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Search indexed NASA NTRS and DOE OSTI research on propulsion, heat transfer, battery materials and energy systems. Follow report and document links to the original sources.

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At least 55 records · Page 3
All sourcesNASA NTRSDOE OSTI
DOE OSTI2018

A Graph Theory-Based Automated Twin Recognition Technique for Electron Backscatter Diffraction Analysis

Abstract The present article introduces a new software, Microstructure Evaluation Tool for Interface Statistics (METIS), that performs high-throughput microstructure statistical analysis from electron backscatter diffraction maps. Emphasis is placed on the detection of twin domains in hexagonal close-packed metals. The numerical framework on which METIS is built leverages graph theory, group structures, and associated numerical algorithms to automatically detect twins and unravel both their intrinsic characteristics features and those pertaining to their interactions. The proposed graphical interface allows for the detection and correction of unlikely twin/parent associations rendering the approach applicable to highly deformed microstructures. Twin statistics and microstructural data are classified and saved in a relational database that can be interrogated via either GUI or SQL requests to reveal a wide spectrum of features of the microstructure. Illustration of the approach is performed in the case of zirconium.

36 MATERIALS SCIENCE↗
DOE OSTI2018

Phase quantification in low carbon Nb-Mo bearing steel by electron backscatter diffraction technique coupled with kernel average misorientation

Highlights: • The microstructures in a low carbon Nb-Mo bearing steel have been investigated. • EBSD combined with a (KAM) map has been used for quantification. • The effects of step size and kernel size on quantification are systemically discussed. • The result indicates that the kernel size should be close to the sub-structure of the granular bainite. - Abstract: An efficient and accurate method is developed for microstructural quantification of complex phases in a low carbon Nb-Mo bearing steel, of which optical micrographs show that it consists of granular bainite and a small amount of ferrite. Our previous work, proposing a method to measure the misorientation angles via electron backscatter diffraction (EBSD) to differentiate granular bainite and ferrite, has been reported. That method is accurate for phase quantification but laborious for the characterization process. To resolve this difficulty, in this study, EBSD combined with a kernel average misorientation (KAM) map is used for phase characterization. Comparisons are made among KAM maps with different kernel sizes (300 to 600 nm) and various step sizes (100 to 600 nm). It is found that a kernel size close to the sub-structure size of granular bainite (500 nm) is optimal for phase identification, while varied step sizes produce relatively invariant results. Therefore, KAM maps can be used for fast and reliable phase quantification, provided that an appropriate kernel size and a large step size are used.

36 MATERIALS SCIENCE↗
NASA NTRS2023

Ceramic Capacitor Grain Size Analysis Using Electron Backscatter Diffraction (EBSD)

The overall scope of this NESC study was to identify (or develop) a tool, methodology, or process that can inspect a ceramic capacitor and consistently return repeatable grain size distribution results. It is important to note that the development of a machine learning technique was considered as an option for this study, but only if an existing automated tool was not available. This report explains why the Electron Backscatter Diffraction analysis method for grain structure and size distribution was deemed a suitable candidate for this work.

Electron Backscatter Diffraction↗
DOE OSTI2021

An automated procedure built on MTEX for reconstructing deformation twin hierarchies from electron backscattered diffraction datasets of heavily twinned microstructures

Here we present a set of algorithms built on the MTEX and MATLAB graph toolboxes for automatic reconstruction of deformation twin hierarchies from Electron Backscatter Diffraction (EBSD) datasets with a focus on developing methods for heavily twinned microstructures (twin fractions >0.5). The algorithms address key issues arising at large strains, mainly: missing twin relationships, grouping of heavily deformed grain fragments into families of similar orientation originating from a single initial grain, identification of parent fragments for large twin volume fractions, and classification of families having twin relationships with multiple families. To facilitate the development of these algorithms, large-grained ultra-high purity α-Ti deformed in compression along two directions is investigated. Graphs are utilized to handle non-local geometric merging and to represent relationships throughout the reconstruction process. When determining if a grain fragment is from the undeformed microstructure, the combined metrics of the fragment's orientation volume fraction in the initial texture and the directed graph centrality measure of out-closeness (the number of nodes reached in a graph from a given node) are essential. To address automation in reconstructing the sequence of twinning and relating fragments originating from a single grain in the initial microstructure, the twin family tree is formulated as a minimum spanning tree emanating from the initial grain family. A scheme constructing the distances associated with twin relationship comprising the spanning tree is developed, and a novel quasi-directional Prim spanning tree algorithm is used to determine the twin family tree. The procedure is demonstrated to significantly improve the level of automation in reconstructing twin hierarchies in heavily twinned microstructure compared to other methodologies in literature. The procedure can readily be applied to analyses of twinning in metals, as well as provide an approach for routinely extracting twin statistics at larger deformation levels than previously possible. Significantly, the procedure is demonstrated to be capable of identifying third generation twinning in α-Ti microstructures.

