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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 19 records
All sourcesNASA NTRSDOE OSTI
DOE OSTI2024

Imaging and Segmenting Grains and Subgrains Using Backscattered Electron Techniques

We present two new methods of processing data from backscattered electron signals in a scanning electron microscope to image grains and subgrains. The first combines data from multiple backscattered electron images acquired at different specimen geometries to (1) better reveal grain boundaries in recrystallized microstructures and (2) distinguish between recrystallized and unrecrystallized regions in partially recrystallized microstructures. The second utilizes spherical harmonic transform indexing of electron backscatter diffraction patterns to produce high angular resolution orientation data that enable the characterization of subgrains. Subgrains are produced during high-temperature plastic deformation and have boundary misorientation angles ranging from a few degrees down to a few hundredths of a degree. Here, we also present an algorithm to automatically segment grains from combined backscattered electron image data or grains and subgrains from high angular resolution electron backscatter diffraction data. Together, these new techniques enable rapid measurements of individual grains and subgrains from large populations.

36 MATERIALS SCIENCE↗
DOE OSTI2026

Validation of electron backscattering in the MCNP6.3 code

A new electron backscattering validation suite has been developed for the MCNP® code. The calculations in this suite cover both condensed history and single-event transport methods, seven different elemental materials ranging from beryllium to uranium, and incident electron energies from 200 eV to 14.1 MeV. In general, the accuracy of the MCNP code for electron backscattering calculations is energy-dependent. For incident electron energies below 2 keV, the condensed history method is not applied while the single-event method shows poor agreement with experimental measurements due to poor accuracy of the underlying atomic data. For incident energies between 2 keV and 256 keV, the single-event method typically shows better agreement with experiments, while for incident energies above 256 keV the condensed history method gives better accuracy. Additionally, agreement with experimental data is generally worse for low- Z materials such as beryllium and carbon, which may reflect deficiencies in the data or physics underlying electron transport through light elements in the MCNP code. The new electron backscattering validation suite, along with the previously introduced electron stopping power and Lockwood energy deposition validation suites, provide MCNP users with a quantified understanding of the uncertainties in electron transport calculations. Future improvements to electron transport in the MCNP code are necessary for low energies (≤ 2 keV) and for low- Z materials.

36 MATERIALS SCIENCE↗
DOE OSTI2025

Modeling and Characterizing the electron backscatter in a cylindrical anode-based distributed X-ray source

Upcoming advancements in computed tomography architectures warrants the investigation of new X-ray source designs and the impacts that electron backscatter can have on these designs. One such design being investigated is a distributed, cylindrical anode-based X-ray source. For such a distributed X-ray source, we developed a modeling pipeline for simulating electron optics and transport to characterize the quality of the primary X-ray beam and the electron backscatter behavior. We report our results on the energy distributions of the bremsstrahlung spectra; electron backscatter ratio; and spatial, temporal, and energy distributions of backscattered electrons that return to the anode.

46 - INSTRUMENTATION RELATED TO NUCLEAR SCIENCE AN↗
NASA NTRS1973

Examination of oxide scales in the SEM using backscattered electron images

The complementary use of the scanning electron microscope in the backscattered electron mode with the more usual secondary electron mode results in a significant increase in the versatility of the instrument, since regions of different chemical composition can be readily detected, and their morphology examined. The use of this technique to examine complex oxide scales formed on heat-resistant alloys is described, and in particular the location of thoria particles in the scale formed on a Ni-20 wt pct Cr-2.3 wt pct ThO2 alloy, and the examination of the behavior of yttrium during the high-temperature oxidation of a Co-Cr-Al-Y alloy are discussed.

Price, C. W.↗
DOE OSTI2023

A Denoising Autoencoder for Improved Kikuchi Pattern Quality and Indexing in Electron Backscatter Diffraction

The rapid collection and indexing of electron diffraction patterns as produced via electron backscatter diffraction (EBSD) has enabled crystallographic orientation and structural determination, as well as additional property-determining strain and dislocation density information with increasing speed, resolution, and efficiency. Pattern indexing quality is reliant on the noise of the collected electron diffraction patterns, which is often convoluted by sample preparation and data collection parameters. EBSD acquisition is sensitive to many factors and thus can result in low confidence index (CI), poor image quality (IQ), and improper minimization of fit, which can result in noisy datasets and misrepresent the microstructure. In an attempt to enable both higher speed EBSD data collection and enable greater orientation fit accuracy with noisy datasets, an image denoising autoencoder was implemented to improve pattern quality. Here, we show that EBSD data processed through the autoencoder results in a higher CI, IQ, and a more accurate degree of fit. In addition, using denoised datasets in HR-EBSD cross correlative strain analysis can result in reduced phantom strain from erroneous calculations due to the increased indexing accuracy and improved correspondence between collected and simulated patterns.

