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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 595 records · Page 33
All sourcesNASA NTRSDOE OSTI
DOE OSTI2024

Characterization and Rationalization of Microstructural Evolution in GRCop-84 Processed by Laser-Powder Bed Fusion (L-PBF)

In this study, prismatic geometries of GRCop-84 [Cu-8Cr-4Nb (at. pct)] were built with laser-powder bed fusion (L-PBF) process. The samples were sectioned parallel or perpendicular to the build direction and characterized in the as-built and after post-processing with a hot-isostatically pressing (HIP) treatment. The microstructure and phase evolutions were evaluated with optical microscopy, scanning electron microscopy (SEM), electron backscattered diffraction (EBSD), and high-temperature X-ray diffraction (HTXRD) up to 1223 K. The samples in the as-built conditions exhibited predominantly columnar epitaxial and misoriented Cu-FCC grains. The microstructure evolutions are discussed based on locations within the overall build geometry, the dynamics of small melt pool shape and sectioning effects. The above grain structure did not change significantly during post-process HIP treatment. The stability of this FCC grain structure is attributed to the formation of primary stable Cr 2 Nb (Laves phase) during L-PBF, even before the emergence of FCC grains from liquid. The stability of Cr 2 Nb in both as-built and HIPed samples were evaluated using high-temperature X-ray diffraction measurements and compared with that of gas-atomized powder. The significance of these results is discussed with reference to aerospace applications.

36 MATERIALS SCIENCE↗
DOE OSTI2018

Microstructure of Friction Stir Welded AlSi9Mg Cast with 5083 and 2017A Wrought Aluminum Alloys

Wrought aluminum alloys 5083 and 2017A were each joined with cast aluminum alloy AlSi9Mg through friction stir welding in butt weld configurations. For each material system, the wrought and cast alloy positions, i.e., the advancing side or the retreating side, were exchanged between welding trials. The produced weldments were free from cracks and discontinuities. For each alloy configuration, a well-defined nugget comprised of alternating bands of the welded alloys characterized the microstructure. The degree of mixing, however, strongly depended on which wrought alloy was present and on its position during processing. In all cases, the cast AlSi9Mg alloy dominated the weld center regardless of its position during welding. Electron backscattered diffraction analysis showed that the grain size in both alloys (bands) constituting the nugget was similar and that the majority of grain boundaries exhibited a high angle character (20°-60°). Regardless of the alloy, however, all grains were elongated along the direction of the material plastic flow during welding. A numerical simulation of the joining process visualized the material flow patterns and temperature distribution and helped to rationalize the microstructural observations. The hardness profiles across the weld reflected the microstructure formed during welding and correlated well with the temperature changes predicted by the numerical model. Tensile specimens consistently fractured in the cast alloy near the weld nugget.

36 MATERIALS SCIENCE↗
DOE OSTI2019

Effect of Preheating and Water Cooling on the Performance of Friction-Stir-Welded Aviation-Grade Aluminum Alloy Joints

This paper examined the effect of preheating and water cooling on the thermal, mechanical, metallurgical, and texture properties of friction-stir-welded AA6082. Joints are fabricated under different preheating (FSW-P) and water cooling (FSW-C) conditions. The experimental outcomes indicate that the preheating and water cooling enhance the mechanical properties of the joint. The maximum tensile strength of 295 MPa is obtained for FSW-P1. It is also observed that preheating has more impact on microhardness. Microstructural analysis using optical microscope and electron backscatter diffraction analysis indicated that FSW produced fine equiaxed grains in the nugget zone due to dynamic recrystallization. Texture analysis shows that finer grain grains are obtained under preheating and water cooling conditions. The minimum grain size of 5.3 µm is obtained under FSW-P1. X-ray diffraction analysis shows that Mg{sub 2}Si phase in nugget zone that is an indication of dissolution and formation of strengthening precipitates. Fracture analysis indicates that preheating also improves the ductility of the joint.

36 MATERIALS SCIENCE↗
DOE OSTI2016

Texture Evolution During Laser Direct Metal Deposition of Ti-6Al-4V

Titanium alloys are used in a wide variety of high performance applications and hence the processing of the titanium and the resulting microstructures after additive manufacturing has received significant attention. During additive manufacturing the processing route involves the transition from a liquid to solid state. The addition of successive layers results in a complex microstructure due to solid-state transformations. The current study focuses on understanding the phase transformations and relate it to the transformation texture in Ti-6Al-4V to identify conditions leading to a strong alpha transformation texture. The as deposited builds were characterized using optical microscopy and electron backscattered diffraction. The results showed columnar prior β grains with a martensitic structure after the deposition of a single layer. On subsequent depositions the martensitic microstructure decomposes to a colony and basketweave microstructure with a stronger transformation texture. The alpha texture with a colony and basketweave microstructure shows a stronger transformation texture as a result of variant selection. Thus by controlling the cooling rate of the build from the β transus it is possible to control the alpha transformation texture.

