the stresses and the strain energy in the transition region is indispensable. We recall a multiphase-field elasticity model based on the force balance and the Hadamard jump condition at the interface. We show the quantitative characteristics of the model by comparing the stresses, strains and configurational forces with theoretical predictions in two-phase cases and with results from sharp interface calculations in a multiphase case. As an application, we choose the martensitic phase transformation process in multigrain systems and demonstrate the influence of the local homogenization scheme within the transition regions on the resulting microstructures.

In Situ Synchrotron X-ray Study of Ultrasound Cavitation and Its Effect on Solidification Microstructures

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

Mi, Jiawei; Tan, Dongyue; Lee, Tung Lik

2014-12-11

Considerable progress has been made in studying the mechanism and effectiveness of using ultrasound waves to manipulate the solidification microstructures of metallic alloys. However, uncertainties remain in both the underlying physics of how microstructures evolve under ultrasonic waves, and the best technological approach to control the final microstructures and properties. We used the ultrafast synchrotron X-ray phase contrast imaging facility housed at the Advanced Photon Source, Argonne National Laboratory, US to study in situ the highly transient and dynamic interactions between the liquid metal and ultrasonic waves/bubbles. The dynamics of ultrasonic bubbles in liquid metal and their interactions with themore » solidifying phases in a transparent alloy were captured in situ. The experiments were complemented by the simulations of the acoustic pressure field, the pulsing of the bubbles, and the associated forces acting onto the solidifying dendrites. The study provides more quantitative understanding on how ultrasonic waves/bubbles influence the growth of dendritic grains and promote the grain multiplication effect for grain refinement.« less

Phase transformations in steels: Processing, microstructure, and performance

DOE PAGES

Gibbs, Paul J.

2014-04-03

In this study, contemporary steel research is revealing new processing avenues to tailor microstructure and properties that, until recently, were only imaginable. Much of the technological versatility facilitating this development is provided by the understanding and utilization of the complex phase transformation sequences available in ferrous alloys. Today we have the opportunity to explore the diverse phenomena displayed by steels with specialized analytical and experimental tools. Advances in multi-scale characterization techniques provide a fresh perspective into microstructural relationships at the macro- and micro-scale, enabling a fundamental understanding of the role of phase transformations during processing and subsequent deformation.

Influence of the composite material thermal expansion on embedded highly birefringent polymer microstructured optical fibers

NASA Astrophysics Data System (ADS)

SzelÄ g, M.; Lesiak, P.; Kuczkowski, M.; Domański, A. W.; Woliński, T. R.

2013-05-01

Results of our research on embedded highly birefringent polymer microstructured fibers are presented. A composite material sample with fibers embedded between two layers of a multi-layer composite structure is fabricated and characterized. Temperature sensitivities of the polymer fibers are measured in a free space and compared with the fibers embedded in the composite material. It appeared that highly birefringent polymer microstructured fibers exhibit a strong increase in temperature sensitivity when embedded in the composite material, which is due to the stress-induced changes in birefringence created by thermally-induced strain.

3D geometrical characterization and modelling of solid oxide cells electrodes microstructure by image analysis

NASA Astrophysics Data System (ADS)

Moussaoui, H.; Debayle, J.; Gavet, Y.; Delette, G.; Hubert, M.; Cloetens, P.; Laurencin, J.

2017-03-01

A strong correlation exists between the performance of Solid Oxide Cells (SOCs), working either in fuel cell or electrolysis mode, and their electrodes microstructure. However, the basic relationships between the three-dimensional characteristics of the microstructure and the electrode properties are not still precisely understood. Thus, several studies have been recently proposed in an attempt to improve the knowledge of such relations, which are essential before optimizing the microstructure, and hence, designing more efficient SOC electrodes. In that frame, an original model has been adapted to generate virtual 3D microstructures of typical SOCs electrodes. Both the oxygen electrode, which is made of porous LSCF, and the hydrogen electrodes, made of porous Ni-YSZ, have been studied. In this work, the synthetic microstructures are generated by the so-called 3D Gaussian `Random Field model'. The morphological representativeness of the virtual porous media have been validated on real 3D electrode microstructures of a commercial cell, obtained by X-ray nano-tomography at the European Synchrotron Radiation Facility (ESRF). This validation step includes the comparison of the morphological parameters like the phase covariance function and granulometry as well as the physical parameters like the `apparent tortuosity'. Finally, this validated tool will be used, in forthcoming studies, to identify the optimal microstructure of SOCs.

Advanced Steel Microstructural Classification by Deep Learning Methods.

PubMed

Azimi, Seyed Majid; Britz, Dominik; Engstler, Michael; Fritz, Mario; Mücklich, Frank

2018-02-01

The inner structure of a material is called microstructure. It stores the genesis of a material and determines all its physical and chemical properties. While microstructural characterization is widely spread and well known, the microstructural classification is mostly done manually by human experts, which gives rise to uncertainties due to subjectivity. Since the microstructure could be a combination of different phases or constituents with complex substructures its automatic classification is very challenging and only a few prior studies exist. Prior works focused on designed and engineered features by experts and classified microstructures separately from the feature extraction step. Recently, Deep Learning methods have shown strong performance in vision applications by learning the features from data together with the classification step. In this work, we propose a Deep Learning method for microstructural classification in the examples of certain microstructural constituents of low carbon steel. This novel method employs pixel-wise segmentation via Fully Convolutional Neural Network (FCNN) accompanied by a max-voting scheme. Our system achieves 93.94% classification accuracy, drastically outperforming the state-of-the-art method of 48.89% accuracy. Beyond the strong performance of our method, this line of research offers a more robust and first of all objective way for the difficult task of steel quality appreciation.

Microstructure evolution and tensile properties of Zr-2.5wt%Nb pressure tubes processed from billets with different microstructures

NASA Astrophysics Data System (ADS)

Kapoor, K.; Saratchandran, N.; Muralidharan, K.

1999-02-01

Starting with identical ingots, billets having different microstructures were obtained by three different processing methods for fabrication of Zr-2.5wt%Nb pressure tubes. The billets were further processed by hot extrusion and cold Pilger tube reducing to the finished product. Microstructural characterization was done at each stage of processing. The effects of the initial billet microstructure on the intermediate and final microstructure and mechanical property results were determined. It was found that the structure at each stage and the final mechanical properties depend strongly on the initial billet microstructure. The structure at the final stage consists of elongated alpha zirconium grains with a network of metastable beta zirconium phase. Some of this metastable phase transforms into stable beta niobium during thermomechanical processing. Billets with quenched structure resulted in less beta niobium at the final stage. The air cooled billets resulted in a large amount of beta niobium. The tensile properties, especially the percentage elongation, were found to vary for the different methods. Higher percentage elongation was observed for billets having quenched structure. Extrusion and forging did not produce any characteristic differences in the properties. The results were used to select a process flow sheet which yields the desired mechanical properties with suitable microstructure in the final product.

High cycle fatigue in the transmission electron microscope

DOE PAGES

Bufford, Daniel C.; Stauffer, Douglas; Mook, William M.; ...

2016-06-28

One of the most common causes of structural failure in metals is fatigue induced by cyclic loading. Historically, microstructure-level analysis of fatigue cracks has primarily been performed post mortem. However, such investigations do not directly reveal the internal structural processes at work near micro- and nanoscale fatigue cracks and thus do not provide direct evidence of active microstructural mechanisms. In this paper, the tension–tension fatigue behavior of nanocrystalline Cu was monitored in real time at the nanoscale by utilizing a new capability for quantitative cyclic mechanical loading performed in situ in a transmission electron microscope (TEM). Controllable loads were appliedmore » at frequencies from one to several hundred hertz, enabling accumulations of 10 6 cycles within 1 h. The nanometer-scale spatial resolution of the TEM allows quantitative fatigue crack growth studies at very slow crack growth rates, measured here at ~10 –12 m·cycle –1. This represents an incipient threshold regime that is well below the tensile yield stress and near the minimum conditions for fatigue crack growth. Evidence of localized deformation and grain growth within 150 nm of the crack tip was observed by both standard imaging and precession electron diffraction orientation mapping. Finally, these observations begin to reveal with unprecedented detail the local microstructural processes that govern damage accumulation, crack nucleation, and crack propagation during fatigue loading in nanocrystalline Cu.« less

Relationship Between Solidification Microstructure and Hot Cracking Susceptibility for Continuous Casting of Low-Carbon and High-Strength Low-Alloyed Steels: A Phase-Field Study

NASA Astrophysics Data System (ADS)

Böttger, B.; Apel, M.; Santillana, B.; Eskin, D. G.

2013-08-01

Hot cracking is one of the major defects in continuous casting of steels, frequently limiting the productivity. To understand the factors leading to this defect, microstructure formation is simulated for a low-carbon and two high-strength low-alloyed steels. 2D simulation of the initial stage of solidification is performed in a moving slice of the slab using proprietary multiphase-field software and taking into account all elements which are expected to have a relevant effect on the mechanical properties and structure formation during solidification. To account for the correct thermodynamic and kinetic properties of the multicomponent alloy grades, the simulation software is online coupled to commercial thermodynamic and mobility databases. A moving-frame boundary condition allows traveling through the entire solidification history starting from the slab surface, and tracking the morphology changes during growth of the shell. From the simulation results, significant microstructure differences between the steel grades are quantitatively evaluated and correlated with their hot cracking behavior according to the Rappaz-Drezet-Gremaud (RDG) hot cracking criterion. The possible role of the microalloying elements in hot cracking, in particular of traces of Ti, is analyzed. With the assumption that TiN precipitates trigger coalescence of the primary dendrites, quantitative evaluation of the critical strain rates leads to a full agreement with the observed hot cracking behavior.

Wearable Contact Lens Biosensors for Continuous Glucose Monitoring Using Smartphones.