36 MATERIALS SCIENCE↗
DOE OSTI2022

Implications of gnomonic distortion on electron backscatter diffraction and transmission Kikuchi diffraction

The effect of gnomonic distortion on orientation indexing of electron backscatter diffraction patterns is explored through simulation of electron diffraction patterns for sample-to-detector geometries associated with transmission Kikuchi diffraction (TKD) and electron backscatter diffraction (EBSD). Simulated data were analysed by computing a similarity index for both Hough transformed data and simulated patterns to determine the sensitivity of each method for detecting subtle differences in the effect of gnomonic distortions on electron diffraction patterns. These results indicate that the increased gnomonic distortions in electron diffraction patterns for a TKD geometry enhance the sensitivity for detecting subtle differences in interband angles. Additionally, the utilisation of a Hough transform-based indexing approach further enhances the sensitivity.

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↗
NASA NTRS1983

Mudrocks examined by backscattered electron microscopy

A method of studying mudrocks is developed using backscattered electrons (BSE) in scanning electron microscopy. Commercially available detectors are utilized to mix the BSE and secondary electron signals in order to obtain the optimum image for a particular material. Thin sections or polished rock chip surfaces are examined with BSE which provides both the atomic number contrast and topographic contrast. This technique provides very detailed information about the form and composition of individual grains in the mudrock thin sections and can be used in studies of the source, mode of deposition, diagenesis, and tectonic deformational history of mudrocks.

Pye, K.↗
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 OSTI2022

Refinements for Bragg coherent X-ray diffraction imaging: electron backscatter diffraction alignment and strain field computation

Bragg coherent X-ray diffraction imaging (BCDI) allows the 3D measurement of lattice strain along the scattering vector for specific microcrystals. If at least three linearly independent reflections are measured, the 3D variation of the full lattice strain tensor within the microcrystal can be recovered. However, this requires knowledge of the crystal orientation, which is typically attained via estimates based on crystal geometry or synchrotron microbeam Laue diffraction measurements. Presented here is an alternative method to determine the crystal orientation for BCDI measurements using electron backscatter diffraction (EBSD) to align Fe–Ni and Co–Fe alloy microcrystals on three different substrates. The orientation matrix is calculated from EBSD Euler angles and compared with the orientation determined using microbeam Laue diffraction. The average angular mismatch between the orientation matrices is less than ∼6°, which is reasonable for the search for Bragg reflections. The use of an orientation matrix derived from EBSD is demonstrated to align and measure five reflections for a single Fe–Ni microcrystal via multi-reflection BCDI. Using this data set, a refined strain field computation based on the gradient of the complex exponential of the phase is developed. This approach is shown to increase accuracy, especially in the presence of dislocations. The results demonstrate the feasibility of using EBSD to pre-align BCDI samples and the application of more efficient approaches to determine the full lattice strain tensor with greater accuracy.

42 ENGINEERING↗
NASA NTRS2011

Metallographic Preparation of Space Shuttle Reaction Control System Thruster Electron Beam Welds for Electron Backscatter Diffraction

A Space Shuttle Reaction Control System (RCS) thruster failed during a firing test at the NASA White Sands Test Facility (WSTF), Las Cruces, New Mexico. The firing test was being conducted to investigate a previous electrical malfunction. A number of cracks were found associated with the fuel closure plate/injector assembly (Fig 1). The firing test failure generated a flight constraint to the launch of STS-133. A team comprised of several NASA centers and other research institutes was assembled to investigate and determine the root cause of the failure. The JSC Materials Evaluation Laboratory was asked to compare and characterize the outboard circumferential electron beam (EB) weld between the fuel closure plate (Titanium 6Al-4V) and the injector (Niobium C-103 alloy) of four different RCS thrusters, including the failed RCS thruster. Several metallographic challenges in grinding/polishing, and particularly in etching were encountered because of the differences in hardness, ductility, and chemical resistance between the two alloys and the bimetallic weld. Segments from each thruster were sectioned from the outboard weld. The segments were hot-compression mounted using a conductive, carbon-filled epoxy. A grinding/polishing procedure for titanium alloys was used [1]. This procedure worked well on the titanium; but a thin, disturbed layer was visible on the niobium surface by means of polarized light. Once polished, each sample was micrographed using bright field, differential interference contrast optical microscopy, and scanning electron microscopy (SEM) using a backscatter electron (BSE) detector. No typical weld anomalies were observed in any of the cross sections. However, areas of large atomic contrast were clearly visible in the weld nugget, particularly along fusion line interfaces between the titanium and the niobium. This prompted the need to better understand the chemistry and microstructure of the weld (Fig 2). Energy Dispersive X-Ray Spectroscopy (EDS) was used to confirm the chemical composition of the variations in contrast in these areas. Niobium alloys generally require exposure to more aggressive chemical reagents than titanium alloys for etching because of niobium s chemical resistance; therefore, the titanium portion of the sample was etched first. A five second immersion in Kroll s reagent revealed a general microstructure on the titanium portion of the sample; however, the titanium heat affected zone closest to the weld, was over-etched due to higher concentrations of refined grains and an increase in eta-phase. The Kroll s etchant also revealed some microstructure in the weld nugget itself; the niobium portion of the sample remained unetched.

Martinez, James↗
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 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↗