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DOE OSTI2024

Selective laser sintering and spark plasma sintering of (Zr,Nb,Ta,Ti,W)C compositionally complex carbide ceramics

Abstract Two advanced manufacturing processes, spark plasma sintering (SPS) and selective laser sintering (SLS), have been developed for synthesis of (Zr,Nb,Ta,Ti,W)C compositionally complex carbide (CCC) via reactive sintering of a powder mixture of constitute monocarbides. X‐ray diffraction analysis confirmed that the single‐phase CCC can be formed by both SPS and SLS. While a homogenous microstructure with uniform metal element distributions was developed during SPS, three‐layer microstructures with a thin TiC‐rich layer and two TaC‐rich layers along with a TiO 2 ‐rich surface layer containing W nanoparticles were formed during SLS. In addition, cellular structures with W, Zr, and Ti element segregation and dislocations on cell boundaries were observed in the SLS‐CCC sample, indicating the effect of nonequilibrium conditions on microstructure formation during laser melting followed by rapid cooling and solidification process. Compared to the SPS‐CCC sample, the SLS‐CCC showed enhanced hardness and reduced thermal conductivity, which may be related to their unique cellular structures.

36 MATERIALS SCIENCE↗

NASA NTRS1985

Improved silicon nitride for advanced heat engines

The AiResearch Casting Company baseline silicon nitride (92 percent GTE SN-502 Si sub 3 N sub 4 plus 6 percent Y sub 2 O sub 3 plus 2 percent Al sub 2 O sub 3) was characterized with methods that included chemical analysis, oxygen content determination, electrophoresis, particle size distribution analysis, surface area determination, and analysis of the degree of agglomeration and maximum particle size of elutriated powder. Test bars were injection molded and processed through sintering at 0.68 MPa (100 psi) of nitrogen. The as-sintered test bars were evaluated by X-ray phase analysis, room and elevated temperature modulus of rupture strength, Weibull modulus, stress rupture, strength after oxidation, fracture origins, microstructure, and density from quantities of samples sufficiently large to generate statistically valid results. A series of small test matrices were conducted to study the effects and interactions of processing parameters which included raw materials, binder systems, binder removal cycles, injection molding temperatures, particle size distribution, sintering additives, and sintering cycle parameters.

Yeh, H. C.↗

NASA NTRS1989

Evaluation, development, and characterization of superconducting materials for space application

Results are reported of low magnetic field studies of dc magnetic susceptibility and ac magnetic susceptibility of bulk samples and powders. These data are analyzed and compared with the microstructures and compositions of the samples as determined by scanning electron microscopic micrographs, X-ray and chemical analysis. Particular emphasis is given to the interpretation of the ac magnetic susceptibility data which were obtained as function of the magnitude and frequency of the ac measuring field, and low values of an applied dc magnetic field. Two general conclusions are given and briefly discussed.

Thorpe, A. N.↗

NASA NTRS1991

Micromechanics thermal stress analysis of composites for space structure applications

This paper presents results from a finite element micromechanics analysis of thermally induced stresses in composites at cryogenic temperatures typical of spacecraft operating environments. The influence of microstructural geometry, constituent and interphase properties, and laminate orientation were investigated. Stress field results indicated that significant matrix stresses occur in composites exposed to typical spacecraft thermal excursions; these stresses varied with laminate orientation and circumferential position around the fiber. The major difference in the predicted response of unidirectional and multidirectional laminates was the presence of tensile radial stresses, at the fiber/matrix interface, in multidirectional laminates with off-axis ply angles greater than 15 deg. The predicted damage initiation temperatures and modes were in good agreement with experimental data for both low (207 GPa) and high (517 GPa) modulus carbon fiber/epoxy composites.

Bowles, David E.↗

NASA NTRS1996

Microstructure, Chemistry, and Origin of Grain Rims on ilmenite from the Lunar Soil Finest Fraction