PubMed

Elsherif, Mohamed; Hassan, Mohammed Umair; Yetisen, Ali K; Butt, Haider

2018-05-17

Low-cost, robust, and reusable continuous glucose monitoring systems that can provide quantitative measurements at point-of-care settings is an unmet medical need. Optical glucose sensors require complex and time-consuming fabrication processes, and their readouts are not practical for quantitative analyses. Here, a wearable contact lens optical sensor was created for the continuous quantification of glucose at physiological conditions, simplifying the fabrication process and facilitating smartphone readouts. A photonic microstructure having a periodicity of 1.6 μm was printed on a glucose-selective hydrogel film functionalized with phenylboronic acid. Upon binding with glucose, the microstructure volume swelled, which modulated the periodicity constant. The resulting change in the Bragg diffraction modulated the space between zero- and first-order spots. A correlation was established between the periodicity constant and glucose concentration within 0-50 mM. The sensitivity of the sensor was 12 nm mM -1 , and the saturation response time was less than 30 min. The sensor was integrated with commercial contact lenses and utilized for continuous glucose monitoring using smartphone camera readouts. The reflected power of the first-order diffraction was measured via a smartphone application and correlated to the glucose concentrations. A short response time of 3 s and a saturation time of 4 min was achieved in the continuous monitoring mode. Glucose-sensitive photonic microstructures may have applications in point-of-care continuous monitoring devices and diagnostics at home settings.

The rheology and microstructure of aging thermoreversible colloidal gels & attractive driven glasses

NASA Astrophysics Data System (ADS)

Wagner, Norman; Gordon, Melissa; Kloxin, Christopher

The properties of colloidal gels and glasses are known to change with age, but the particle-level mechanisms by which aging occurs is are fully understood, which limits our ability to predict macroscopic behavior in these systems. In this work, we quantitatively relate rheological aging to structural aging of a model, homogenous gel and attractive driven glass by simultaneously measuring the bulk properties and gel microstructure using rheometry and small angle neutron scattering (Rheo-SANS), respectively. Specifically, we develop a quantitative and predictive relationship between the macroscopic properties and the underlying microstructure (i . e . , the effective strength of attraction) of an aging colloidal gel and attractive driven glass and study it as a function of the thermal and shear history. Analysis with mode coupling theory is consistent with local particle rearrangements as the mechanism of aging, which lead to monotonically increasing interaction strengths in a continuously evolving material and strongly supports aging as a trajectory in the free energy landscape dominated by local particle relaxations. The analyses and conclusions of this study may be 1) industrially relevant to products that age on commercial timescales, such as paints and pharmaceuticals, 2) applicable to other dynamically arrested systems, such as metallic glasses, and 3) used in the design of new materials. NIST Center for Neutron Research CNS cooperative agreement number #70NANB12H239 and NASA Grant No. NNX15AI19H.

High cycle fatigue in the transmission electron microscope

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

Bufford, Daniel C.; Stauffer, Douglas; Mook, William M.

One of the most common causes of structural failure in metals is fatigue induced by cyclic loading. Historically, microstructure-level analysis of fatigue cracks has primarily been performed post mortem. However, such investigations do not directly reveal the internal structural processes at work near micro- and nanoscale fatigue cracks and thus do not provide direct evidence of active microstructural mechanisms. In this paper, the tension–tension fatigue behavior of nanocrystalline Cu was monitored in real time at the nanoscale by utilizing a new capability for quantitative cyclic mechanical loading performed in situ in a transmission electron microscope (TEM). Controllable loads were appliedmore » at frequencies from one to several hundred hertz, enabling accumulations of 10 6 cycles within 1 h. The nanometer-scale spatial resolution of the TEM allows quantitative fatigue crack growth studies at very slow crack growth rates, measured here at ~10 –12 m·cycle –1. This represents an incipient threshold regime that is well below the tensile yield stress and near the minimum conditions for fatigue crack growth. Evidence of localized deformation and grain growth within 150 nm of the crack tip was observed by both standard imaging and precession electron diffraction orientation mapping. Finally, these observations begin to reveal with unprecedented detail the local microstructural processes that govern damage accumulation, crack nucleation, and crack propagation during fatigue loading in nanocrystalline Cu.« less

Matrix remodeling between cells and cellular interactions with collagen bundle

NASA Astrophysics Data System (ADS)

Kim, Jihan; Sun, Bo

When cells are surrounded by complex environment, they continuously probe and interact with it by applying cellular traction forces. As cells apply traction forces, they can sense rigidity of their local environment and remodel the matrix microstructure simultaneously. Previous study shows that single human carcinoma cell (MDA-MB-231) remodeled its surrounding extracellular matrix (ECM) and the matrix remodeling was reversible. In this study we examined the matrix microstructure between cells and cellular interaction between them using quantitative confocal microscopy. The result shows that the matrix microstructure is the most significantly remodeled between cells consisting of aligned, and densified collagen fibers (collagen bundle)., the result shows that collagen bundle is irreversible and significantly change micromechanics of ECM around the bundle. We further examined cellular interaction with collagen bundle by analyzing dynamics of actin and talin formation along with the direction of bundle. Lastly, we analyzed dynamics of cellular protrusion and migrating direction of cells along the bundle.

Textural analysis of optical coherence tomography skin images: quantitative differentiation between healthy and cancerous tissues

NASA Astrophysics Data System (ADS)

Adabi, Saba; Conforto, Silvia; Hosseinzadeh, Matin; Noe, Shahryar; Daveluy, Steven; Mehregan, Darius; Nasiriavanaki, Mohammadreza

2017-02-01

Optical Coherence Tomography (OCT) offers real-time high-resolution three-dimensional images of tissue microstructures. In this study, we used OCT skin images acquired from ten volunteers, neither of whom had any skin conditions addressing the features of their anatomic location. OCT segmented images are analyzed based on their optical properties (attenuation coefficient) and textural image features e.g., contrast, correlation, homogeneity, energy, entropy, etc. Utilizing the information and referring to their clinical insight, we aim to make a comprehensive computational model for the healthy skin. The derived parameters represent the OCT microstructural morphology and might provide biological information for generating an atlas of normal skin from different anatomic sites of human skin and may allow for identification of cell microstructural changes in cancer patients. We then compared the parameters of healthy samples with those of abnormal skin and classified them using a linear Support Vector Machines (SVM) with 82% accuracy.

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

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

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

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

Microfluidic droplet trapping array as nanoliter reactors for gas-liquid chemical reaction.

PubMed

Zhang, Qingquan; Zeng, Shaojiang; Qin, Jianhua; Lin, Bingcheng

2009-09-01

This article presents a simple method for trapping arrays of droplets relying on the designed microstructures of the microfluidic device, and this has been successfully used for parallel gas-liquid chemical reaction. In this approach, the trapping structure is composed of main channel, lateral channel and trapping region. Under a negative pressure, array droplets can be generated and trapped in the microstructure simultaneously, without the use of surfactant and the precise control of the flow velocity. By using a multi-layer microdevice containing the microstructures, single (pH gradient) and multiple gas-liquid reactions (metal ion-NH3 complex reaction) can be performed in array droplets through the transmembrane diffusion of the gas. The droplets with quantitative concentration gradient can be formed by only replacing the specific membrane. The established method is simple, robust and easy to operate, demonstrating the potential of this device for droplet-based high-throughput screening.

Specific features of direct formation of graphite-like microstructures in polycarbonate samples by single femtosecond laser pulses

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

Ganin, D V; Lapshin, K E; Obidin, A Z

2015-11-30

We present the result of the experiments on producing graphite-like cylindrical microstructures by focusing single femtosecond laser pulses into the bulk of a transparent polymer (polycarbonate). The microstructures are embedded in a cladding with a modified refractive index, possessing waveguide properties. In the experiments with nontransparent screens and diaphragms, placed in the laser beam in front of the entrance pupil of the objective with a large numerical aperture, we have found that the paraxial rays are blocked by the peripheral ones, which reduces the length of the destruction region in the pre-focal zone. In the experiments with transparent screens andmore » diaphragms, introducing optical delays τ{sub d} between the paraxial and peripheral rays, the quantitative dependence of the destruction region length in the pre-focal zone on the value of τ{sub d} is determined. (interaction of laser radiation with matter. laser plasma)« less

Experimental and Numerical Analysis of Microstructures and Stress States of Shot-Peened GH4169 Superalloys

NASA Astrophysics Data System (ADS)

Hu, Dianyin; Gao, Ye; Meng, Fanchao; Song, Jun; Wang, Rongqiao

2018-04-01

Combining experiments and finite element analysis (FEA), a systematic study was performed to analyze the microstructural evolution and stress states of shot-peened GH4169 superalloy over a variety of peening intensities and coverages. A dislocation density evolution model was integrated into the representative volume FEA model to quantitatively predict microstructural evolution in the surface layers and compared with experimental results. It was found that surface roughness and through-depth residual stress profile are more sensitive to shot-peening intensity compared to coverage due to the high kinetic energy involved. Moreover, a surface nanocrystallization layer was discovered in the top surface region of GH4169 for all shot-peening conditions. However, the grain refinement was more intensified under high shot-peening coverage, under which enough time was permitted for grain refinement. The grain size gradient predicted by the numerical framework showed good agreement with experimental observations.

The development and characterization of stimuli-responsive systems for performance materials

NASA Astrophysics Data System (ADS)

Gordon, Melissa B.