36 MATERIALS SCIENCE↗
DOE OSTI2020

An Electron Backscatter Diffraction Analysis of Grain Boundary Initiated Discontinuous Precipitation in U-10Mo

The effect of varied thermomechanical processing on discontinuous precipitation (DP) in U-10Mo was investigated, with specific emphasis on understanding the role of grain boundary misorientation in DP. Varied prior homogenization heat treatment and thermomechanical processing resulted in differences in both the fraction of DP and the colony width, and was attributed to variations in the grain boundary misorientation distribution. Regardless of the degree of DP-based transformation, extensive growth of DP colonies was dominant on 30°–45° misorientation boundaries. Interestingly, misorientation histograms of the deformed and annealed specimens suggest the processing steps involved may have inhibited DP colony growth along a small fraction of these high angle boundaries. Large-area electron backscatter diffraction montages coupled with high resolution mapping suggest symmetric {110}-type interfaces may be important considerations for mitigating extensive DP growth in this alloy system.

Discontinuous Precipitation, Uranium, Electron Bac↗
DOE OSTI2014

STRAIN CORRELATIONS IN ALLOY 690 MATERIALS USING ELECTRON BACKSCATTER DIFFRACTION AND VICKERS HARDNESS

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

Alloy 690↗
DOE OSTI2021

Application of electron backscatter diffraction techniques to quantify effects of aging on sub-grain and spatial heterogeneity in NMC cathodes

Identification and evaluation of structural heterogeneity in spent cathode materials is crucial to developing appropriate remediation strategies for novel recycling processes. Native heterogeneities may be exacerbated during the cell's operational lifetime, as sub-particle-scale variations induce anisotropic expansion and contraction upon cycling. Structural transformations resulting from repeated cycling and calendar aging predominantly occur at the secondary particle surface and at the grain boundaries (GBs) between primary particles. However, the diffusion and stress build up around and across GBs are poorly understood. In this study, electron backscatter diffraction (EBSD) is employed to track sub-grain lattice structure across a statistically relevant number of Li(Ni0.33Mn0.33Co0.33)O2 (NMC-111) particles. Specifically, differences in lattice misorientation – measured as the deviation from the grain's average orientation – are tracked as a function of position within the electrode (near current collector, middle, and near separator) and as a function of electrochemical cycling. Further, a novel method of structural analysis is developed, offering insight into sub-grain diffusion behavior by comparing lattice misorientation near the grain boundary versus in the grain bulk. The present results suggest that electrode-scale spatial heterogeneity in lattice structure is induced by initial manufacturing conditions, and that radial gradients in lattice misorientation evolve at the primary particle scale with repeated electrochemical cycling.

25 ENERGY STORAGE↗
DOE OSTI2017

Influence of Noise-Generating Factors on Cross-Correlation Electron Backscatter Diffraction (EBSD) Measurement of Geometrically Necessary Dislocations (GNDs)

Abstract Studies of dislocation density evolution are fundamental to improved understanding in various areas of deformation mechanics. Recent advances in cross-correlation techniques, applied to electron backscatter diffraction (EBSD) data have particularly shed light on geometrically necessary dislocation (GND) behavior. However, the framework is relatively computationally expensive—patterns are typically saved from the EBSD scan and analyzed offline. A better understanding of the impact of EBSD pattern degradation, such as binning, compression, and various forms of noise, is vital to enable optimization of rapid and low-cost GND analysis. This paper tackles the problem by setting up a set of simulated patterns that mimic real patterns corresponding to a known GND field. The patterns are subsequently degraded in terms of resolution and noise, and the GND densities calculated from the degraded patterns using cross-correlation ESBD are compared with the known values. Some confirmation of validity of the computational degradation of patterns by considering real pattern degradation is also undertaken. The results demonstrate that the EBSD technique is not particularly sensitive to lower levels of binning and image compression, but the precision is sensitive to Poisson-type noise. Some insight is also gained concerning effects of mixed patterns at a grain boundary on measured GND content.