Analytical transmission electron microscope (TEM) observations reveal that ilmenite grains sampled from the sub-10 micron size fraction of Apollo 11 (10084) and Apollo 16 (61221, 67701) soils have rims 10-300 nm thick that are chemically and microstructurally distinct from the host ilmenite. The rims have a thin outer sublayer 10-50 nm thick that contains the ilmenite-incompatible elements Si, Al, Ca and S. This overlies a relatively thicker (50-250 nm) inner sublayer of nanocrystalline Ti-oxide precipitates in a matrix of single-crystal ilmenite that is structurally continuous with the underlying host grain. Microstructural information, as well as data from x-ray spectrometry (EDS) and electron energy loss spectrometry (EELS) analysis of the inner sublayer, suggest that both the inner and outer sublayer assemblages are reduced and that the inner layer is depleted in Fe relative to the underlying ilmenite. The chemistry of the outer sublayer suggests that it is a surface deposit of sputtered or impact-vaporized components from the bulk lunar soil. The inner sublayer is part of the original host grain that has been physically and chemically processed, but not amorphized, by solar ion irradiation and possibly some subsolidus heating. The fact that the deposited outer sublayer is consistently much thinner than the radiation-altered inner sublayer indicates that only a minor fraction of the total rim volume is a product of vapor or sputter deposition. This finding is in contrast to recent descriptions of thick deposited layers on one-third of regolith silicate grains and indicates that ilmenite and silicate rims as a group are different in the fraction of deposited material that they contain.

Christoffersen, Roy↗

NASA NTRS1999

Wetting Characteristics of Immiscibles

Early microgravity experiments with immiscible alloys were usually carried out with the intent of forming dispersed microstructures. By processing under microgravity conditions, the main mechanism leading to gross phase separation could be eliminated. However, analysis of flight samples revealed a separated structure where the minor phase was present along the outer surface, while the major phase was present in the center. The Wetting Characteristics of Immiscibles (WCI) project, which flew aboard the USMP-4 (United States Microgravity Payload) mission in November of 1997, was designed to gain insight into the mechanisms causing segregation of these alloys. This investigation utilized an immiscible transparent organic alloy system and a transparent container in order to facilitate direct observation of the separation process. A range of immiscible alloy compositions was utilized in order to obtain variations in the minor and major phases present and observe the influence on the segregation processes. A small composition range was found where the minor liquid phase perfectly wet the cell gasket. Unexplained observations were made at the extremes of the composition range.

Andrews, J. B.↗

DOE OSTI2026

TEM Approaches for Microstructure-Informed Prediction of Mechanical Properties in Structural Alloys

Predicting the mechanical performance of structural alloys from their evolving microstructure remains a major challenge in materials science, particularly for nuclear structural materials, where irradiation-induced defects span multiple types and length scales and interact through complex mechanisms. The dispersed barrier hardening (DBH) [1] and Friedel–Kroupa–Hirsch (FKH) [2,3] models have been widely used to evaluate the hardening contributions of individual obstacles and to estimate tensile strength from quantified microstructures; however, when multiple size-dependent obstacles coexist and evolve, predicting temperature-dependent tensile strength becomes significantly more complex, and a fully consistent hardening model is still lacking. Transmission electron microscopy (TEM) plays a central role in refining hardening models and enabling predictive assessments of tensile strength evolution by providing quantitative characterization of dislocations, irradiation-induced defects (e.g., dislocation loops and cavities), precipitates, and grain structure (Fig. 1.). These experimentally measured defect densities are incorporated into physically based hardening models with size- and shape- dependent obstacle strengths [4], using root-sum-square superposition for obstacles of comparable strength and linear superposition for dissimilar ones [5]. In addition, recent advances in TEM [6-8], including high-resolution imaging, 4D-STEM strain mapping, EDS/EELS elemental analysis, and flash-polishing-based TEM specimen preparation and extraction-replica methods (Fig. 2), further improve the accuracy of microstructural quantification. By comparison with prior studies as well as our own results, we show that when TEM-derived microstructural information is carefully integrated with physically grounded hardening models, yield strength (or irradiation-induced hardening) measured at room temperature can be predicted with good quantitative agreement across multiple alloy classes. In-situ TEM combined with high-temperature mechanical testing represents an important next step for refining hardening models by directly probing dislocation–obstacle interactions across varying irradiation doses and temperatures [9]. Because the barrier strength factor (α) depends on both temperature and obstacle size, it should not be treated as a constant fitting parameter; rather, it must be explicitly evaluated to achieve physically meaningful predictions of mechanical behaviour at operating temperatures. This presentation therefore discusses why all strengthening contributions (e.g., Peierls stress, solid-solution strengthening, voids, bubbles, dislocation loops, dislocation lines, and grain boundaries) must be considered collectively, why appropriate superposition methods are essential when obstacles possess different barrier strength factors, how hardness measurements can be meaningfully related to tensile properties, and how TEM-derived microstructural information can be systematically incorporated into hardening models. More broadly, it outlines a pathway toward microstructure-informed prediction of mechanical properties and supports the goal of establishing science-based tools for evaluating structural materials in extreme environments [10].