In nature, living organisms adjust to their surroundings by responding to environmental cues, such as light, temperature or force. Stimuli-triggered processes, such as the contraction of eyes in response to bright light or wound healing in skin after a cut, motivate the design of "smart" materials which are designed to respond to environmental stimuli. Responsive materials are used as self-healing materials, shape memory polymers and responsive coatings; moreover, responsive materials may also be employed as model systems, which enhance understanding of complex behavior. The overall goal of this work is to design a material that offers self-healing functionality, which will allow for self-repair following material fatigue or failure, and increased strength in response to ballistic or puncture threats through the incorporation of colloidal particles. The target application for this material is as a protective barrier in extreme environments, such as outer space. Towards this end, the dissertation is focused on the development and characterization of each component of the protective material by (1) designing and testing novel light- and force-sensitive polymers for self-healing applications and (2) examining and characterizing long-time behavior (i.e., aging) in model thermoreversible colloidal gels and glasses. Towards the development of novel stimuli-responsive materials, a photo-responsive polymer network is developed in which a dynamic bond is incorporated into the network architecture to enable a light-triggered, secondary polymerization, which increases the modulus by two orders of magnitude while strengthening the network by over 100%. Unlike traditional two-stage polymerization systems, in which the secondary polymerization is triggered by a leachable photoinitiator, the dynamic nature is imparted by the material itself via the dissociation of its own crosslinks to become stronger in response to light. Several attributes of the photo-responsive network are shown including: (1) photo-induced healing and strengthening of a specimen after it has been severed, (2) photopatterning for effecting spatially confined property changes on demand, and (3) locking in the film's 3D geometry using light after reshaping. The utility of the photo-responsive dynamic bond is enhanced by demonstrating that it is also responsive to mechanical force. Force-responsive materials are activated by the energy from the damage event itself, thereby enabling healing without human intervention. Specifically, selective cleavage of a polymer containing a dynamic trithiocarbonate group initiates a force-driven radical polymerization, thus enabling the material to constructively respond to force via gelation on an experimentally relevant timescale. To enhance the stress response of the self-healing materials described above, a protective material composed of colloidal particles is proposed. Toward this goal, the second half of this dissertation investigates the microstructural basis of rheological aging in colloidal gels and glasses using a model thermoreversible colloidal dispersion. In this work, rheological aging is quantitatively related to microstructural aging in glasses and gels by simultaneously measuring the bulk properties and sample microstructure using rheometry and small angle neutron scattering (Rheo-SANS), respectively. A one-to-one correspondence between the evolution in storage modulus and microstructure as the sample ages is observed, which is investigated as a function of thermal and shear history. The microstructural measurements are consistent with the hypothesis of aging as a trajectory in a free energy landscape, which combined with analysis with mode coupling theory, support local particle rearrangements as the mechanism of aging. Moreover, by using a system that is fully rejuvenated by thermal cycling, the effectiveness of shear as a rejuvenation method is investigated by directly comparing microstructure and bulk properties following thermal and mechanical rejuvenation. The conclusions of this study may be industrially relevant to products that age on commercial timescales, such as pharmaceuticals, applicable to other dynamically arrested systems, such as metallic glasses, and provide pathways to advanced composite materials such as those envisioned in this work.

Discussion on Microwave-Matter Interaction Mechanisms by In Situ Observation of "Core-Shell" Microstructure during Microwave Sintering.

PubMed

Liu, Wenchao; Xu, Feng; Li, Yongcun; Hu, Xiaofang; Dong, Bo; Xiao, Yu

2016-02-23

This research aims to deepen the understanding of the interaction mechanisms between microwave and matter in a metal-ceramic system based on in situ synchrotron radiation computed tomography. A special internal "core-shell" microstructure was discovered for the first time and used as an indicator for the interaction mechanisms between microwave and matter. Firstly, it was proved that the microwave magnetic field acted on metal particles by way of inducing an eddy current in the surface of the metal particles, which led to the formation of a "core-shell" microstructure in the metal particles. On this basis, it was proposed that the ceramic particles could change the microwave field and open a way for the microwave, thereby leading to selective heating in the region around the ceramic particles, which was verified by the fact that all the "core-shell" microstructure was located around ceramic particles. Furthermore, it was indicated that the ceramic particles would gather the microwaves, and might lead to local heating in the metal-ceramic contact region. The focusing of the microwave was proved by the quantitative analysis of the evolution rate of the "core-shell" microstructure in a different region. This study will help to reveal the microwave-matter interaction mechanisms during microwave sintering.

Miniaturization of Fresnel lenses for solar concentration: a quantitative investigation.

PubMed

Duerr, Fabian; Meuret, Youri; Thienpont, Hugo

2010-04-20

Sizing down the dimensions of solar concentrators for photovoltaic applications offers a number of promising advantages. It provides thinner modules and smaller solar cells, which reduces thermal issues. In this work a plane Fresnel lens design is introduced that is first analyzed with geometrical optics. Because of miniaturization, pure ray tracing may no longer be valid to determine the concentration performance. Therefore, a quantitative wave optical analysis of the miniaturization's influence on the obtained concentration performance is presented. This better quantitative understanding of the impact of diffraction in microstructured Fresnel lenses might help to optimize the design of several applications in nonimaging optics.

Effect of Ar9+ irradiation on Zr-1Nb-1Sn-0.1Fe alloy characterized by Grazing Incidence X-ray diffraction technique

NASA Astrophysics Data System (ADS)

Dutta, Argha; Das, Kalipada; Gayathri, N.; Menon, Ranjini; Nabhiraj, P. Y.; Mukherjee, Paramita

2018-03-01

The microstructural parameters such as domain size and microstrain have been estimated from Grazing Incidence X-ray Diffraction (GIXRD) data for Ar9+ irradiated Zr-1Nb-1Sn-0.1Fe sample as a function of dpa (dose). Detail studies using X-ray Diffraction Line Profile Analysis (XRDLPA) from GIXRD data has been carried out to characterize the microstructural parameters like domain size and microstrain. The reorientation of the grains due to effect of irradiation at high dpa (dose) has been qualitatively assessed by the texture parameter P(hkl).

From Powders to Dense Metal Parts: Characterization of a Commercial AlSiMg Alloy Processed through Direct Metal Laser Sintering

PubMed Central

Manfredi, Diego; Calignano, Flaviana; Krishnan, Manickavasagam; Canali, Riccardo; Ambrosio, Elisa Paola; Atzeni, Eleonora

2013-01-01

In this paper, a characterization of an AlSiMg alloy processed by direct metal laser sintering (DMLS) is presented, from the analysis of the starting powders, in terms of size, morphology and chemical composition, through to the evaluation of mechanical and microstructural properties of specimens built along different orientations parallel and perpendicular to the powder deposition plane. With respect to a similar aluminum alloy as-fabricated, a higher yield strength of about 40% due to the very fine microstructure, closely related to the mechanisms involved in this additive process is observed. PMID:28809344

From Powders to Dense Metal Parts: Characterization of a Commercial AlSiMg Alloy Processed through Direct Metal Laser Sintering.

PubMed

Manfredi, Diego; Calignano, Flaviana; Krishnan, Manickavasagam; Canali, Riccardo; Ambrosio, Elisa Paola; Atzeni, Eleonora

2013-03-06

In this paper, a characterization of an AlSiMg alloy processed by direct metal laser sintering (DMLS) is presented, from the analysis of the starting powders, in terms of size, morphology and chemical composition, through to the evaluation of mechanical and microstructural properties of specimens built along different orientations parallel and perpendicular to the powder deposition plane. With respect to a similar aluminum alloy as-fabricated, a higher yield strength of about 40% due to the very fine microstructure, closely related to the mechanisms involved in this additive process is observed.

MaRIE: Probing Dynamic Processes in Soft Materials Using Advanced Light Sources

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

Sykora, Milan; Kober, Edward Martin

Los Alamos National Laboratory has developed a concept for a new research facility, MaRIE: Matter-Radiation Interactions in Extremes. The key motivation for MaRIE is to develop new experimental capabilities needed to fill the existing gaps in our fundamental understanding of materials important for key National Nuclear Security Agency (NNSA) goals. MaRIE will bring two major new capabilities: (a) the ability to characterize the meso- and microstructure of materials in bulk as well as local dynamic response characteristics, and (b) the ability to characterize how this microstructure evolves under NNSA-relevant conditions and impacts the material’s performance in this regime.

Transmission electron microscopy characterization of microstructural features of Al-Li-Cu alloys

NASA Technical Reports Server (NTRS)

Avalos-Borja, M.; Pizzo, P. P.; Larson, L. A.

1983-01-01

A transmission electron microscopy (TEM) examination of aluminum-lithium-copper alloys was conducted. The principal purpose is to characterize the nature, size, and distribution of stringer particles which result from the powder metallurgy (P/M) processing of these alloys. Microstructural features associated with the stringer particles are reported that help explain the stress corrosion susceptibility of the powder metallurgy-processed Al-Li-Cu alloys. In addition, matrix precipitation events are documented for a variety of heat treatments and process variations. Hot rolling is observed to significant alter the nature of matrix precipitation, and the observations are correlated with concomitant mechanical property variations.

Topograph for inspection of engine cylinder walls.

PubMed

Franz, S; Leonhardt, K; Windecker, R; Tiziani, H J

1999-12-20

The microstructural inspection of engine cylinder walls is an important task for quality management in the automotive industry. Until recently, mainly tactile methods were used for this purpose. We present an optical instrument based on microscopic fringe projection that permits fast, reliable, and nondestructive measurements of microstructure. The field of view is 0.8 mm x 1.2 mm, with a spatial sampling of 1100 x 700 pixels. In contrast to conventional tactile sensors, the optical method provides fast in situ three-dimensional surface characterizations that provide more information about the surface than do line profiles. Measurements are presented, and advantages of this instrument for characterization of a surface are discussed.

Transmission electron microscopy characterization of microstructural features in aluminum-lithium-copper alloys

NASA Technical Reports Server (NTRS)

Avalos-Borja, M.; Larson, L. A.; Pizzo, P. P.

1984-01-01

A transmission electron microscopy (TEM) examination of aluminum-lithium-copper alloys was conducted. The principal purpose is to characterize the nature, size, and distribution of stringer particles which result from the powder metallurgy (P/M) processing of these alloys. Microstructural features associated with the stringer particles are reported that help explain the stress corrosion susceptibility of the powder metallurgy-processed Al-Li-Cu alloys. In addition, matrix precipitaton events are documented for a variety of heat treatments and process variations. Hot rolling is observed to significantly alter the nature of matrix precipitation, and the observations are correlated with concomitant mechanical property variations.

Micromechanical Characterization and Texture Analysis of Direct Cast Titanium Alloys Strips

NASA Technical Reports Server (NTRS)

2000-01-01

This research was conducted to determine a post-processing technique to optimize mechanical and material properties of a number of Titanium based alloys and aluminides processed via Melt Overflow Solidification Technique (MORST). This technique was developed by NASA for the development of thin sheet titanium and titanium aluminides used in high temperature applications. The materials investigated in this study included conventional titanium alloy strips and foils, Ti-1100, Ti-24Al-11Nb (Alpha-2), and Ti-48Al-2Ta (Gamma). The methodology used included micro-characterization, heat-treatment, mechanical processing and mechanical testing. Characterization techniques included optical, electron microscopy, and x-ray texture analysis. The processing included heat-treatment and mechanical deformation through cold rolling. The initial as-cast materials were evaluated for their microstructure and mechanical properties. Different heat-treatment and rolling steps were chosen to process these materials. The properties were evaluated further and a processing relationship was established in order to obtain an optimum processing condition. The results showed that the as-cast material exhibited a Widmanstatten (fine grain) microstructure that developed into a microstructure with larger grains through processing steps. The texture intensity showed little change for all processing performed in this investigation.