Materials Science↗
DOE OSTI2018

Electron Backscattered Diffraction Study of Pulse Electrodeposited Cu-Y{sub 2}O{sub 3} Composite Coating

The current investigation is an effort of correlating the grain growth, crystallographic orientation and second-phase Y{sub 2}O{sub 3} particles to the mechanical properties of the electrodeposited pure copper (Cu) and Cu-Y{sub 2}O{sub 3} coatings. Energy-dispersive spectrum and elemental mapping confirm the codeposition of Y{sub 2}O{sub 3} in the composite coating matrix, which indeed justifies the composite (Cu-Y{sub 2}O{sub 3}) coating. Both pure Cu and Cu-Y{sub 2}O{sub 3} coatings have (101) preferred orientation; however, the volume fraction is found comparatively lower in composite coating. Both microstructural and textural characterization through electron backscattered diffraction technique show significant grain refinement in case of Cu-Y{sub 2}O{sub 3} composite coating compared to pure Cu coating, and prominent 〈011〉 fiber texture is observed in case of pure Cu coating compared to composite coating. By the addition of second-phase Y{sub 2}O{sub 3} in the matrix, the 〈011〉 fiber texture is disintegrated and concentrated at ϕ{sub 1} = 37°, ϕ = 45°, ϕ{sub 2} = 0°. Despite lower volume fraction of 〈011〉 fiber texture, better mechanical properties (hardness and wear resistance) of the composite coating compared to pure Cu coating can be attributed to finer grain size, higher misorientation angle and incorporation of second-phase Y{sub 2}O{sub 3} particles.

36 MATERIALS SCIENCE↗
NASA NTRS2009

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

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

Timms, Nick↗
DOE OSTI2024

Determination of α lamellae orientation in a β-Ti alloy using electron backscatter diffraction

The spatial orientation of α lamellae in a metastable β-Ti matrix of Timetal LCB (Ti–6.8 Mo–4.5 Fe–1.5 Al in wt%) was examined and the orientation of the hexagonal close-packed α lattice in the α lamella was determined. For this purpose, a combination of methods of small-angle X-ray scattering, scanning electron microscopy and electron backscatter diffraction was used. The habit planes of α laths are close to {111} β , which corresponds to (1$\bar3$20) α in the hexagonal coordinate system of the α phase. The longest α lamella direction lies approximately along one of the $\langle$110$\rangle$ β directions which are parallel to the specific habit plane. Taking into account the average lattice parameters of the β and α phases in aged conditions in Timetal LCB, it was possible to index all main axes and faces of an α lath not only in the cubic coordinate system of the parent β phase but also in the hexagonal system of the α phase.

36 MATERIALS SCIENCE↗
DOE OSTI2023

Characterization of the radial microstructural evolution in LWR UO 2 using electron backscatter diffraction

Studies on high burnup UO 2 subjected to loss-of-coolant accident conditions have shown that restructured regions of the fuel are susceptible to pulverization and eventual dispersal. Due to a lack of pre-test characterization, the distinct microstructural features rendering the fuel prone to fragmentation remain ambiguous. Four samples of commercially irradiated light-water reactor UO 2 have been characterized utilizing electron backscatter diffraction to assess the susceptible microstructure. The microscopy focused on determining the burnup and temperature conditions responsible for the formation of the different microstructural regions where the regions were denoted as the high-burnup structure (HBS), HBS transition, mid-radial, restructured central, and central region. Previous works have outlined the specific conditions required for the restructuring of the microstructure into the HBS, but the conditions responsible for the restructuring in the central region of the fuel are not well understood. The four analyzed samples confirm a burnup threshold of 61 GWd/tU, and an unknown temperature range is needed to facilitate the formation of the restructured central region. In conclusion, additional fuel performance evaluations are needed to quantify the temperature range promoting restructuring in the central region.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗
DOE OSTI2019

A comparison of adiabatic shear bands in wrought and additively manufactured 316L stainless steel using nanoindentation and electron backscatter diffraction

The resistance of stainless steels to shear localization is dependent on processing and microstructure. The amount of research evaluating the shear response of additively manufactured (AM) stainless steels compared to traditionally manufactured ones is limited. To address this gap, experiments were performed on directed energy deposition AM as-built and wrought 316L stainless steel using a forced shear technique with a hat-shaped specimen and a Split-Hopkinson pressure bar. The resulting adiabatic shear bands were characterized with electron backscatter diffraction (EBSD) and nanoindentation to quantify the changes in microstructure and deformation hardening across shear band regions and between the wrought and AM materials. Despite significant differences between the wrought and AM materials including the forced shear response, the postmortem states of work hardening due to the shear band deformation are nearly the same. The maximum nanoindentation stresses occurred in the shear band center with similar magnitudes and only minor differences away from the shear band. Although EBSD data cannot be resolved in the shear band center, misorientation trends, particularly grain reference orientation deviation, were found to closely resemble nanoindentation trends. In conclusion, the combination of EBSD misorientation and nanoindentation, which are linked through changes in dislocation density, is a viable protocol to quantify local changes to macroscopically applied deformation.

