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Results for “Electron backscatter diffraction”

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 37 records · Page 2
All sourcesNASA NTRSDOE OSTI
DOE OSTI2025

Microstructural, Oxidation, and Mechanical Behavior of NbTi-Based Refractory Alloys with 5 to 10 Pct Co, Cr, and Ni Additions

NbTi-based refractory alloys with additions of Co, Cr, and Ni represent an interesting medium-entropy alloy system with potential for protective oxide film formation, high strength, and ductility. This study investigates the microstructural evolution, oxidation behavior, and mechanical properties of NbTi-based alloys containing 5 to 10 at. pct Co, Cr, and Ni. CALPHAD predictions suggest that this composition range can be heat treated to obtain a predominantly body-centered cubic matrix phase. Mechanical properties, including microhardness, yield strength, maximum strength, and specific strength are evaluated through isothermal compression tests conducted between room temperature and 800 °C. The oxidation kinetics of these alloys are assessed through discontinuous oxidation tests. Parabolic oxidation kinetics were observed for NbTi–10Ni and NbTi–5Co, while linear oxidation kinetics were found for NbTi–10Cr and NbTi–10(CoCrNi). Microstructures and oxide layers are characterized using X-ray diffraction, electron backscatter diffraction, energy-dispersive X-ray spectroscopy, and scanning electron microscopy. All alloys exhibit significant mechanical softening between room temperature and 800 °C, with elastic-perfectly plastic flow observed at 800 °C. The addition of 10 pct Cr to NbTi resulted in two BCC phases up to 1050 °C, conflicting with CALPHAD predictions of a single-phase solid solution at this temperature, and resulting in higher flow stress at 800 °C. NbTi–10(CoCrNi) exhibited the lowest flow stress at 800 °C despite having more ‘cocktail effect’ potential and insufficient molar fractions of Co, Cr, or Ni to form a desirable protective oxide film.

36 MATERIALS SCIENCE↗
DOE OSTI2023

Rapid grain refinement and compositional homogenization in a cast binary Cu50Ni alloy achieved by friction stir processing

Friction stir processing (FSP) has been increasingly adopted for joining and processing materials in automotive, aerospace and industrial construction. During FSP a dynamic competition between high-speed shear deformation and deformation-induced heating brings about a complex competition between multiple dynamic microstructural evolution mechanisms making it difficult to predict the microstructural evolution pathway. Hence, improved understanding of microstructural evolution mechanisms during FSP can be beneficial for continued growth in the adoption of FSP for demanding applications of future. Towards this goal, this study uses a model binary Cu – 50 at.% Ni alloy to clarify the effect of single and double pass FSP on the microstructural evolution of a coarse grained and compositionally heterogeneous cast microstructure. High energy synchrotron X-ray diffraction, electron backscatter diffraction, and nanoindentation are used to clarify the microstructural evolution due to FSP. The process of compositional homogenization of as-cast segregations is studied by energy dispersive spectroscopy and atom probe tomography. Our results show that a single fast FSP pass at 30 mm.s -1 produces a 100 µm deep layer of submicrometric and hall-petch hardened CuNi grains. The initial cast compositional heterogeneities in a micrometric scale is rapidly transformed to nano-sized domains, mainly confined at grain boundaries. Double pass FSP increases the penetration depth of the processed layer and leads to a 2.9 times grain growth relative to single pass FSP. Grain fragmentation, discontinuous dynamic recrystallization, grain growth, and twinning mechanisms are discussed. In conclusion, these results highlight the value of FSP for ultrafast grain refinement and compositional homogenization of cast alloys.

36 MATERIALS SCIENCE↗
DOE OSTI2025

The Measurement of Grain Size by Electron Beam Backscattered Diffraction

The method of electron back-scatter diffraction provides an analytic means to identify crystalline phase and the grain size of structural materials. The need to utilize imaging parameters consistent with revealing the contributing microstructural scale is often overlooked through packaged imaging scripts. It is shown that imaging parameters consistent with a post processing assessment of low misorientation angles between boundaries are achievable as using pixel sizes on the order of 10 1 nm.