Fabrication and thermophysical property characterization of UN/U 3Si 2 composite fuel forms

DOE PAGES

White, Joshua Taylor; Travis, Austin William; Dunwoody, John Tyler; ...

2017-09-21

High uranium density composite fuels composed of UN and U 3Si 2 have been fabricated using a liquid phase sintering route at temperatures between 1873 K and 1973 K and spanning compositions of 10 vol% to 40 vol% U 3Si 2. Microstructural analysis and phase characterization revealed the formation of an U-Si-N phase of unknown structure. Microcracking was observed in the U-Si portion of the composite microstructure that likely originates from the mismatched coefficient of thermal expansion between the UN and U 3Si 2 leading to stresses on heating and cooling of the composite. Thermal expansion coefficient, thermal diffusivity, andmore » thermal conductivity were characterized for each of the compositions as a function of temperature to 1673 K. Hysteresis is observed in the thermal diffusivity for the 20 vol% through 40 vol% specimens between room temperature and 1273 K, which is attributed to the microcracking in the U-Si phase. Thermal conductivity of the composites was modeled using the MOOSE framework based on the collected microstructure data. In conclusion, the impact of irradiation on thermal conductivity was also simulated for this class of composite materials.« less

Fabrication and thermophysical property characterization of UN/U 3Si 2 composite fuel forms

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

White, Joshua Taylor; Travis, Austin William; Dunwoody, John Tyler

High uranium density composite fuels composed of UN and U 3Si 2 have been fabricated using a liquid phase sintering route at temperatures between 1873 K and 1973 K and spanning compositions of 10 vol% to 40 vol% U 3Si 2. Microstructural analysis and phase characterization revealed the formation of an U-Si-N phase of unknown structure. Microcracking was observed in the U-Si portion of the composite microstructure that likely originates from the mismatched coefficient of thermal expansion between the UN and U 3Si 2 leading to stresses on heating and cooling of the composite. Thermal expansion coefficient, thermal diffusivity, andmore » thermal conductivity were characterized for each of the compositions as a function of temperature to 1673 K. Hysteresis is observed in the thermal diffusivity for the 20 vol% through 40 vol% specimens between room temperature and 1273 K, which is attributed to the microcracking in the U-Si phase. Thermal conductivity of the composites was modeled using the MOOSE framework based on the collected microstructure data. In conclusion, the impact of irradiation on thermal conductivity was also simulated for this class of composite materials.« less

A Study of Drop-Microstructured Surface Interactions during Dropwise Condensation with Quartz Crystal Microbalance

PubMed Central

Su, Junwei; Charmchi, Majid; Sun, Hongwei

2016-01-01

Dropwise condensation (DWC) on hydrophobic surfaces is attracting attention for its great potential in many industrial applications, such as steam power plants, water desalination, and de-icing of aerodynamic surfaces, to list a few. The direct dynamic characterization of liquid/solid interaction can significantly accelerate the progress toward a full understanding of the thermal and mass transport mechanisms during DWC processes. This work reports a novel Quartz Crystal Microbalance (QCM) based method that can quantitatively analyze the interaction between water droplets and micropillar surfaces during different condensation states such as filmwise, Wenzel, and partial Cassie states. A combined nanoimprinting lithography and chemical surface treatment approach was utilized to fabricate the micropillar based superhydrophobic and superhydrophilic surfaces on the QCM substrates. The normalized frequency shift of the QCM device together with the microscopic observation of the corresponding drop motion revealed the droplets growth and their coalescence processes and clearly demonstrated the differences between the three aforementioned condensation states. In addition, the transition between Cassie and Wenzel states was successfully captured by this method. The newly developed QCM system provides a valuable tool for the dynamic characterization of different condensation processes. PMID:27739452

The growth of metastable peritectic compounds

NASA Technical Reports Server (NTRS)

Larson, D. J., Jr.; Pirich, R. G.

1981-01-01

The influence of gravitationally driven thermosolutal convection on the directional solidification of peritectic alloys is considered as well as the relationships between the solidification processing conditions, and the microstructure, chemistry, and magnetic properties of such alloys. Analysis of directionally solidified Pb-Bi peritectic samples indicates that appreciable macrosegregation occurs due to thermosolutal convection and/or Soret diffusion. A peritectic solidification model which accounts for partial mixing in the liquid ahead of the planar solidification interface and describes macrosegregation has been developed. Two-phase dendritic and banded microstructures were grown in the Pb-Bi peritectic system, refined two-phase microstructures have were observed, and candidate formation mechanisms proposed. Material handling, containment, casting, microstructural and magnetic characterization techniques were developed for the Sm-Co system. Alloys produced with these procedures are homogeneous.

Long-term aging of Ag/a-C:H:O nanocomposite coatings in air and in aqueous environment

NASA Astrophysics Data System (ADS)

Drábik, Martin; Pešička, Josef; Biederman, Hynek; Hegemann, Dirk

2015-04-01

Nanocomposite coatings of silver particles embedded in a plasma polymer matrix possess interesting properties depending on their microstructure. The film microstructure is affected among others also by the RF power supplied during the deposition, as shown by transmission electron microscopy. The optical properties are characterized by UV-vis-NIR spectroscopy. An anomalous optical absorption peak from the Ag nanoparticles is observed and related to the microstructure of the nanocomposite films. Furthermore, a long-term aging of the coatings is studied in-depth in ambient air and in aqueous environments. It is shown that the studied films are not entirely stable. The deposition conditions and the microstructure of the films affect the processes taking place during their aging in both environments.

High strength, high ductility low carbon steel

DOEpatents

Koo, Jayoung; Thomas, Gareth

1978-01-01

A high strength, high ductility low carbon steel consisting essentially of iron, 0.05-0.15 wt% carbon, and 1-3 wt% silicon. Minor amounts of other constituents may be present. The steel is characterized by a duplex ferrite-martensite microstructure in a fibrous morphology. The microstructure is developed by heat treatment consisting of initial austenitizing treatment followed by annealing in the (.alpha. + .gamma.) range with intermediate quenching.

Microstructural processes in irradiated materials

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

Byun, Thak Sang; Morgan, Dane; Jiao, Zhijie

2016-04-01

This is an editorial article (preface) for the publication of symposium papers in the Journal of Nuclear materials: These proceedings contain the papers presented at two symposia, the Microstructural Processes in Irradiated Materials (MPIM) and Characterization of Nuclear Reactor Materials and Components with Neutron and Synchrotron Radiation, held in the TMS 2015, 144th Annual Meeting & Exhibition at Walt Disney World, Orlando, Florida, USA on March 15–19, 2015.

Complex dark-field contrast and its retrieval in x-ray phase contrast imaging implemented with Talbot interferometry.

PubMed

Yang, Yi; Tang, Xiangyang

2014-10-01

Under the existing theoretical framework of x-ray phase contrast imaging methods implemented with Talbot interferometry, the dark-field contrast refers to the reduction in interference fringe visibility due to small-angle x-ray scattering of the subpixel microstructures of an object to be imaged. This study investigates how an object's subpixel microstructures can also affect the phase of the intensity oscillations. Instead of assuming that the object's subpixel microstructures distribute in space randomly, the authors' theoretical derivation starts by assuming that an object's attenuation projection and phase shift vary at a characteristic size that is not smaller than the period of analyzer grating G₂ and a characteristic length dc. Based on the paraxial Fresnel-Kirchhoff theory, the analytic formulae to characterize the zeroth- and first-order Fourier coefficients of the x-ray irradiance recorded at each detector cell are derived. Then the concept of complex dark-field contrast is introduced to quantify the influence of the object's microstructures on both the interference fringe visibility and the phase of intensity oscillations. A method based on the phase-attenuation duality that holds for soft tissues and high x-ray energies is proposed to retrieve the imaginary part of the complex dark-field contrast for imaging. Through computer simulation study with a specially designed numerical phantom, they evaluate and validate the derived analytic formulae and the proposed retrieval method. Both theoretical analysis and computer simulation study show that the effect of an object's subpixel microstructures on x-ray phase contrast imaging method implemented with Talbot interferometry can be fully characterized by a complex dark-field contrast. The imaginary part of complex dark-field contrast quantifies the influence of the object's subpixel microstructures on the phase of intensity oscillations. Furthermore, at relatively high energies, for soft tissues it can be retrieved for imaging with a method based on the phase-attenuation duality. The analytic formulae derived in this work to characterize the complex dark-field contrast in x-ray phase contrast imaging method implemented with Talbot interferometry are of significance, which may initiate more activities in the research and development of x-ray differential phase contrast imaging for extensive biomedical applications.

Correlation of microstructure and thermo-mechanical properties of a novel hydrogen transport membrane

NASA Astrophysics Data System (ADS)

Zhang, Yongjun

A key part of the FutureGen concept is to support the production of hydrogen to fuel a "hydrogen economy," with the use of clean burning hydrogen in power-producing fuel cells, as well as for use as a transportation fuel. One of the key technical barriers to FutureGen deployment is reliable and efficient hydrogen separation technology. Most Hydrogen Transport Membrane (HTM) research currently focuses on separation technology and hydrogen flux characterization. No significant work has been performed on thermo-mechanical properties of HTMs. The objective of the thesis is to understand the structure-property correlation of HTM and to characterize (1) thermo mechanical properties under different reducing environments and thermal cycles (thermal shock), and (2) evaluate the stability of the novel HTM material. A novel HTM cermet bulk sample was characterized for its physical and mechanical properties at both room temperature and at elevated temperature up to 1000°C. Micro-structural properties and residual stresses were evaluated in order to understand the changing mechanism of the microstructure and its effects on the mechanical properties of materials. A correlation of the microstructural and thermo mechanical properties of the HTM system was established for both HTM and the substrate material. Mechanical properties of both selected structural ceramics and the novel HTM cermet bulk sample are affected mainly by porosity and microstructural features, such as grain size and pore size-distribution. The Young's Modulus (E-value) is positively correlated to the flexural strength for materials with similar crystallographic structure. However, for different crystallographic materials, physical properties are independent of mechanical properties. Microstructural properties, particularly, grain size and crystallographic structure, and thermodynamic properties are the main factors affecting the mechanical properties at both room and high temperatures. The HTM cermet behaves more like an elastic material at room temperature and as a ductile material at temperature above 850°C. The oxidation and the plasticity of Pd phase mainly affected the mechanical properties of HTM cermet at high temperature, also as a result of thermal cycling. Residual stress induced in the HTM by thermo cycles also plays a very critical role in defining the thermo-mechanical properties.