Lin, Yan-Ru [ORNL] (ORCID:0000000339991473)↗

NASA NTRS2015

Microstructural Influence on Deformation and Fatigue Life of Composites Using the Generalized Method of Cells

A fully coupled deformation and damage approach to modeling the response of composite materials and composite laminates is presented. It is based on the semi-‐analytical generalized method of cells (GMC) micromechanics model as well as its higher fidelity counterpart, HFGMC, both of which provide closed-form constitutive equations for composite materials as well as the micro scale stress and strain fields in the composite phases. The provided constitutive equations allow GMC and HFGMC to function within a higher scale structural analysis (e.g., finite element analysis or lamination theory) to represent a composite material point, while the availability of the micro fields allow the incorporation of lower scale sub‐models to represent local phenomena in the fiber and matrix. Further, GMC's formulation performs averaging when applying certain governing equations such that some degree of microscale field accuracy is surrendered in favor of extreme computational efficiency, rendering the method quite attractive as the centerpiece in a integrated computational material engineering (ICME) structural analysis; whereas HFGMC retains this microscale field accuracy, but at the price of significantly slower computational speed. Herein, the sensitivity of deformation and the fatigue life of graphite/epoxy PMC composites, with both ordered and disordered microstructures, has been investigated using this coupled deformation and damage micromechanics based approach. The local effects of fiber breakage and fatigue damage are included as sub‐models that operate on the microscale for the individual composite phases. For analysis of laminates, classical lamination theory is employed as the global or structural scale model, while GMC/HFGMC is embedded to operate on the microscale to simulate the behavior of the composite material within each laminate layer. A key outcome of this study is the statistical influence of microstructure and micromechanics idealization (GMC or HFGMC) on the overall accuracy of unidirectional and laminated composite deformation and fatigue response.

Microscale Models↗

DOE OSTI2025

A Parametric, Data-Driven, Non-Intrusive Reduced-Order Model Framework for Crystal Plasticity Simulations of Voids

The influence of the internal structure at micrometer length scales on the deformation of polycrystalline materials can be effectively captured using crystal plasticity finite element methods (CPFEM). However, the complexity and nonlinearity of the deformation equations CPFEM solves demand significant computational power and resources to achieve accurate predictions, limiting its broader application. To address this challenge, we have identified a reduced-order representation of the complex data in order to establish a computationally efficient reduced-order models (ROM) and drastically reduce the computational expense of CPFEM. Specifically, in this work, we developed a parametric, data-driven, and non-intrusive ROM framework for CPFEM using proper orthogonal decomposition (POD) and sparse variational Gaussian process (SVGP) regression for single-crystal microstructures under tensile loading conditions. The developed protocol enables one to compress field into a latent/low-dimensional space described by principal component analysis (PCA) via the singular value decomposition (SVD) algorithm. As a result, the high-dimensional data are reduced to a significantly smaller amount of dimensions with POD bases and POD coefficients. Furthermore, we deployed an ensemble of SVGPs—extended from the classical Gaussian process (GP) regression for scalability and handling big data—in a massively parallel manner to train and predict latent POD coefficients using known POD bases from a set of previously obtained simulations results. Lastly, using the predicted POD coefficients, we reconstructed the full-field results and showed reasonable agreement compared with the true values obtained from running CPFEM. The developed framework is validated with a set of CPFEM simulations of a single embedded void in single-crystal aluminum alloy. While the framework is broadly applicable, this work specifically focuses on single-crystal microstructures, a single load case (e.g., tensile), and a specific void geometry (spherical).

Anisotropy↗

DOE OSTI2024

Study of Helium Irradiation Effect on Al6061 Alloy Fabricated by Additive Friction Stir Deposition

Additive friction stir deposition (AFS-D) is considered a productive method of additive manufacturing (AM) due to its ability to produce dense mechanical parts at a faster deposition rate compared to other AM methods. Al6061 alloy finds extensive application in aerospace and nuclear engineering; nevertheless, exposure to radiation or high-energy particles over time tends to deteriorate their mechanical performance. However, the effect of radiation on the components manufactured using the AFS-D method is still unexamined. In this work, samples from the as-fabricated Al6061 alloy, by AFS-D, and the Al6061 feedstock rod were irradiated with He+ ions to 10 dpa at ambient temperature. The microstructural and mechanical changes induced by irradiation of He+ were examined using a scanning electron microscope (SEM), energy-dispersive X-ray spectroscopy (EDS), transmission electron microscopy (TEM), and nanoindentation. This study demonstrates that, at 10 dpa of irradiation damage, the feedstock Al6061 produced a bigger size of He bubbles than the AFS-D Al6061. Nanoindentation analysis revealed that both the feedstock Al6061 and AFS-D Al6061 samples have experienced radiation-induced hardening. These studies provide a valuable understanding of the microstructural and mechanical performance of AFS-D materials in radiation environments, offering essential data for the selection of materials and processing methods for potential application in aerospace and nuclear engineering.