36 MATERIALS SCIENCE↗
DOE OSTI2025

Microstructural Evolution of Steel During Magnetic Field-Assisted Processing

Advancing magnetic field-assisted processing, as an energy-efficient method for tailoring steel microstructures, requires a thorough understanding of how the high magnetic field impacts microstructural evolution, particularly its effect on prior austenite grain structures. The current investigation of a near-eutectoid composition, Fe-C alloy, uses electron backscatter diffraction to examine the morphology and orientation of martensite and pearlite microstructures, and to reconstruct the parent austenite microstructures present during equivalent heating under varied magnetic field strengths (0-T, 2-T, 5-T, and 9-T). It was observed that the magnetic field has a negligible effect on martensite lath/block width, slightly decreases prior austenite grain size, and increases the fraction of austenite grains with annealing twins. Additionally, the magnetic field increases the phase fraction of proeutectoid ferrite but has a negligible effect on pearlite block size and the distribution of boundary misorientation angles. No preferred texture was induced by the magnetic field, regardless of the applied field direction, in the proeutectoid ferrite phase or the martensite and prior austenite microstructures. Furthermore, the observed results contradict previous literature, and the differences are discussed.

Magnetic Materials↗
DOE OSTI2025

Corrosion Response of Ni-19Cr-5Fe in Molten NaCl-MgCl 2 Salt

Ni-based alloys are strong candidates for use in high-temperature molten salt reactors due to their superior corrosion resistance and mechanical stability compared to stainless steels. In this study, the static corrosion behavior of a Ni-19Cr-5Fe model alloy was systematically evaluated in a purified molten NaCl-MgCl 2 salt at 700°C for 30, 240, and 500 h. Post-exposure analyses were conducted to assess microstructural evolution, corrosion depth, and elemental depletion profiles. Corrosion rates, quantified by chromium depletion depth, followed an inverse power-law trend with increasing exposure time, indicating diffusion-limited kinetics. This trend is attributed to limitations in mass transport in the static salt and to the progressive local depletion of reactive chromium species. Coupled electron backscatter diffraction and energy dispersive X-ray spectroscopy analysis further revealed that the grain boundary character significantly influences corrosion susceptibility: high-angle grain boundaries exhibited pronounced Cr depletion and pitting, while low-angle and Σ3 boundaries remained comparatively resistant. These results offer valuable insight into the role of microstructure in corrosion processes and reinforce the importance of time-dependent material evaluation in molten salt environments relevant to advanced reactor designs.

11 - NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗
DOE OSTI2024

Automated Grain Boundary (GB) Segmentation and Microstructural Analysis in 347H Stainless Steel Using Deep Learning and Multimodal Microscopy

Austenitic 347H stainless steel offers superior mechanical properties and corrosion resistance required for extreme operating conditions such as high temperature. The change in microstructure due to composition and process variations is expected to impact material properties. Identifying microstructural features such as grain boundaries thus becomes an important task in the process-microstructure-properties loop. Applying convolutional neural network (CNN)-based deep learning models is a powerful technique to detect features from material micrographs in an automated manner. In contrast to microstructural classification, supervised CNN models for segmentation tasks require pixel-wise annotation labels. However, manual labeling of the images for the segmentation task poses a major bottleneck for generating training data and labels in a reliable and reproducible way within a reasonable timeframe. Microstructural characterization especially needs to be expedited for faster material discovery by changing alloy compositions. Here, in this study, we attempt to overcome such limitations by utilizing multimodal microscopy to generate labels directly instead of manual labeling. We combine scanning electron microscopy images of 347H stainless steel as training data and electron backscatter diffraction micrographs as pixel-wise labels for grain boundary detection as a semantic segmentation task. The viability of our method is evaluated by considering a set of deep CNN architectures. We demonstrate that despite producing instrumentation drift during data collection between two modes of microscopy, this method performs comparably to similar segmentation tasks that used manual labeling. Additionally, we find that naïve pixel-wise segmentation results in small gaps and missing boundaries in the predicted grain boundary map. By incorporating topological information during model training, the connectivity of the grain boundary network and segmentation performance is improved. Finally, our approach is validated by accurate computation on downstream tasks of predicting the underlying grain morphology distributions which are the ultimate quantities of interest for microstructural characterization.