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

PubMed

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

2004-03-01

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

Microstructural analysis of the 2195 aluminum-lithium alloy welds

NASA Technical Reports Server (NTRS)

Talia, George E.

1993-01-01

The principal objective of this research was to explain a tendency of 2195 Al-Li alloy to crack at elevated temperature during welding. Therefore, a study was made on the effect of welding and thermal treatment on the microstructure of Al-Li Alloy 2195. The critical roles of precipitates, boundaries, phases, and other features of the microstructure were inferred from the crack propagation paths and the morphology of fracture surface of the alloy with different microstructures. Particular emphasis was placed on the microstructures generated by the welding process and the mechanisms of crack propagation in such structures. Variation of the welding parameters and thermal treatments were used to alter the micro/macro structures, and they were characterized by optical and scanning electron microscopy. A theoretical model is proposed to explain changes in the microstructure of welded material. This model proposes a chemical reaction in which gases from the air (i.e., nitrogen) release hydrogen inside the alloy. Such a reaction could generate large internal stresses capable to induce porosity and crack-like delamination in the material.

Relating microstructure to rheology of a bundled and cross-linked F-actin network in vitro

NASA Astrophysics Data System (ADS)

Shin, J. H.; Gardel, M. L.; Mahadevan, L.; Matsudaira, P.; Weitz, D. A.

2004-06-01

The organization of individual actin filaments into higher-order structures is controlled by actin-binding proteins (ABPs). Although the biological significance of the ABPs is well documented, little is known about how bundling and cross-linking quantitatively affect the microstructure and mechanical properties of actin networks. Here we quantify the effect of the ABP scruin on actin networks by using imaging techniques, cosedimentation assays, multiparticle tracking, and bulk rheology. We show how the structure of the actin network is modified as the scruin concentration is varied, and we correlate these structural changes to variations in the resultant network elasticity.

Supercooling effects in faceted eutectic Nb-Si alloys

NASA Technical Reports Server (NTRS)

Gokhale, A. B.; Sarkar, G.; Abbaschian, G. J.; Haygarth, J. C.; Wojcik, C.

1988-01-01

The effect of melt supercooling on the microstructure of an Nb-58 at. pct Si alloy is investigated experimentally using an electromagnetic levitation apparatus. It is found that, starting with an alloy nominally of eutectic composition, nucleation of Nb5Si3 occurs in the supercooled liquid first. Upon further cooling, the remaining liquid continues to supercool until the second phase, NbSi2 is nucleated, which is commonly accompanied by rapid recalescence. The primary phase exibits a eutectoid-type decomposition. The observations are discussed with reference to the results of quantitative microstructural measurements, compositional and thermal analysis, and preliminary thermodynamic modeling of the phase diagram.

Defects-tolerant Co-Cr-Mo dental alloys prepared by selective laser melting.

PubMed

Qian, B; Saeidi, K; Kvetková, L; Lofaj, F; Xiao, C; Shen, Z

2015-12-01

CrCoMo alloy specimens were successfully fabricated using selective laser melting (SLM). The aim of this study was to carefully investigate microstructure of the SLM specimens in order to understand the influence of their structural features inter-grown on different length scales ranging from nano- to macro-levels on their mechanical properties. Two different sets of processing parameters developed for building the inner part (core) and the surface (skin) of dental prostheses were tested. Microstructures were characterized by SEM, EBSD and XRD analysis. The elemental distribution was assessed by EDS line profile analysis under TEM. The mechanical properties of the specimens were measured. The microstructures of both specimens were characterized showing formation of grains comprised of columnar sub-grains with Mo-enrichment at the sub-grain boundaries. Clusters of columnar sub-grains grew coherently along one common crystallographic direction forming much larger single crystal grains which are intercrossing in different directions forming an overall dendrite-like microstructure. Three types of microstructural defects were occasionally observed; small voids (<10 μm), fine cracks at grain boundaries (<10 μm) and cracks at weld line boundaries (>10 μm). Despite the presence of these defects, the yield and the ultimate tensile strength (UTS) were 870 and 430MPa and 1300MPa and 1160MPa, respectively, for the skin and core specimens which are higher than casted dental alloy. Although the formation of microstructural defects is hard to be avoided during the SLM process, the SLM CoCrMo alloys can achieve improved mechanical properties than their casted counterparts, implying they are "defect-tolerant". Copyright © 2015 Academy of Dental Materials. Published by Elsevier Ltd. All rights reserved.

Microstructural investigation of vintage pipeline steels highly susceptible to stress corrosion cracking

NASA Astrophysics Data System (ADS)

Torres, Monica

The use of pipelines for the transmission of gas offers not only efficiency, but a number of economic advantages. Nevertheless, pipelines are subject to aggressive operating conditions and environments which can lead to in-service degradation [1] and thus to failures. These failures can have catastrophic consequences, such as environmental damage and loss of life [2]. One of the most dangerous threats to pipeline integrity is stress corrosion cracking (SCC). Despite the substantial progress that has been achieved in the field, due to the complex nature of this phenomenon there is still not a complete understanding of this form of external corrosion. This makes its detection and prevention a challenge and therefore a risk to pipeline integrity, and most importantly, to the safety of the population. SCC cracks are the result of the interaction between a corrosive environment, applied stresses, and a susceptible microstructure. To date, what defines a susceptible microstructure remains ambiguous, as SCC has been observed in a range of steel grades, microstructures, chemical composition, and grain sizes. Therefore, in order to be able to accurately predict and prevent this hazardous form of corrosion, it is imperative to advance our knowledge on the subject and gain a better understanding on the microstructural features of highly susceptible pipeline materials, especially in the subsurface zone where crack nucleation must take place. Therefore, a microstructural characterization of the region near the surface layer was carried-out utilizing TEM. TEM analysis revealed the dislocation character, ferrite morphology, and apparent carbide precipitation in some grain boundaries. Furthermore, light microscopy, SEM, and hardness testing were performed to expand our knowledge on the microscopical features of highly SCC susceptible service components. This investigation presents a new approach to SCC characterization, which exposed the sub-surface region microscopical characteristics of service components with confirmed SCC.

Effects of Irradiation on the Microstructure of U-7Mo Dispersion Fuel with Al-2Si Matrix

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

Dennis D. Keiser, Jr.; Jan-Fong Jue; Adam B. Robinson

2012-06-01

The Reduced Enrichment for Research and Test Reactor program is developing low-enriched uranium U-Mo dispersion fuels for application in research and test reactors around the world. As part of this development, fuel plates have been irradiated in the Advanced Test Reactor and then characterized using optical metallography (OM) and scanning electron microscopy (SEM) to determine the as-irradiated microstructure. To demonstrate the irradiation performance of U-7Mo dispersion fuel plates with 2 wt% Si added to the matrix, fuel plates were tested to medium burnups at intermediate fission rates as part of the RERTR-6 experiment. Further testing was performed to higher fissionmore » rates as part of the RERTR-7A experiment, and very aggressive testing (high temperature, high fission density, high fission rate) was performed in the RERTR-9A, RERTR-9B and AFIP-1 experiments. As-irradiated microstructures were compared to those observed after fabrication to determine the effects of irradiation on the microstructure. Based on comparison of the microstructural characterization results for each irradiated sample, some general conclusions can be drawn about how the microstructure evolves during irradiation: there is growth of the fuel/matrix interaction layer (FMI), which was present in the samples to some degree after fabrication, during irradiation; Si diffuses from the FMI layer to deeper depths in the U-7Mo particles as the irradiation conditions are made more aggressive; lowering of the Si content in the FMI layer results in an increase in the size of the fission gas bubbles; as the FMI layer grows during irradiation more Si diffuses from the matrix to the FMI layer/matrix interface, and interlinking of fission gas bubbles in the fuel plate microstructure that may indicate breakaway swelling is not observed.« less

Evolution of microstructure, texture and inhibitor along the processing route for grain-oriented electrical steels using strip casting

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

Liu, Hai-Tao, E-mail: liuht@ral.neu.edu.cn; Institute of Research of Iron and Steel, Shasteel, Zhangjiagang 215625, Jiangsu; Yao, Sheng-Jie

2015-08-15

In the present work, a regular grade GO sheet was produced successively by strip casting, hot rolling, normalizing annealing, two-stage cold rolling with intermediate annealing, primary recrystallization annealing, secondary recrystallization annealing and purification. The aim of this paper was to characterize the evolution of microstructure, texture and inhibitor along the new processing route by comprehensive utilization of optical microscopy, X-ray diffraction and transmission electron microscopy. It was found that a fine microstructure with the ferrite grain size range of 7–12 μm could be obtained in the primary recrystallization annealed sheet though a very coarse microstructure was produced in the initialmore » as-cast strip. The main finding was that the “texture memory” effect on Goss texture started on the through-thickness intermediate annealed strip after first cold rolling, which was not similar to the “texture memory” effect on Goss texture starting on the surface layers of the hot rolled strip in the conventional production route. As a result, the origin of Goss nuclei capable of secondary recrystallization lied in the grains already presented in Goss orientation in the intermediate annealed strip after first cold rolling. Another finding was that fine and dispersive inhibitors (mainly AlN) were easy to be produced in the primary recrystallization microstructure due to the initial rapid solidification during strip casting and the subsequent rapid cooling, and the very high temperature reheating usually used before hot rolling in the conventional production route could be avoided. - Highlights: • A regular grade grain-oriented electrical steel was produced. • Evolution of microstructure, texture and inhibitor was characterized. • Origin of Goss nuclei lied in the intermediate annealed strip. • A fine primary recrystallization microstructure could be produced. • Effective inhibitors were easy to be obtained in the new processing route.« less

Characterization of aging-induced microstructural changes in M250 maraging steel using magnetic parameters

NASA Astrophysics Data System (ADS)

Rajkumar, K. V.; Vaidyanathan, S.; Kumar, Anish; Jayakumar, T.; Raj, Baldev; Ray, K. K.