36 MATERIALS SCIENCE↗

DOE OSTI2026

Tailoring Thermal and Mechanical Performance Through Multimaterial Laser Powder Directed Energy Deposition of Copper and 17-4PH Stainless Steel

This study investigates the additive manufacturing (AM) processing, microstructural evolution, and resulting mechanical and thermal properties of multimaterial components combining 17-4PH stainless steel and pure copper (Cu) fabricated via laser powder directed energy deposition (LP-DED). Conventional tooling steels exhibit limited thermal conductivity, significantly constraining production throughput in high-volume processes. Incorporating Cu, with its superior thermal conductivity, could significantly enhance tool performance, though Cu and steel present metallurgical incompatibilities when processed via AM. A systematic investigation was conducted across compositions ranging from 0 to 100 wt% Cu, revealing critical thresholds influencing solidification behavior, defect formation, microstructure, hardness, and thermal transport. Optical microscopy, electron backscatter diffraction (EBSD), hardness testing, and thermal conductivity measurements provided comprehensive process–structure–property correlations. Severe hot cracking occurred at low-Cu contents (6–25 wt%), aligning generally well with crack susceptibility modeling, with an unexpected discrepancy at 25 wt%. Porosity remained low (≥99% dense) throughout the compositional spectrum. EBSD analysis revealed a transformation from columnar martensitic structures at low-Cu contents to equiaxed FCC Cu-dominated structures at higher Cu concentrations, highlighting the complex microstructural transitions driven by Cu-induced changes in solidification and phase stability. Hardness decreased from 330 HV (pure 17-4PH) to 62 HV (pure Cu), consistent with microstructural changes. Concurrently, thermal conductivity improved substantially from 13.5 W/m K to 367.9 W/m K, emphasizing Cu’s dominant role in thermal transport. The findings highlight the feasibility of leveraging compositional gradients between 17-4PH and Cu to achieve tailored tooling with optimized thermal and mechanical performance.

17-4PH↗

NASA NTRS1993

Containerless processing of undercooled melts

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

Perepezko, J. H.↗

NASA NTRS2012

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

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

Goldberg, Robert K.↗

NASA NTRS1987

Structure and grain coarsening during the processing of engineering ceramics

Studies have been made of three ceramic systems (Al2O3, Y2O3/MgO, and SiC/C/B), both to explore a surface area/density diagram approach to examining the coarsening processes during sintering and to explore an alternative coarsening parameter, i.e., the grain boundary surface area (raising it at a given value of the density) and not the pore surface area; therefore, pinning of the grain boundaries by solid-solution drag is the only function evidenced by these results. The importance of such pinning even at densities as low as 75% of theoretical is linked to the existence of microstructural inhomogeneities. The early stages of sintering of Y2O3 powder have been examined using two techniques, BET surface area analysis and transmission electron microscopy. Each has given some insight into the process occurring and, used together, have provided some indication of the effect of MgO on coarsening during sintering. Attempts to further elucidate effects of MgO on the coarsening behavior of Y2O3 by the surface area/density diagram approach were unsuccessful due to masking effects of contaminating reactions during sintering and/or thermal etching. The behavior of the undoped SiC which only coarsens can be clearly distinguished by the surface area/density diagram from that of SiC/C/B which also concurrently densifies. Little additional information was obtainable by this method due to unfavorable sample etching characteristics. The advantages, disadvantages, and difficulties of application of these techniques to the study of coarsening during sintering are discussed.

Shaw, Nancy J.↗

NASA NTRS2006

Metallurgical Design and Development of NASA Crawler/Transporter Tread Belt Shoe Castings