36 MATERIALS SCIENCE↗
DOE OSTI2022

Critical differences between electron beam melted and selective laser melted Ti-6Al-4 V

Effective optimization of the production of Ti-6Al-4 V using AM requires a fundamental understanding of the relative importance of different microstructural features to the deformation and failure mechanisms, particularly features that vary between production methods. In this study, the tensile response and deformation mechanisms of electron beam melted (EBM) AM Ti-6Al-4 V material loaded in different orientations and produced using various powder sizes were compared to those of selective laser melted (SLM) AM Ti-6Al-4 V material. The density and morphology of pores, phase fractions, prior-β grains, and defect microstructures were evaluated using scanning electron microscopy, X-ray computed tomography, electron backscatter diffraction, and transmission electron microscopy before and after deformation. The results were used to evaluate the relative importance of each feature on strengthening, deformation, and failure initiation mechanisms. Results focused primarily on coarse-powder EBM materials indicated that phase distribution and defect density were most influential for determining material yield strength as well as maximum possible strain to failure. Porosity was lower overall in EBM Ti-6Al-4 V than in SLM, allowing for occasional increases in part strain to failure, but remained a limiting factor determining overall part ductility.

36 MATERIALS SCIENCE↗
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 OSTI2025

Microstructure characteristics of LPBF&HIP fabricated graded composite transition joint between ferritic steel and austenitic stainless steel

Graded composite transition joints (GCTJs) offer a promising alternative to conventional dissimilar metal welds (DMWs) by enabling smooth compositional and microstructural transitions. However, GCTJs fabricated solely through additive manufacturing (AM) face challenges such as heat accumulation, complex parameter control, and elemental segregation. In this study, we propose a novel approach that relies on AM to design a spatially graded structure in one alloy and then employs hot isostatic pressing (HIP) as a diffusion bonding method to join it with a second alloy. Here, this method combines the flexibility of AM with the powder net-shaping advantage of HIP. Specifically, a series of closely packed austenitic stainless steel 304 conical structures were printed using laser powder bed fusion (LPBF) and then combined with ferritic steel P91 powder via HIP. By using electron backscatter diffraction (EBSD), electron probe microanalysis (EPMA), and transmission electron microscopy (TEM) techniques, the microstructure characteristics of the GCTJ of 304&P91, especially the interdiffusion zone (IDZ), have been systematically investigated. The microstructure at the interface transitions from austenite-ferrite (A+F) to austenite-martensite-ferrite (A+M+F), and finally to martensite-ferrite (M+F) due to diffusion. Additionally, the diffusion width between 304 and P91 increases with the volume fraction of P91. This unique design also ensures a gradual transition in both hardness and thermal expansion coefficient from 304 to P91, thereby enabling a smooth gradient in functional properties. Overall, this study proposes a novel approach for fabricating GCTJs and contributes to advancing design concepts in the field of dissimilar metal joining.

Additively manufacturing (AM)↗
DOE OSTI2022

Heterogenous activation of dynamic recrystallization and twinning during friction stir processing of a Cu-4Nb alloy

An interplay between high degree of shear deformation and deformation-induced heating occurs during friction stir processing (FSP) of metals. In medium-to-low stacking fault energy Cu alloys, this can lead to a complex spatially heterogenous activation of dynamic recrystallization (DRX) and twinning mechanisms. Within the Cu-Nb system, the presence of Nb is further expected to influence the DRX mechanism of the Cu matrix. However, the microstructural changes induced by the co-deformation of Nb during FSP are still not well understood. So, this study uses a combination of multimodal microstructural characterization, solution thermodynamics-based predictions, and computational crystal plasticity simulation to reveal the various microstructural evolution mechanisms that can occur during FSP of a Cu-4at.%Nb binary model alloy. The formation of softer DRX zones, and harder shear localization regions are revealed using electron backscatter diffraction, transmission electron microscopy, atom probe tomography, and crystal plasticity modeling.