2007-05-01

The best combinations of mechanical properties (yield stress and fracture toughness) of M250 maraging steel is obtained through short-term thermal aging (3-10 h) at 755 K. This is attributed to the microstructure containing precipitation of intermetallic phases in austenite-free low-carbon martensite matrix. Over-aged microstructure, containing reverted austenite degrades the mechanical properties drastically. Hence, it necessitates identification of a suitable non-destructive evaluation (NDE) technique for detecting any reverted austenite unambiguously during aging. The influence of aging on microstructure, room temperature hardness and non-destructive magnetic parameters such as coercivity ( Hc), saturation magnetization ( Ms) and magnetic Barkhausen emission (MBE) RMS peak voltage is studied in order to derive correlations between these parameters in aged M250 maraging steel. Hardness was found to increase with precipitation of intermetallics during initial aging and decrease at longer durations due to austenite reversion. Among the different magnetic parameters studied, MBE RMS peak voltage was found to be very sensitive to austenite reversion (non-magnetic phase) as they decreased drastically up on initiation of austenite reversion. Hence, this parameter can be effectively utilized to detect and quantify the reverted austenite in maraging steel specimen. The present study clearly indicates that the combination of MBE RMS peak voltage and hardness can be used for unambiguous characterization of microstructural features of technological and practical importance (3-10 h of aging duration at 755 K) in M250 grade maraging steel.

Higher-Order Theory for Functionally Graded Materials

NASA Technical Reports Server (NTRS)

Aboudi, Jacob; Pindera, Marek-Jerzy; Arnold, Steven M.

1999-01-01

This paper presents the full generalization of the Cartesian coordinate-based higher-order theory for functionally graded materials developed by the authors during the past several years. This theory circumvents the problematic use of the standard micromechanical approach, based on the concept of a representative volume element, commonly employed in the analysis of functionally graded composites by explicitly coupling the local (microstructural) and global (macrostructural) responses. The theoretical framework is based on volumetric averaging of the various field quantities, together with imposition of boundary and interfacial conditions in an average sense between the subvolumes used to characterize the composite's functionally graded microstructure. The generalization outlined herein involves extension of the theoretical framework to enable the analysis of materials characterized by spatially variable microstructures in three directions. Specialization of the generalized theoretical framework to previously published versions of the higher-order theory for materials functionally graded in one and two directions is demonstrated. In the applications part of the paper we summarize the major findings obtained with the one-directional and two-directional versions of the higher-order theory. The results illustrate both the fundamental issues related to the influence of microstructure on microscopic and macroscopic quantities governing the response of composites and the technologically important applications. A major issue addressed herein is the applicability of the classical homogenization schemes in the analysis of functionally graded materials. The technologically important applications illustrate the utility of functionally graded microstructures in tailoring the response of structural components in a variety of applications involving uniform and gradient thermomechanical loading.

Microstructural characterization of an SA508–309L/308L–316L domestic dissimilar metal welded safe-end joint

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

Ming, Hongliang; Zhang, Zhiming; Wang, Jianqiu, E-mail: wangjianqiu@imr.ac.cn

2014-11-15

The microstructure of an SA508–309L/308L–316L domestic dissimilar metal welded safe-end joint was characterized in this work by optical microscopy, scanning electron microscopy (with electron back scattering diffraction) and micro-hardness testing. Epitaxial growth and competitive growth are evident in the 308L–316L fusion boundary regions. A martensite layer, carbon-depleted zones, and type-II and type-I boundaries are found in the SA508–309L fusion boundary regions, while only martensite and austenite mixed zones are observed in the SA508–308L fusion boundary regions. The microstructure near the fusion boundary and the microstructure transition in the SA508 heat affected zone are quite complex. Both for SA508–309L/308L and 308L–316L,more » the highest residual strain is located on the outside of the weldment. The residual strain and the grain boundary character distribution change with increasing distance from the fusion boundary in the heat affected zone of 316L. Micro-hardness measurements also reveal non-uniform mechanical properties across the weldment. - Highlights: • The microstructure of SA508 HAZ, especially near the FB, is very complex. • The outside of the dissimilar metal welded joint has the highest residual. • The micro-hardness distributions along the DMWJ are non-uniform.« less

Characterization of PCBs from computers and mobile phones, and the proposal of newly developed materials for substitution of gold, lead and arsenic.

PubMed

Dervišević, Irma; Minić, Duško; Kamberović, Željko; Ćosović, Vladan; Ristić, Mirjana

2013-06-01

In this paper, we have analyzed parts of printed circuit board (PCB) and liquid crystal display (LCD) screens of mobile phones and computers, quantitative and qualitative chemical compositions of individual components, and complete PCBs were determined. Differential thermal analysis (DTA) and differential scanning calorimetry (DSC) methods were used to determine the temperatures of phase transformations, whereas qualitative and quantitative compositions of the samples were determined by X-ray fluorescence spectrometry (XRF), inductively coupled plasma optical emission spectrometry (ICP-OES), and scanning electron microscopy (SEM)-energy dispersive X-ray spectrometry (EDS) analyses. The microstructure of samples was studied by optical microscopy. Based on results of the analysis, a procedure for recycling PCBs is proposed. The emphasis was on the effects that can be achieved in the recycling process by extraction of some parts before the melting process. In addition, newly developed materials can be an adequate substitute for some of the dangerous and harmful materials, such as lead and arsenic are proposed, which is in accordance with the European Union (EU) Restriction of the use of certain hazardous substances (RoHS) directive as well as some alternative materials for use in the electronics industry instead of gold and gold alloys.

Nonlinear ultrasonics for material state awareness

NASA Astrophysics Data System (ADS)

Jacobs, L. J.

2014-02-01

Predictive health monitoring of structural components will require the development of advanced sensing techniques capable of providing quantitative information on the damage state of structural materials. By focusing on nonlinear acoustic techniques, it is possible to measure absolute, strength based material parameters that can then be coupled with uncertainty models to enable accurate and quantitative life prediction. Starting at the material level, this review will present current research that involves a combination of sensing techniques and physics-based models to characterize damage in metallic materials. In metals, these nonlinear ultrasonic measurements can sense material state, before the formation of micro- and macro-cracks. Typically, cracks of a measurable size appear quite late in a component's total life, while the material's integrity in terms of toughness and strength gradually decreases due to the microplasticity (dislocations) and associated change in the material's microstructure. This review focuses on second harmonic generation techniques. Since these nonlinear acoustic techniques are acoustic wave based, component interrogation can be performed with bulk, surface and guided waves using the same underlying material physics; these nonlinear ultrasonic techniques provide results which are independent of the wave type used. Recent physics-based models consider the evolution of damage due to dislocations, slip bands, interstitials, and precipitates in the lattice structure, which can lead to localized damage.

Bioelectrocatalytic application of titania nanotube array for molecule detection.

PubMed

Xie, Yibing; Zhou, Limin; Huang, Haitao

2007-06-15

A bioelectrocatalysis system based on titania nanotube electrode has been developed for the quantitative detection application. Highly ordered titania nanotube array with inner diameter of 60 nm and total length of 540 nm was formed by anodizing titanium foils. The functionalization modification was achieved by embedding glucose oxidases inside tubule channels and electropolymerizing pyrrole for interfacial immobilization. Morphology and microstructure characterization, electrochemical properties and bioelectrocatalytic reactivities of this composite were fully investigated. The direct detection of hydrogen peroxide by electrocatalytic reduction reaction was fulfilled on pure titania nanotube array with a detection limit up to 2.0 x 10(-4)mM. A biosensor based on the glucose oxidase-titania/titanium electrode was constructed for amperometric detection and quantitative determination of glucose in a phosphate buffer solution (pH 6.8) under a potentiostatic condition (-0.4V versus SCE). The resulting glucose biosensor showed an excellent performance with a response time below 5.6s and a detection limit of 2.0 x 10(-3)mM. The corresponding detection sensitivity was 45.5 microA mM(-1)cm(-2). A good operational reliability was also achieved with relative standard deviations below 3.0%. This novel biosensor exhibited quite high response sensitivity and low detection limit for potential applications.

Quantitative micro-elastography: imaging of tissue elasticity using compression optical coherence elastography

PubMed Central

Kennedy, Kelsey M.; Chin, Lixin; McLaughlin, Robert A.; Latham, Bruce; Saunders, Christobel M.; Sampson, David D.; Kennedy, Brendan F.