36 MATERIALS SCIENCE↗
DOE OSTI2024

Location-Specific Microstructure Characterization Within AM Bench 2022 Nickel Alloy 718 3D Builds

Abstract The Additive Manufacturing Benchmark Test Series (AM Bench) is a broad effort to produce rigorous measurement datasets for validating AM computer simulations across the range of processing, structure, and properties, for many additive manufacturing (AM) build methods and material classes. Here, the microstructures of nickel alloy 718 AM Bench 2022 test artifacts produced using laser-based powder bed fusion (PBF-LB), in both as-built and fully heat-treated conditions, are examined. Cross sections are primarily characterized using large area scanning electron microscopy (SEM) electron backscatter diffraction (EBSD) and example analyses of the crystallographic textures are described. These data are part of a large set of in situ and ex situ measurements from both three-dimensional builds and laser tracks on bare plates. All the measurement data are available online with download links at www.nist.gov/ambench .

Levine, L. E. (ORCID:0000000334484229)↗
DOE OSTI2015

Friction Stir Welding of ODS and RAFM Steels

Advanced structural materials such as oxide dispersion strengthened steels and reduced-activation ferritic/martensitic steels are desired in fusion reactors as primary candidate materials for first wall and blanket structures, due to their excellent radiation and high-temperature creep resistance. However, their poor fusion weldability has been the major technical challenge limiting practical applications. For this reason, solid-state friction stir welding (FSW) has been considered for such applications. In this paper, the effect of FSW parameters on joining similar and dissimilar advanced structural steels was investigated. Scanning electron microscopy and electron backscatter diffraction methods were used to reveal the effects of FSW on grain size, micro-texture distribution, and phase stability. Hardness mapping was performed to evaluate mechanical properties. Finally, post weld heat treatment was also performed to tailor the microstructure in the welds in order to match the weld zone mechanical properties to the base material.

36 MATERIALS SCIENCE↗
DOE OSTI2015

Correlations Between Spall Damage Mode Preference and Microstructure in Shocked Polycrystalline Copper: A 3-D X-Ray Tomography Study

Nondestructive characterization techniques are essential for maximizing the amount of high fidelity data obtained from post mortem mechanically tested materials, particularly for the complex experimental techniques used for shock loading. Polycrystalline copper samples of varying thermomechanical histories were shock loaded to induce incipient spall damage conditions via plate impacts at low pressures. Electron backscattering diffraction (EBSD) and 3-D X-ray tomography (XRT) were utilized to obtain microstructural and void volume data, respectively. Voids were fit to ellipsoids using their inertia tensors obtained from the 3-D XRT data, and the results compared to EBSD data. This, in turn, enabled establishing quantitative correlations between void shapes and preferential damage mode, either inter- or trans-granular, for each thermomechanical history. Greater than 60 % of voids present in heat-treated samples were spherical, indicative of transgranular damage preference. Greater than 90 % of voids present in as-received rolled samples were flat sheetlike voids or unsymmetrical oblate ellipsoids, indicative of intergranular and coalesced damage modes. Analyzing grain boundary damage statistics in conjunction with global damage mode distributions indicate that boundaries become less dominant as preferential void nucleation sites within the spall plane as the bulk strength of the material decreases from heat treatments.

Microstructure↗
DOE OSTI2014

Effect of tungsten crystallographic orientation on He-ion-induced surface morphology changes

In order to study the early stages of nanofuzz growth in fusion-plasma-facing tungsten, mirror-polished high-purity tungsten was exposed to 80 eV helium at 1130 C to a fluence of 4 1024 He/m2. The previously smooth surface shows morphology changes, and grains form one of four qualitatively different morphologies: smooth, wavy, pyramidal, or terraced/wide waves. Combining high-resolution scanning electron microscopy (SEM) observations to determine the morphology of each grain with quantitative measurement of the grain's orientation via electron backscatter diffraction (EBSD) in SEM shows that the normal-direction crystallographic orientation of the underlying grain controls the growth morphology. Specifically, near-<001> || normal direction (ND) grains formed pyramids, near-<114> to <112> || ND grains formed wavy and stepped structures, and near-<103> || ND grains remained smooth. Comparisons to control specimens indicate no changes to underlying bulk crystallographic texture, and the effects are attributed to surface energy anisotropy, although, surprisingly, the expected {101} low-energy planes were not the most stable. Future developments to control tungsten texture via thermomechanical processing, ideally obtaining a sharp near- <103> || ND processing texture, may delay the formation of nanofuzz.

