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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 73 records · Page 4
All sourcesNASA NTRSDOE OSTI
DOE OSTI2024

Voltage and temperature effects on low cobalt lithium-ion battery cathode degradation

Degradation of low cobalt lithium-ion cathodes was tested using a full factorial combination of upper cut-off voltage (4.0 V and 4.3 V vs. Li/Li + ) and operating temperature (25 °C and 60 °C). Half-cell batteries were analyzed with electrochemical and microstructural characterization methods. Electrochemical performance was assessed with galvanostatic cycling, cyclic voltammetry (CV), and electrochemical impedance spectroscopy (EIS) supported by distribution of relaxation times (DRT) analysis. Electrode microstructure was characterized with scanning electron microscopy (SEM), X-ray diffraction (XRD), and X-ray absorption near edge structure (XANES) imaging. Higher cut-off voltage cycling shows presence of NiO x formation, a low diffusivity rock-salt phase, in both CV and XRD data. XRD patterns confirmed that the rock-salt phase was beginning to form at the low cut-off voltage at high temperature, but in much lower intensity than at the high cut-off voltage. Higher temperature accelerates degradation processes at both voltages. Degradation factors at high temperature include NiO x formation, cathode material dissolution, and electrolyte decomposition. SEM analysis suggests that supporting phases may isolate and disconnect active material particles reducing capacity retention and battery life cycle. DRT analysis and XANES imaging show that both high temperature samples revealed a NiO x phase based on an increased diffusive impedance and a visible shift in the XANES spectra. The low cut-off voltage, high temperature sample showed a split peak and shift to lower energies indicating early formation of the NiO x phase. The diffusive impedance, which hinders intercalation and deintercalation, is driven by the formation of the NiO x phase. While primarily driven by cut-off voltage, elevated temperature also contributes to this degradation mechanism.

electrochemical impedance spectroscopy↗
DOE OSTI2025

Improving microstructures segmentation via pretraining with synthetic data

Image analysis of material microstructures through microscopy is an integral capability in the field of materials science. The topological and chemical information obtained through microscopy allow us to draw vital connections between material microstructures, properties, and processing. While scanning electron microscopy (SEM) is able to yield a considerable wealth of information interpretable by the intuition of experts, there has been considerable interest in using machine learning, convolutional neural networks (CNNs) in particular, for such image analysis task. Training CNNs for an image analysis task requires a large annotated dataset. However, in many materials science applications, obtaining a large annotated dataset is cost and labor intensive. In this work, we study the use of synthetic data to enlarge the available annotated experimental data of uranium oxide. We utilize a modified Potts model to simulate uranium oxide particles with morphologies similar to those observed experimentally. We then leverage an image-to-image translation model to synthesize the simulated particles as if they are acquired with SEM. Through this process, we obtain pairs of particle images and their corresponding SEM representations, which corresponds to pairs of annotations and images. Unlike previous works, we leverage synthetic data for pretraining a CNN model prior, and finetune that model further with experimental data. We experimentally demonstrate that using synthetic data as incremental learning process benefits the overall performance compared to training a model on combined synthetic and experimental data.

36 MATERIALS SCIENCE↗
DOE OSTI2026

Thermal loading effects on chalk hydromechanical behavior for nuclear waste disposal

Safe disposal of heat-generating nuclear waste depends on host rock stability under thermal, hydrological, and mechanical stresses. This study investigates the effect of thermal loading on mechanical behavior of the shallowly buried Ghareb formation chalk through triaxial and hydrostatic constant strain rate and creep tests at temperatures up to 100 ˚C and effective pressures up to 20.7 MPa. Experimental results show that thermal loading reduces the elastic moduli of chalk by 50–75%, and a transition occurs above 60 ˚C where creep rates increase rapidly. Water saturation nearly doubles the thermally induced strain compared to dry conditions and strongly decreases material rigidity. Thermal loading also leads to significant pore pressure increases under undrained conditions and leads to reductions in the apparent permeability during drained conditions. Laboratory experimental data were used to parameterize and develop a preliminary constitutive model for predicting future deformation during repository operations in the Ghareb. The strongly coupled effects – mechanical weakening, fluid pressure fluctuations, and permeability modification – demonstrate that elevated repository temperatures will have a pronounced effect on the near field Ghareb behavior during waste disposal operations. The findings indicate that the coupled interactions must be considered in predictive models and repository design to ensure long-term nuclear waste isolation and safety.

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗
DOE OSTI2025

Effect of Plutonium on Uranium Oxide Microstructural Fingerprint

The analysis of particulates from environmental sampling is routinely performed for nuclear forensics applications. In order to increase the tools available for nuclear forensics applications, capability development materials (CDMs), or reference particulates, are necessary for developing and benchmarking new analytical methods. Historically, these CDM particulates have been produced with highly controlled and characterized isotopic and size parameters for applications in developing and benchmarking particle sizers and mass spectrometry analytical methods [1- 4]. However, the development of CDMs with highly characterized particle morphology and phase of the particles is vital for aiding in the development and benchmarking of particle analytical methods for those parameters. In many cases, key properties such as crystallographic phase, morphology, and microstructure, may be correlated to processing history of environmental sampling particulates [5]. To that end, this work investigates determining the structural fingerprint of produced Pu-doped uranium oxide CDMs using transmission electron microscopy (TEM). The particulates, one of which shown in Figure 1, were synthesized to Fig. 1. Single particulate of uranium oxide fabricated using the THESEUS technique. develop capabilities for environmental sampling investigations. These particles are monodisperse at diameter of 1 μm and a range of plutonium concentrations from 0- 1,000 ppm. Given their small diameter, TEM analysis was ideal for studying the particulate structural fingerprint in detail. Previous investigations confirmed the external homogeneity of the particulates at different plutonium concentrations, however this analysis focuses on determining the grain structure, phase distribution, and porosity of the particulates.