2015-01-01

Probing the mechanical properties of tissue on the microscale could aid in the identification of diseased tissues that are inadequately detected using palpation or current clinical imaging modalities, with potential to guide medical procedures such as the excision of breast tumours. Compression optical coherence elastography (OCE) maps tissue strain with microscale spatial resolution and can delineate microstructural features within breast tissues. However, without a measure of the locally applied stress, strain provides only a qualitative indication of mechanical properties. To overcome this limitation, we present quantitative micro-elastography, which combines compression OCE with a compliant stress sensor to image tissue elasticity. The sensor consists of a layer of translucent silicone with well-characterized stress-strain behaviour. The measured strain in the sensor is used to estimate the two-dimensional stress distribution applied to the sample surface. Elasticity is determined by dividing the stress by the strain in the sample. We show that quantification of elasticity can improve the ability of compression OCE to distinguish between tissues, thereby extending the potential for inter-sample comparison and longitudinal studies of tissue elasticity. We validate the technique using tissue-mimicking phantoms and demonstrate the ability to map elasticity of freshly excised malignant and benign human breast tissues. PMID:26503225

In Situ Imaging during Compression of Plastic Bonded Explosives for Damage Modeling

NASA Astrophysics Data System (ADS)

Yeager, John; Manner, Virginia; Patterson, Brian; Walters, David; Cordes, Nikolaus; Henderson, Kevin; Tappan, Bryce; Luscher, Darby

2017-06-01

The microstructure of plastic bonded explosives (PBXs) is known to influence behavior during insults such as deformation, heating or initiation to detonation. Obtaining three-dimensional microstructural data can be difficult due in part to fragility of the material and small feature size. X-ray computed tomography (CT) is an ideal characterization technique but the explosive crystals and binder in formulations such as PBX 9501 do not have sufficient x-ray contrast to differentiate between the components. Here, we have formulated several PBXs using octahydro-1,3,5,7-tetranitro-1,3,5,7- tetrazocine (HMX) crystals and low-density binder systems. The full three-dimensional microstructure of these samples has been characterized using microscale CT during uniaxial mechanical compression in an interrupted in situ modality. The rigidity of the binder was observed to significantly influence fracture, crystal-binder delamination, and material flow. Additionally, the segmented, 3D images were meshed for finite element simulation. Initial results of the mesoscale modeling exhibit qualitatively similar delamination. Los Alamos National Laboratory - LDRD.

(The relationship between microstructure and magnetic properties in high-energy permanent magnets characterized by polytwinned structures)

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

Not Available

1992-01-01

This report summarizes the results of a study of the relationship between microstructure and magnetic properties in a unique genre of ferromagnetic material characterized by a polysynthetically twinned structure which arises during solid state transformation. These results stem from the work over a period of approximately 27 months of a nominal 3 year grant period. The report also contains a proposal to extend the research project for an additional 3 years. The polytwinned structures produce an inhomogeneous magnetic medium in which the easy axis of magnetization varies quasi-periodically giving rise to special domain configurations which are expected to markedly influencemore » the mechanism of magnetization reversal and hysteresis behavior of these materials in bulk or thin films. The extraordinary permanent magnet properties exhibited by the well-known Co-Pt alloys as well as the Fe-Pt and Fe-Pd systems near the equiatomic composition derive from the formation of a polytwinned microstructure.« less

[The relationship between microstructure and magnetic properties in high-energy permanent magnets characterized by polytwinned structures

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

Not Available

1992-07-01

This report summarizes the results of a study of the relationship between microstructure and magnetic properties in a unique genre of ferromagnetic material characterized by a polysynthetically twinned structure which arises during solid state transformation. These results stem from the work over a period of approximately 27 months of a nominal 3 year grant period. The report also contains a proposal to extend the research project for an additional 3 years. The polytwinned structures produce an inhomogeneous magnetic medium in which the easy axis of magnetization varies quasi-periodically giving rise to special domain configurations which are expected to markedly influencemore » the mechanism of magnetization reversal and hysteresis behavior of these materials in bulk or thin films. The extraordinary permanent magnet properties exhibited by the well-known Co-Pt alloys as well as the Fe-Pt and Fe-Pd systems near the equiatomic composition derive from the formation of a polytwinned microstructure.« less

Effective properties of a fly ash geopolymer: Synergistic application of X-ray synchrotron tomography, nanoindentation, and homogenization models

DOE PAGES

Das, Sumanta; Yang, Pu; Singh, Sudhanshu S.; ...

2015-09-02

Microstructural and micromechanical investigation of a fly ash-based geopolymer using: (i) synchrotron x-ray tomography (XRT) to determine the volume fraction and tortuosity of pores that are influential in fluid transport, (ii) mercury intrusion porosimetry (MIP) to capture the volume fraction of smaller pores, (iii) scanning electron microscopy (SEM) combined with multi-label thresholding to identify and characterize the solid phases in the microstructure, and (iv) nanoindentation to determine the component phase elastic properties using statistical deconvolution, is reported in this paper. The phase volume fractions and elastic properties are used in multi-step mean field homogenization (Mori- Tanaka and double inclusion) modelsmore » to determine the homogenized macroscale elastic modulus of the composite. The homogenized elastic moduli are in good agreement with the flexural elastic modulus determined on macroscale paste beams. As a result, the combined use of microstructural and micromechanical characterization tools at multiple scales provides valuable information towards the material design of fly ash geopolymers.« less

The relationship between microstructure and magnetic properties in high-energy permanent magnets characterized by polytwinned structures

NASA Astrophysics Data System (ADS)

This report summarizes the results of a study of the relationship between microstructure and magnetic properties in a unique genre of ferromagnetic material characterized by a polysynthetically twinned structure which arises during solid state transformation. These results stem from the work over a period of approximately 27 months of a nominal 3 year grant period. The report also contains a proposal to extend the research project for an additional 3 years. The polytwinned structures produce an inhomogeneous magnetic medium in which the easy axis of magnetization varies quasi-periodically giving rise to special domain configurations which are expected to markedly influence the mechanism of magnetization reversal and hysteresis behavior of these materials in bulk or thin films. The extraordinary permanent magnet properties exhibited by the well-known Co-Pt alloys as well as the Fe-Pt and Fe-Pd systems near the equiatomic composition derive from the formation of a polytwinned microstructure.

Multi-scale invertigation of the relationship between the microstructure and mechanical properties in dual phase steels

NASA Astrophysics Data System (ADS)

Zhang, Fan

Dual phase steel alloys belong to the first generation of advanced high strength steels that are widely used in the automotive industry to form body structure and closure panels of vehicles. A deeper understanding of the microstructural features, such as phase orientation and morphology are needed in order to establish their effect on the mechanical performance and to design a material with optimized attributes. In this work, our goal is to establish what kind of relationship exist between the mechanical properties and the microstructural representation of dual phase steels obtained from experimental observations. Microstructure in different specimens are characterized with advanced experimental techniques as optical microscopy, scanning electron microscopy, transmission electron microscopy, electron backscatter diffraction pattern, scanning probe microscopy, and nanoindentation. Nanoindentation, Vickers hardness and tensile testing are conducted to reveal a multi-scale mechanical performance on original material and also specimens under a variety combinations of temperatures, cooling rates, and rolling conditions. To quantify the single phase properties in each sample, an inverse method is adopted using experimental nanoindentation load-depth curves to obtain tensile stress-strain curves for each phase, and the inverse results were verified with the true stress-strain curves from tensile tests. This work also provides the insight on spatial phase distribution of different phases through a 2-point correlation statistical methodology and relate to material strength and formability. The microstructure information is correlated with the results of mechanical tests. The broken surfaces from tensile testing are analyzed to discover the fracture mechanism in relation to martensite morphology and distribuion. Viscoplastic self-consistent fast Fourier Transformation simulations is also used to compute efficiently the local and the homogenized viscoplastic response of the polycrystalline microstructure. The specific objectives of this work are 1) the development of etching techniques and electron backscatter diffraction strategies to characterize ferrite and martensite phases in steel; 2) the uncovering of a relationship between strength/ductility and material microstructure, 3) a statistical description to quantify the spatial distributions of these phases; and finally 4) the simulation of the microstructural evolution using parameters obtained from the experiments.

Graphite Microstructural Characterization Using Time-Domain and Correlation-Based Ultrasonics

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

Spicer, James

Among techniques that have been used to determine elastic modulus in nuclear graphites, ultrasonic methods have enjoyed wide use and standards using contacting piezoelectric tranducers have been developed to ensure repeatability of these types of measurements. However, the use of couplants and the pressures used to effectively couple transducers to samples can bias measurements and produce results that are not wholly related to the properties of the graphite itself. In this work, we have investigated the use of laser ultrasonic methods for making elastic modulus measurements in nuclear graphites. These methods use laser-based transmitters and receivers to gather data andmore » do not require use of ultrasonic couplants or mechanical contact with the sample. As a result, information directly related to the elastic responses of graphite can be gathered even if the graphite is porous, brittle and compliant. In particular, we have demonstrated the use of laser ultrasonics for the determination of both Young’s modulus and shear modulus in a range of nuclear graphites including those that are being considered for use in future nuclear reactors. These results have been analyzed to assess the contributions of porosity and microcracking to the elastic responses of these graphites. Laser-based methods have also been used to assess the moduli of NBG-18 and IG-110 where samples of each grade were oxidized to produce specific changes in porosity. These data were used to develop new models for the elastic responses of nuclear graphites and these models have been used to infer specific changes in graphite microstructure that occur during oxidation that affect elastic modulus. Specifically, we show how ultrasonic measurements in oxidized graphites are consistent with nano/microscale oxidation processes where basal plane edges react more readily than basal plane surfaces. We have also shown the use of laser-based methods to perform shear-wave birefringence measurements and have shown how these measurements can be used to assess elastic anisotropy in nuclear graphites. Using models developed in this program, ultrasonic data were interpreted to extract orientation distribution coefficients that could be used to represent anisotropy in these materials. This demonstration showed the use of ultrasonic methods to quantify anisotropy and how these methods provide more detailed information than do measurements of thermal expansion – a technique commonly used for assessing anisotropy in nuclear graphites. Finally, we have employed laser-based, ultrasonic-correlation techniques in attempts to quantify aspects of graphite microstructure such as pore size and distribution. Results of these measurements indicate that additional work must be performed to make this ultrasonic approach viable for quantitative microstructural characterization.« less

Evolution of microstructure in stainless martensitic steel for seamless tubing

NASA Astrophysics Data System (ADS)

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

2017-12-01

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

Microstructural and Mechanical Characterization of Shear Formed Aluminum Alloys for Airframe and Space Applications

NASA Technical Reports Server (NTRS)

Troeger, L. P.; Domack, M. S.; Wagner, J. A.

1998-01-01

Advanced manufacturing processes such as near-net-shape forming can reduce production costs and increase the reliability of launch vehicle and airframe structural components through the reduction of material scrap and part count and the minimization of joints. The current research is an investigation of the processing-microstructure-property relationship for shear formed cylinders of the Al-Cu-Li-Mg-Ag alloy 2195 for space applications and the Al-Cu-Mg-Ag alloy C415 for airframe applications. Cylinders which have undergone various amounts of shear-forming strain have been studied to assess the microstructure and mechanical properties developed during and after shear forming.