Parish, Chad M↗
DOE OSTI2015

Texture enhancement during grain growth of magnesium alloy AZ31B

In this paper, the microstructure and texture evolution during annealing of rolled Mg alloy AZ31B, at temperatures ranging from 260 to 450°C, is characterized, and a grain growth exponent of n=5, indicating inhibition of grain growth, is observed. Broadening of the normalized grain size distributions, which indicates abnormal grain growth, was observed at all temperatures investigated. It is shown, using a Zener-type analysis for pinning of grain boundaries by particles, that impurity-based particles are responsible for grain growth inhibition and abnormal grain growth. The strong basal texture which develops during rolling of the Mg alloy, resulting in an initial peak intensity in the (0002) pole figure of nine multiples of a random distribution (MRD), increases to ~15 MRD during annealing at 400 and 450°C. Furthermore, a specific texture component {0001}(1120) is observed in the orientation distribution, which increases from 10 to 23 MRD at 400°C. It is hypothesized that the anisotropic grain boundary properties (i.e. low angle boundaries have low energy and mobility) are responsible for the texture strengthening. Additionally, electron backscattered diffraction reveals the recrystallized microstructure to contain a significant number of boundaries with ~30° misorientation about the <0001> direction, and this boundary type persists throughout most annealing treatments explored.

36 MATERIALS SCIENCE↗
DOE OSTI2017

Structure/property (constitutive and spallation response) of additively manufactured 316L stainless steel

For additive manufacturing (AM) of metallic materials, the certification and qualification paradigm needs to evolve as there is currently no broadly accepted “ASTM- or DIN-type” additive manufacturing certification process or AM-produced material specifications. Accordingly, design, manufacture, and subsequent implementation and insertion of AM materials to meet engineering applications requires detailed quantification of the constitutive (strength and damage) properties of these evolving materials, across the spectrum of metallic AM methods, in comparison/contrast to conventionally-manufactured metals and alloys. For this paper, cylindrical samples of 316L SS were produced using a LENS MR-7 laser additive manufacturing system from Optomec (Albuquerque, NM) equipped with a 1 kW Yb-fiber laser. The microstructure of the AM-316L SS was characterized in both the “as-built” AM state and following a heat-treatment designed to obtain full recrystallization to facilitate comparison with annealed wrought 316L SS. The constitutive behavior as a function of strain rate and temperature was characterized and is compared to that of annealed wrought 316L SS plate material. The dynamic shock-loading-induced damage evolution and failure response of all three 316L SS materials was quantified using flyer-plate impact driven spallation experiments at peak stresses of 4.7 and 6.5 GPa. The spall strength of AM-produced 316L SS and the recrystallized-AM-316L SS were found to decrease with increasing peak shock stress while the annealed wrought 316L SS spall strength remained essentially constant. Finally, the damage evolution, characterized using optical metallography and electron-backscatter diffraction (EBSD), was found to vary significantly across the three 316L SS microstructures while the three samples loaded to a peak shock stress of 6.5 GPa displayed only ~12% differences in spall strength.

316L SS↗
DOE OSTI2018

Enhanced high-temperature tensile property by gradient twin structure of duplex high-Nb-containing TiAl alloy

A pre-deformation process was employed for a TiAl alloy via high-temperature torsion, in which the stability of the constituent phases was tailored, resulting in enhanced hardening capability and ductility via a gradient microstructure. A sample with a pre-torsion of 360° exhibited a yield strength of 475 MPa and an ultimate tensile strength of 592 MPa, with a tensile ductility of 47% at 850 °C. The tensile properties were significantly enhanced compared with the as-forged sample, which exhibited values of 395 MPa, 494 MPa, and 4.6%, respectively. The physical mechanisms for the significant enhancement of the mechanical property of the TiAl alloys were studied in-depth via of transmission electron microscopy, electron-backscattered diffraction, and high-energy X-ray diffraction techniques. The high strength is mainly attributed to the twin structure formed during torsion, while high fracture elongation correlates to the recrystallization of the γ phase at twin-twin sections and the load partitioning regulated by a hierarchical microstructure. When the tensile micro-strains along the loading direction and transverse direction in the γ phase of the pre-deformed TiAl alloy, a higher mechanical performance was obtained. Moreover, the fracture mode of the pre-torsional tensile sample is a combination of pores and cleavage facets which resulted from the microstructure after torsion. Finally, the gradient twin structure approach in this study provides a strategy for developing TiAl alloys with exceptionally high-temperature tensile property, and the results of the micromechanical behavior-microstructure-property relationship may improve the understanding of the plastic deformation of TiAl alloys.