36 MATERIALS SCIENCE↗
DOE OSTI2024

Microstructure Clones

Microstructure drives component behavior. Contemporary crystal plasticity studies compare strain measurements of polycrystal specimens to models. Because each specimen is unique, it is impossible to know which differences are significant. In this project, we invented microstructure clones and explored their use in understanding crystal plasticity. Microstructure clones are specimens with nearly identical microstructures, which allows for multiple destructive tests of a microstructure, insight into how a specimen will deform, variability quantification, and the ability to measure the effects of microstructural changes. Several sets of microstructure clones, pure nickel tensile bars, were tested. The techniques of digital image correlation, crystal plasticity finite element analysis, high resolution electron backscatter diffraction, transmission electron microscopy, and dislocation dynamics were used to understand the structural behavior of these microstructures. This work reshapes the fields of crystal plasticity and structure-property relationships by providing a technique to control for specific variables, quantify microstructural stochasticity, and replicate experiments.

36 MATERIALS SCIENCE↗
DOE OSTI2024

Radiation Damage Mitigation in FeCrAl Alloy at Sub-Recrystallization Temperatures

Traditional defect recovery methods rely on high-temperature annealing, often exceeding 750 °C for FeCrAl. In this study, we introduce electron wind force (EWF)-assisted annealing as an alternative approach to mitigate irradiation-induced defects at significantly lower temperatures. FeCrAl samples irradiated with 5 MeV Zr 2+ ions at a dose of 10 14 cm −2 were annealed using EWF at 250 °C for 60 s. We demonstrate a remarkable transformation in the irradiated microstructure, where significant increases in kernel average misorientation (KAM) and low-angle grain boundaries (LAGBs) typically indicate heightened defect density; the use of EWF annealing reversed these effects. X-ray diffraction (XRD) confirmed these findings, showing substantial reductions in full width at half maximum (FWHM) values and a realignment of peak positions toward their original states, indicative of stress and defect recovery. To compare the effectiveness of EWF, we also conducted traditional thermal annealing at 250 °C for 7 h, which proved less effective in defect recovery as evidenced by less pronounced improvements in XRD FWHM values.

FeCrAl alloys↗
DOE OSTI2022

Mechanical response and microstructure evolution from multiaxial stress relaxation in textured zircaloy nuclear cladding

Modern energy markets provide motivation for nuclear reactors to increase operational flexibility and load following capacity of existing reactor designs. The operational power changes result in fuel pellet expansion and contraction resulting in pellet-cladding mechanical interaction (PCMI) and high cladding stresses that are strongly related to stressed corrosion cracking (SCC) which can lead to fuel rod failure. This work aims to quantify the stress fields in cladding with a focus on multiaxial stress relaxation response from an imposed strain and the resulting microstructure changes in textured zircaloy claddings. Stress relaxation tests resulting in multiaxial stress fields are performed to measure the material response of Zircaloy-4 nuclear cladding. Multiple experiments using samples from the same piece of cladding are performed so samples with the same processing history may be removed at strategic points throughout mechanical testing for microstructure characterization. The microstructure evolution is analyzed with mechanical response to evaluate the static recovery impact on crystallographic texture and grain morphology. Experiments are performed at Idaho National Laboratory using an experimental device capable of applying internal pressure and independent axial load to commercial nuclear cladding at elevated temperatures with stress- or strain-controlled experimental capability. X-ray diffraction and electron backscatter diffraction are used for microstructure analysis. Rheological models are used to visualize the multiaxial stress-strain relationships and isolate elastic, plastic, and viscoplastic material properties for analysis.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗
DOE OSTI2023

In situ synchrotron X-ray diffraction analysis of ultrasonically assisted microstructure refinement during laser melting process

This work investigates the effect of ultrasonic treatment (UST) on the microstructure of AA4043 alloy during laser melting process. Here, the study utilizes in situ synchrotron X-ray diffraction (SXRD) and postmortem electron backscatter diffraction (EBSD) techniques to examine the ultrasonic grain refinement mechanism. The SXRD diffraction patterns exhibit higher continuity of major diffraction rings in the UST-test pattern, indicating a more refined grain structure. The presence of new diffraction spots in the post-test diffraction pattern with UST suggests the breakdown of epitaxial growth of columnar dendrites during solidification. Thermal profiles determined by analyzing the lattice parameter evolution show a faster cooling rate with UST. The inverse pole figures and aspect ratio distribution from EBSD reveal that the UST samples exhibit a refined, more equiaxed grain structure along the weld centerline. UST sample also develops more fine-sized low angle grain boundaries (LAGBs). These features offer better hot-cracking resistance in aluminum alloys.