Simultaneous Noncontact Precision Imaging of Microstructural and Thickness Variation in Dielectric Materials Using Terahertz Energy

NASA Technical Reports Server (NTRS)

Roth, Don J.; Seebo, Jeffrey P.; Winfree, William P.

2008-01-01

This article describes a noncontact single-sided terahertz electromagnetic measurement and imaging method that simultaneously characterizes microstructural (egs. spatially-lateral density) and thickness variation in dielectric (insulating) materials. The method was demonstrated for two materials-Space Shuttle External Tank sprayed-on foam insulation and a silicon nitride ceramic. It is believed that this method can be used as an inspection method for current and future NASA thermal protection system and other dielectric material inspection applications, where microstructural and thickness variation require precision mapping. Scale-up to more complex shapes such as cylindrical structures and structures with beveled regions would appear to be feasible.

The microstructure and microhardness of friction stir welded dissimilar copper/Al-5% Mg alloys

NASA Astrophysics Data System (ADS)

Kalashnikova, T. A.; Shvedov, M. A.; Vasilyev, P. A.

2017-12-01

A friction stir welded joint between copper and aluminum alloy has been investigated and characterized for the microstructure and microhardness number distribution. The microstructural evolution of the joint is studied using optical microscopy and microhardness. The mechanical characteristics in structural zones of FSW joints are determined by Vickers microhardness measurements. Samples were cut across the cross section. It is shown that intermetallic Cu/Al particles are formed at interfaces. The intermetallics microhardness in the dissimilar aluminum/cooper FSW joint differs from that of the joint produced by fusion welding. The grain structures obtained in different dissimilar joint zones are examined.

Response of DP 600 products to dynamic impact loads

NASA Astrophysics Data System (ADS)

Clark, Deidra Darcell

The objective of this study was to compare the microstructural response of various DP 600 products subjected to low velocity, dynamic impact tests, typically encountered in a car crash. Since the response of steel is sensitive to its microstructure as controlled by the alloying elements, phase content, and processing; various DP 600 products may respond differently to crashes. The microstructure before and after dynamic impact deformation at 5 and 10 mph was characterized with regards to grain size, morphology, and phase content among vendors A, B, and C to evaluate efficiency in absorbing energy mechanisms during a crash simulated by dynamic impact testing in a drop tower.

Biphasic thermoelectric materials derived from the half-Heusler/full-Heusler system Ti-Ni-Sn

NASA Astrophysics Data System (ADS)

Douglas, Jason Everett

Among the possible avenues for increasing the efficiency of global energy usage, thermoelectrics are an exciting, solid-state option. Thermoelectric materials, which convert an internal temperature gradient into a voltage and vice versa, have found applications in refrigeration as well as power generation from waste heat. TiNiSn, a semiconductor of the half-Heusler (hH) crystal structure, is of particular interest due to its very favorable electronic transport properties, conductivity (sigma) and Seebeck coefficient ( S), at relevant temperature regimes (between 600 K and 900 K). Unfortunately, its overall efficiency is hampered by a comparatively high thermal conductivity (kappa). In the design of thermoelectric materials, a number of approaches have been taken to increase the thermoelectric figure of merit, ZT = ( S2sigma/kappa)T, where T is temperature. In this work we examine how microstructure can be used to alter these thermoelectric propertiesin a biphasic Ti-Ni-Sn materials containing full-Heusler (fH) TiNi2Sn embedded within hH thermoelectric TiNiSn. We explored a wide range of Ni compositions in TiNi1+xSn--from stoichiometric TiNiSn to high Heusler volume fraction, TiNi1.25Sn--materials prepared by levitation induction melting followed by annealing. Phase distributions and microstructure were characterized using synchrotron x-ray diffraction and optical and electron microscopy. In a sample of the nominal composition TiNi1.15Sn, a significant decrease in thermal conductivity (about 30%) is observed for the biphasic material despite the metallic second-phase particles existing at the micrometer scale; a 50% increase in the electrical conductivity is also measured. These result in a maximum figure of merit, ZT, of 0.44 at 800 K, which is 25% greater than is observed for the x = 0 sample. Density functional theory calculations using hybrid functionals were performed to determine band alignments between the half- and full-Heusler compounds, as well as comparative energies of formation. We discuss the effects of thermal treatment on the microstructure of biphasic materials comprising hH and fH phases, as well as on their associated thermal transport properties. The fH phase is observed to be semi-coherent with the hH majority phase. Microstructural analysis, both in 2-D and 3-D, shows that the fH solidifies first and the hH then nucleates on these fH dendrites as the melt becomes depleted of Ni. The various heat treatments generated microstructures containing second phase precipitates ranging from 10 nm to a few micrometers, reducing the connectivity of the percolated network observed previously. The materials were characterized with regard to morphology, size, shape and orientation relationship of the fH precipitates with the hH matrix. The precipitate size and morphology are very sensitive to Ni concentration in fH/hH phase. The thermal conductivity is found to drop by 50% as the precipitate size increases; however, this enhancement was not retained after high temperature exposure. In addition to the microstructural implications of TiNi 1+xSn alloying, the (crystal) structural implications of excess Ni in the TiNiSn hH compound were investigated next through a combination of synchrotron x-ray and neutron scattering studies, in conjunction with first principles density functional theory calculations on supercells. Despite the phase diagram suggesting that TiNiSn is a line compound with no solid solution, for small x in TiNi 1+xSn there is indeed an appearance--from careful analysis of the scattering--of some solubility, with the excess Ni occupying the interstitial tetrahedral site in the hH structure. The analysis performed here would point to the excess Ni not being statistically distributed, but rather occurring as coherent nanoclusters. First principles calculations of energetics, carried out using supercells, support a scenario of Ni interstitials clustering, rather than a statistical distribution. Finally, we also used a unique advanced tomographic technique with multimodal characterization capabilities, necessary to understand TiNiSn/TiNi2Sn composites. The three-dimensional microstructure of levitation melted TiNi 1.20Sn was characterized using the TriBeam system, a scanning electron microscope equipped with a femtosecond laser for rapid serial sectioning, to map the character of interfaces, in a 155 microm x 178 microm x 210 microm volume. We found the phase boundaries and grain boundaries to be decoupled and that the predominant phases present in the material, TiNiSn and TiNi2Sn, have a percolated structure. The distribution of coherent interfaces and high-angle interfaces has been measured quantitatively.

Hydrocarbon-Based Polymer Electrolyte Membranes: Importance of Morphology on Ion Transport and Membrane Stability.

PubMed

Shin, Dong Won; Guiver, Michael D; Lee, Young Moo

2017-03-22

A fundamental understanding of polymer microstructure is important in order to design novel polymer electrolyte membranes (PEMs) with excellent electrochemical performance and stabilities. Hydrocarbon-based polymers have distinct microstructure according to their chemical structure. The ionic clusters and/or channels play a critical role in PEMs, affecting ion conductivity and water transport, especially at medium temperature and low relative humidity (RH). In addition, physical properties such as water uptake and dimensional swelling behavior depend strongly on polymer morphology. Over the past few decades, much research has focused on the synthetic development and microstructural characterization of hydrocarbon-based PEM materials. Furthermore, blends, composites, pressing, shear field, electrical field, surface modification, and cross-linking have also been shown to be effective approaches to obtain/maintain well-defined PEM microstructure. This review summarizes recent work on developments in advanced PEMs with various chemical structures and architecture and the resulting polymer microstructures and morphologies that arise for potential application in fuel cell, lithium ion battery, redox flow battery, actuators, and electrodialysis.

Retained austenite thermal stability in a nanostructured bainitic steel

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

Avishan, Behzad, E-mail: b_avishan@sut.ac.ir; Garcia-Mateo, Carlos, E-mail: cgm@cenim.csic.es; Yazdani, Sasan, E-mail: yazdani@sut.ac.ir

2013-07-15

The unique microstructure of nanostructured bainite consists of very slender bainitic ferrite plates and high carbon retained austenite films. As a consequence, the reported properties are opening a wide range of different commercial uses. However, bainitic transformation follows the T{sub 0} criteria, i.e. the incomplete reaction phenomena, which means that the microstructure is not thermodynamically stable because the bainitic transformation stops well before austenite reaches an equilibrium carbon level. This article aims to study the different microstructural changes taking place when nanostructured bainite is destabilized by austempering for times well in excess of that strictly necessary to end the transformation.more » Results indicate that while bainitic ferrite seems unaware of the extended heat treatment, retained austenite exhibits a more receptive behavior to it. - Highlights: • Nanostructured bainitic steel is not thermodynamically stable. • Extensive austempering in these microstructures has not been reported before. • Precipitation of cementite particles is unavoidable at longer austempering times. • TEM, FEG-SEM and XRD analysis were used for microstructural characterization.« less

Microstructural Characterization of Thermomechanical and Heat-Affected Zones of an Inertia Friction Welded Astroloy

NASA Astrophysics Data System (ADS)

Oluwasegun, K. M.; Olawale, J. O.; Ige, O. O.; Shittu, M. D.; Adeleke, A. A.; Malomo, B. O.

2014-08-01

The behaviour of γ' phase to thermal and mechanical effects during rapid heating of Astroloy, a powder metallurgy nickel-based superalloy has been investigated. The thermo-mechanical-affected zone (TMAZ) and heat-affected zone (HAZ) microstructures of an inertia friction welded (IFW) Astroloy were simulated using a Gleeble thermo-mechanical simulation system. Detailed microstructural examination of the simulated TMAZ and HAZ and those present in actual IFW specimens showed that γ' particles persisted during rapid heating up to a temperature where the formation of liquid is thermodynamically favored and subsequently re-solidified eutectically. The result obtained showed that forging during the thermo-mechanical simulation significantly enhanced resistance to weld liquation cracking of the alloy. This is attributable to strain-induced rapid isothermal dissolution of the constitutional liquation products within 150 μm from the center of the forged sample. This was not observed in purely thermally simulated samples. The microstructure within the TMAZ of the as-welded alloy is similar to the microstructure in the forged Gleeble specimens.

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

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.