The NASA Crawler/Transporters (CT-1 and CT-2) used to transport the Space Shuffles are one of the largest tracked vehicles in existence today. Two of these machines have been used to move space flight vehicles at Kennedy Space Center since the Apollo missions of the 1960's and relatively few modifications have been made to keep them operational. In September of 2003 during normal Crawler/Transporter operations cracks were observed along the roller pad surfaces of several tread belt shoes. Further examination showed 20 cracked shoes on CT-1 and 40 cracked shoes on CT-2 and a formal failure analysis investigation was undertaken while the cracked shoes were replaced. Six shoes were cross-sectioned with the fracture surfaces exposed and it was determined that the cracks were due to fatigue that initiated on the internal casting web channels at pre-existing casting defects and propagated through thickness both transgranularly and intergranularly between internal shrinkage cavities, porosity, and along austenitic and ferritic grain boundaries. The original shoes were cast during the 1960's using a modified 861330 steel with slightly higher levels of chromium, nickel and molybdenum followed by heat treatment to achieve a minimum tensile strength of 11 Oksi. Subsequent metallurgical analysis of the tread belt shoes after multiple failures showed excessive internal defects, alloy segregation, a nonuniform ferritic/ bainitic/martensitic microstructure, and low average tensile properties indicative of poor casting and poor heat-treatment. As a result, NASA funded an initiative to replace all of the tread belt shoes on both crawler/transporters along with a redesign of the alloy, manufacturing, and heat-treatment to create a homogeneous cast structure with uniform mechanical and metallurgical properties. ME Global, a wholly owned subsidiary of ME Elecmetal based in Minneapolis, MN was selected as manufacturing and design partner to develop the new shoes and this paper describes the research, development, and manufacturing that resulted in the successful delivery of 1044 new Crawler/Transporter tread belt shoes all meeting rigid metallurgical and mechanical design criteria derived from finite element modeling of the stress loads required for safe space shuttle transport.

Parker, Donald S.↗

DOE OSTI2026

Affine Transformations to Correlate Experimental and Simulated EDS Spectra for Multi-Element Systems

Energy Dispersive X-ray Spectroscopy (EDS) is an essential technique for determining elemental concentrations and distributions within microstructures, critical for materials discovery, optimization, and qualification. However, most published EDS data is qualitative because current quantitative EDS analysis methods require extensive calibration and post-processing, limiting their practicality and widespread adoption. This work seeks to establish a framework for accelerated EDS characterization and spectrum analysis that can leverage ML to analyze correlations between various elemental compositions and resulting EDS spectra. The complex physics and data result in a high-dimensional problem that grows exponentially with the number of elements in the system and the complexity of the spectrum analysis. ML provides a way to compute and optimize the results of this highly dimensional problem in a flexible way to tailor it to the user’s specific needs and material system. However, the framework emphasizes transparency through a strictly mathematical affine transformation, so the analysis remains understandable and reviewable to facilitate adoption by the scientific community. While currently implemented methods are simplistic and unvalidated, further development and demonstration of this framework could enable high-throughput, accurate, and accessible EDS characterization.

11 - NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

DOE OSTI2025

A deep learning and finite element approach for exploration of inverse structure–property designs of lightweight hybrid composites

Hybrid composites have important applications, such as high-performance and lightweight materials in aerospace and automotive industries. Hybrid composites utilize the synergy of diverse fillers to achieve desired material properties, but usually have more complicated microstructures. While topology optimization can optimize a particular property, designing hybrid composites for customized mechanical performances, e.g. full-range stress–strain curve, remains challenging. Here, a computational framework that integrated finite element analysis (FEA) and artificial intelligence (AI) methods of Conditional Generative Adversarial Networks (cGAN) deep learning and transfer learning was developed to establish inverse structure–property relationships and design tailor-made hybrid composites. Based on FEA-generated datasets of hybrid fiber-particle–matrix microstructures and their corresponding full-range stress–strain curves, a cGAN architecture was trained to generate tailored microstructures and establish structure–property relationships. Similarity in microstructural features and well-matched stress–strain curves based on the AI-generated composites were achieved. In conclusion, transfer learning was used to expand the pre-trained model for designing different materials systems.

Hybrid composites↗

NASA NTRS1993

Detailed analysis of Honeywell In-Space Accelerometer data - STS-32

The Honeywell In-Space Accelerometer (HISA) system collected data in the mid-deck area of the Shuttle Columbia during the flight of STS-32, January 1990. The resulting data were to be used to investigate the response of crystal microstructure to different types of residual acceleration. The HISA is designed to detect and record transient and oscillatory accelerations. The sampling and electronics package stored averaged accelerations over two sampling periods; two sampling rates were available: 1 Hz and 50 Hz. Analysis of the HISA data followed the CMMR Acceleration Data Processing Guide, considering in-house computer modelling of a float-zone indium crystal growth experiment. Characteristic examples of HISA data showing the response to the primary reaction control system, Orbiter Maneuvering System operations, and crew treadmill activity are presented. Various orbiter structural modes are excited by these and other activities.

Rogers, Melissa J. B.↗