36 MATERIALS SCIENCE↗
NASA NTRS2001

Crystallographic Texture and Orientation Variants in Al2O3-Y3Al5O12 Directionally Solidified Eutectic Crystals

Eutectic rods of Al2O3 and Y3Al5O12 were grown by a laser-heated float zone method, and their microstructure and crystallographic texture were studied by scanning electron microscopy, electron backscattered diffraction and x-ray diffraction. The composites were found to be highly textured with two twin-related crystallographic orientation relationships between the phases. Electron backscattered diffraction was employed to determine the spatial distribution of the orientational variants within the samples and to define the crystallographic orientation of various microstructural features.

Frazer, Colleen S.↗
DOE OSTI2022

Characterizing defect structures in AM steel using direct electron detection EBSD

The mechanical properties of additive and traditionally manufactured alloys are largely dependent on the characteristics and distribution of dislocation cell networks that develop during the fabrication process. This work demonstrates the ability to quantitatively characterize these dislocation structures by high angular resolution electron backscatter diffraction analysis using a direct electron detector. The defect structures are characterized in terms of the geometrically necessary dislocation density and the associated Burgers vector and line direction. Furthermore, the results are discussed in terms of potential defect formation mechanisms.

36 MATERIALS SCIENCE↗
DOE OSTI2023

Assessing Manufacturability of the Oxide Dispersion Strengthened (ODS) 14YWT Alloy Fuel Cladding Tube Using SolidStir™ Technology

The 14YWT (Fe–14Cr–3W–0.4Ti–0.3Y2O3 (wt.%)) alloy is a potential candidatematerial for fabricating fuel cladding tubes and other structural components to be used in next-generation advanced nuclear reactors. Due to inherent limitations of current processing routes, this research explored a new variant of friction stir processing, commercially referred to as SolidStir™ Extrusion (patent pending) technology from Enabled Engineering to consolidate and extrude 14YWT powder into a fuel cladding tube. Several single-layer and multiple-layer consolidation experiments were carried out in an Inconel 625 die to determine the suitable processing parameters for SolidStir™ extrusion of the 14YWT alloy cladding tube. With these processing parameters, a 16–18 mm long tube of the 14YWT alloy with no visible defects was successfully extruded using this novel technology. Microstructural characterization results obtained using optical microscopy, scanning electron microscopy, energy dispersive spectroscopy, electron backscatter diffraction, and transmission electron microscopy will be presented.

Advanced Materials and Manufacturing Technology↗
DOE OSTI2023

Material flow behavior and microstructural refinement of AA6061 alloy during friction extrusion

In this work we used friction extrusion (FE), a solid phase processing technique, to produce dense, fully consolidated 5?mm rods of aluminum alloy 6061 (AA6061). The combination of large shear stresses and high temperatures at the tool-billet interface during extrusion produced equiaxed, dynamically recrystallized grains and finely distributed precipitates. Texture and microstructure evolution during extrusion was investigated in detail using scanning electron microscopy, electron backscatter diffraction, and transmission electron microscopy. Smoothed particle hydrodynamics simulation was performed to study complex material flow during extrusion. Simulation results suggest spiral material flow during extrusion which corroborated experimental results. Advantages of friction extruded microstructure over conventionally extruded counterparts are also explored using flash annealing for solution treatment followed by artificial aging. Mechanical properties of the as-friction extruded, and the artificially aged specimens were evaluated using tensile testing and compared with conventional extruded material properties.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2023

Microstructural evolution in shear-punch tests: A comparative study of pure Cu and Cu-Cr alloy