36 MATERIALS SCIENCE↗
DOE OSTI2018

Steps and { 11 2 ¯ 1 } secondary twinning associated with { 11 2 ¯ 2 } twin in titanium

{$11\overline{2}2$} twinning commonly takes place in α-titanium (α-Ti). High-resolution transmission electron microscopies (HRTEM) explored various steps along {$11\overline{2}2$} coherent twin boundary. Topological model of {$11\overline{2}2$} twin revealed twinning disconnections (TDs) that are represented by ( b i , i h {$11\overline{2}2$} ) corresponding to a step height i h {$11\overline{2}2$} and a shear vector b i . Atomistic simulations were conducted to study the energies and kinetics of TDs. Combining microscopies and atomistic simulations, we concluded that ( b 3 , 3 h {$11\overline{2}2$} ) is the elementary TD and ( b 1 , h {$11\overline{2}2$} ) is the reassemble TD. Steps observed in HRTEM thus can be treated as a reassembly of ( b 3 , 3 h {$11\overline{2}2$} ) TDs and ( b 1 , h {$11\overline{2}2$} ) TDs. In addition, Electron Backscatter Diffraction (EBSD) maps revealed {$11\overline{2}2$} → {$11\overline{2}1$} double twins in α-Ti. Using two-dimensional and three-dimensional atomistic simulations, we demonstrated the nucleation of ( b 1 , h {$11\overline{2}2$} ) TD and {$11\overline{2}2$} → {$11\overline{2}1$} double twin through the interaction between basal $\langle$$a$$\rangle$ dislocation and {$11\overline{2}2$} twin. In conclusion, our results enrich the understanding of {$11\overline{2}2$} twinning including TDs, steps, and {$11\overline{2}1$} secondary twins in hexagonal metals.

36 MATERIALS SCIENCE↗
DOE OSTI2020

Modeling the role of local crystallographic correlations in microstructures of Ti-6Al-4V using a correlated structure visco-plastic self-consistent polycrystal plasticity formulation

This paper presents a multi-level crystal plasticity-based simulation framework for modeling mechanical response and microstructure evolution of Ti-6Al-4V with α-lath/lamellar microstructures. Here, the model is a correlated structure visco-plastic self-consistent (CS-VPSC) formulation linking three scales: a single crystals micro-scale, a lath/lamellar colony meso-scale, and a lath/lamellar aggregate macro-scale. A selected hardening law for the evolution of critical resolved shear stress per slip system used in CS-VPSC is phenomenological. However, it adjusts the resistances of basal and prismatic slip systems based on the geometry of slip transfer between adjacent lamellae. Consistent with experimental evidences, the resolved shear stress on the pyramidal slip planes is dependent not only on the stress in the direction of slip but also on the two orthogonal shear stress components and the three normal stress components (non-Schmid effects). Electron backscatter diffraction (EBSD) data in conjunction with a procedure relying on α→β phase transformation is used to construct paired variants of α-laths/lamellae satisfying their local crystallographic correlations. The procedure fits volume fractions of individual laths/lamellae with the experimental EBSD data and selects a distribution of habit planes between adjacent variants with respect to the loading direction. The simulation framework is applied to interpret the deformation behavior in tension and compression along two sample directions of Ti-6Al-4V fabricated via laser powder bed fusion. Moreover, the model is used to simulate texture evolution during rolling of the material to large strains. It is demonstrated that the model is capable of predicting plastic anisotropy/asymmetry and the concomitant texture evolution. While the model reveals a significant effect of habit plane inclination with respect to the loading direction on yield stress, the comparison of the data and model predictions shows that a random distribution of habit planes fits the flow response. It is further inferred that the tension-compression asymmetry arises from the non-Schmid effects.

36 MATERIALS SCIENCE↗
DOE OSTI2022

Origin, parameters, and underlying deformation mechanisms of propagating deformation bands in irradiated 316L stainless steel

Lüders-type propagating deformation bands were observed in specimens of irradiated 316L stainless steel samples removed from Spallation Neutron Source target vessels after service. Mechanical testing with digital image correlation (DIC) and in-situ tensile testing with scanning electron microscopy electron backscatter diffraction showed that the observed Lüders-type behavior was not related to the known transformation-induced plasticity or twinning-induced plasticity behavior. Instead, the phenomenon occurs at small local strain values before a significant amount of martensite or deformation twins appear in the microstructure. Microstructural analysis and in-situ mechanical test results suggest Lüders-type band formation and propagation were related to the appearance and evolution of defect-free channels—analogous to slip bands. A modified Swift equation with a Ludwigson-like component was offered to rationalize the phenomenon and model the strain-softening processes at small strain values. Finally, the results indicate complex microstructural processes and deformation mechanisms were active at small strain values and underline the benefits of advanced mechanical test approaches such as DIC.

36 MATERIALS SCIENCE↗