36 MATERIALS SCIENCE↗
DOE OSTI2023

Determining Stress in Metallic Conducting Layers of Microelectronics Devices Using High Resolution Electron Backscatter Diffraction and Finite Element Analysis

Delayed failure due to stress voiding is a concern with some aging microelectronics, as these voids can grow large enough to cause an open circuit. Local measurements of stress in the metallic layers are crucial to understanding and predicting this failure, but such measurements are complicated by the fact that exposing the aluminum conducting lines will relieve most of their stress. In this study, we instead mechanically thin the device substrate and measure distortions on the thinned surface using high resolution electron backscatter diffraction (HREBSD). These measurements are then related to the stresses in the metallic layers through elastic simulations. This study found that in legacy components that had no obvious voids, the stresses were comparable to the theoretical stresses at the time of manufacture (≈300 MPa). Distortion fields in the substrate were also determined around known voids, which may be directly compared to stress voiding models. In conclusion, the technique presented here for stress determination, HREBSD coupled with finite element analysis to infer subsurface stresses, is a valuable tool for assessing failure in layered microelectronics devices.

HREBSD↗
DOE OSTI2024

High-Throughput Microstructural Characterization and Process Correlation Using Automated Electron Backscatter Diffraction

The need to optimize the processing conditions of additively manufactured (AM) metals and alloys has driven advances in throughput capabilities for material property measurements such as tensile strength or hardness. High-throughput (HT) characterization of AM metal microstructure has fallen significantly behind the pace of property measurements due to intrinsic bottlenecks associated with the artisan and labor-intensive preparation methods required to produce highly polished surfaces. This inequality in data throughput has led to a reliance on heuristics to connect process to structure or structure to properties for AM structural materials. In this study, we show a transformative approach to achieve laser powder bed fusion (LPBF) printing, HT preparation using dry electropolishing and HT electron backscatter diffraction (EBSD). This approach was used to construct a library of > 600 experimental EBSD sample sets spanning a diverse range of LPBF process conditions for AM Kovar. This vast library is far more expansive in parameter space than most state-of-the-art studies, yet it required only approximately 10 labor hours to acquire. Build geometries, surface preparation methods, and microscopy details, as well as the entire library of >600 EBSD data sets over the two sample design versions, have been shared with intent for the materials community to leverage the data and further advance the approach. Using this library, we investigated process–structure relationships and uncovered an unexpected, strong dependence of microstructure on location within the build, when varied, using otherwise identical laser parameters.

Characterization and Analytical Technique↗
DOE OSTI2026

Emerging hierarchical dislocation structures: Insights from scanning electron microscopy-electron backscatter diffraction in situ tensile testing and multifractal analysis

Understanding the evolution of dislocation structures during plastic deformation is critical for predicting the mechanical performance of metallic materials. In this work, we applied in situ scanning electron microscopy/electron backscatter diffraction tensile testing combined with multifractal (MF) analysis to assess deformation-induced dislocation structure evolution in solution-annealed 304 L stainless steel, both in its as-received and neutron-irradiated states (5.4 displacements per atom). The analysis of kernel average misorientation patterns revealed the formation of hierarchical dislocation arrangements that exhibit clear MF scaling behavior. Despite pronounced visual differences between nonirradiated and irradiated specimens—most notably, the appearance of dislocation channels after irradiation—the singularity spectra suggest that both conditions give rise to similar underlying hierarchical structures. MF analysis provides a quantitative measure of the spatial complexity and self-organization of dislocation patterns, highlighting the accelerated emergence and evolution of the dislocation structures in irradiated polycrystalline materials, as well as the limitation of their spatial extent. The findings indicate that irradiation not only modifies microstructure but also alters correlation-driven dislocation organization. More generally, they demonstrate that MF analysis is a powerful tool for probing mesoscale deformation mechanisms.

Dislocation structures↗