Understanding the mechanisms behind microstructural evolution during shear deformation has been a long-standing area of interest. However, establishing a connection between microstructure, mechanical properties, and extent of shear deformation is challenging and requires refined experimental approaches. Shear-punch testing (SPT) provides a controlled method to introduce shear into small volumes of material that later can be subjected to detailed microstructural characterization. In this study, we utilize an SPT device to induce shear deformation to pure copper and a binary copper-chromium alloy. Electron backscatter diffraction and transmission electron microscopy were used to study the mechanisms of plastic deformation after SPT. Our results indicate that shear deformation of pure Cu produces a dense network of intercepting microshear bands upon sustained deformation. Twin boundaries undergo degradation into high angle grain boundaries due to simultaneous deviation from the axis-angle pair condition of 60° misorientation on [111] direction. The presence of 50% volume Cr particles in the soft Cu matrix fundamentally altered the shear deformation mechanism. Preferential deformation of the Cu matrix led to accelerated shear-induced formation of low and high angle grain boundaries, and subsequent grain refinement. Comparatively, no grain refinement occurred in pure Cu at a strain ~10 times larger (ϵ = 4.73) than that of the copper-chromium case (ϵ = 0.42). Overall, our study sheds light on the microstructural evolution during shear deformation and highlights the significant influence of particle reinforcements on the shear deformation mechanisms of metals.

36 MATERIALS SCIENCE↗
NASA NTRS2020

Mechanical twinning of monazite expels radiogenic Pb

Mechanical twins form by the simple shear of the crystal lattice during deformation In order to test the potential of narrow twins in monazite to record the timing of their formation, a ~1,700 Ma monazite grain deformed at ~980 Ma was investigated by electron backscattered diffraction (EBSD), transmission electron microscopy (TEM) and atom probe tomography (APT). APT 208Pb/232Th ages indicate that the twin was entirely reset by radiogenic Pb-loss during its formation at conditions far below the monazite closure temperature. The results are consistent with a model where Pb is liberated during rupture of REE-O bonds in the large REEO9 polyhedra during twinning. Liberated Pb is likely to migrate along fast diffusion pathways such as crystal defects. The combination of a quantitative microstructural investigation and nanogeochronology provides a new approach for understanding the history of accessory phases.

monazite↗
NASA NTRS2024

Microstructural Evolution of the Civet Cat Norite (72255)

The ‘Civet Cat Norite’ is a ~ 2.5 cm clast within the Apollo impact melt breccia sample 72255 collected during Apollo 17 EVA 2 at Boulder 1. The norite is primarily composed of plagioclase and orthopyroxene with fine-scale exsolution lamellae of augite. The plagioclase and orthopyroxene (OPX) coexist with minor quartz and augitic clinopyroxene (CPX), and accessory apatite, baddeleyite, chromite, ilmenite, loveringite, merrillite, rutile and zircon. The major minerals range from 1 to 4 mm in size and show a cataclastic texture indicated by banding of the light and dark phases]. The chemical composition of the orthopyroxene, augitic exsolution lamellae, and exsolved oxides suggest the norite crystallized in the lower crust of the Moon (10 – 70 km depth) and was subsequently excavated by impact(s). Shock pressure estimates for the norite range from 15 – 35 GPa based on maskeleynite formation within the plagioclase, kink banding in pyroxenes, and granular recrystallization in the accessory phosphates. Previous Rb-Sr and 40 Ar/ 39 Ar analyses recalculated with modern decay constants yield relatively young ages of 4.16 ± 0.05 Ga and 3.99 ± 0.03 Ga, respectively. However, recent U-Pb analyses of some zircon grains from within the Civet Cat yield an age of 4.45 ± 0.03 Ga. While this is the oldest age for any rock recovered from the Moon, the full age spread of zircon from the Civet Cat range from ca. 4.46 to 4.02 Ga, indicating variable Pb-loss and complicating interpretation of the primary age. Recent atom probe analyses indicate minimal Pb mobilization within the oldest zircon grain from Civet Cat, supporting the interpretation that these ancient zircon ages reflect the age of the norite, rather than an apparent antiquity caused by reverse discordance. To investigate the potential antiquity and deep crustal origin of the Civet Cat norite, we have undertaken high resolution microstructural analyses of the major, minor, and accessory minerals to characterize the primary igneous textures and secondary overprinting by impact and metamorphism. The employed analytical techniques include scanning electron microscope-based electron backscatter diffraction (EBSD) analyses, electron probe microanalyzer (EPMA) chemical analyses, and transmission electron microscopy (TEM) of pyroxene, plagioclase, quartz, zircon, and phosphates.

T M Erickson↗