Mayer, Jack [Univ. of Florida, Gainesville, FL (Un↗
DOE OSTI2025

High resolution microstructural, chemical studies and localized burnup analysis in an irradiated U–10Zr metallic fuel

This study involves high resolution characterization of a sodium bonded solid uranium (U)-10 wt% zirconium (Zr) metallic fuel irradiated in Fast Flux Test Facility (FFTF). The fuel centerline temperature during irradiation was estimated to be around 675 °C with the peak burnup 13.1 atomic percent. Samples for transmission electron microscopy (TEM) and atom probe tomography (APT) were prepared from different regions/zones in the fuel cross section radially to elucidate the microstructural changes and chemical redistribution of solute elements as well as fission products during irradiation experiment. TEM results indicate the irradiation in fast flux testing leads to the formation of extensive Zr-rich precipitates with varying sizes in the U–Zr fuel matrix. APT analysis performed to investigate redistribution of Zr, U and fission products along the radial direction of fuel pin showed Zr-rich precipitates entrapping the fission products in higher concentration as compared to the α-U phases. Here, the local burnup ( 235 U depletion) is found to be consistent, calculated by quantification of 235 U, 236 U and 238 U isotopes from mass spectrum obtained from APT along the radial direction. Zr-rich precipitation and its implication on fuel constitutional redistribution are discussed based on SEM, TEM and APT results.

APT↗
DOE OSTI2024

Data-Driven Surrogate Modeling with Microstructure-Sensitivity of Viscoplastic Creep in Grade 91 Steel

Abstract To support the development of advanced steel alloys tailored to withstand extreme conditions, it is imperative to account for the mechanical performance of components, while considering the influence of local microstructure on the macroscopic response. To this end, this study focuses on the development of microstructure-sensitive constitutive models for the mechanical response of Grade 91 steel exposed to extreme thermo-mechanical environments. Polynomial chaos expansion (PCE) surrogates are used to emulate high-fidelity polycrystal simulations of the viscoplastic response of Grade 91 steel as a function of the microstructure fingerprint (e.g., dislocations and precipitates). To cover a wide temperature–stress domain, two separate PCE surrogates—one that captures softening and the other that captures hardening behavior—are combined using another (sparse) Gaussian process regression model. The resulting constitutive creep surrogate model is integrated within the MOOSE finite element framework to simulate the intricate effects of microstructure, in particular MX-phase precipitates, on a component with a graded microstructure. Surrogate sensitivity analysis is applied to quantify the relevant impact of spatially varying microstructure on the creep response in a test-case involving a Grade 91 alloy with a prototypical weld.

36 MATERIALS SCIENCE↗
DOE OSTI2025

Concavity-based local erosion and sphere-size-based local dilation applied to lithium-ion battery electrode microstructures for particle identification

Performance metrics of lithium-ion batteries can be extracted from the analysis of electrode microstructures nanoscale imaging. The characterization workflow can involve a challenging particle identification, or instance segmentation, step. In this work, we propose a new identification method based on an original transformation: a sphere-size-based local dilation followed by a concavity-based local erosion, that is local morphology closing. The new transformation is much more efficient than the global morphology closing, with correct identification achieved with only 1.7 % dilation volume and 2.6 % erosion volume on a test geometry, compared to 39.2 % and more than 50 %, respectively, with its global counterpart. The new method has been then benchmarked versus other identification algorithms (watershed and pseudo coulomb repulsive field) on a real electrode microstructure with equal or better segmentation achieved.

25 ENERGY STORAGE↗
DOE OSTI2025

Microstructurally informed synchrotron x-ray analysis revealing helium defect transitions in ultrafine grained tungsten

The formation of insoluble gaseous defects in materials due to nuclear transmutation or ion implantation involves the diffusion of impurity atoms to form atomic defect clusters that coalesce into bubbles or cavities and ultimately degrade the material properties. Transmission electron microscopy (TEM) is limited in its ability to resolve sub-nanometer gas clusters whereas X-ray diffraction (XRD) provides information pertaining to local atomic changes. Here, in this study, helium (He) implanted ultrafine grained tungsten is explored through a multimodal defect characterization campaign combining TEM-informed Small Angle X-ray Scattering (SAXS) analysis, XRD lattice parameter measurements, and nanoscale He cluster quantification from a region of reciprocal space accessible via Wide Angle X-ray Scattering (WAXS). Moderate elevated temperature implantations are shown to produce high concentrations of sub-nanoscale He clusters and small, homogeneously distributed cavities, which collectively are linked to lattice expansion and further substantiated through complementary atomistic simulations. Increased implantation temperatures encourage the diffusion of these defects to the grain boundaries (GBs), leading to lattice relaxation and the growth of large GB cavities manifesting as bimodal size distributions in the SAXS analysis. Overall, our results demonstrate the utility of multimodal synchrotron X-ray analysis in bridging the gap between microscale He cavity quantification and atomic-scale defect analysis.

36 MATERIALS SCIENCE↗
DOE OSTI2025

Quadrilateral particle arrangement within shocks in a two-dimensional dusty plasma

The microscopic structure within a two-dimensional shock was studied using data from a dusty plasma experiment. A single layer of charged microparticles, levitated in a glow-discharge plasma, was perturbed by an electrically floating wire that was moved at a steady supersonic speed to excite a compressional shock. A rearrangement of particles was observed, from a hexagonal lattice in the preshock into a quadrilateral microstructure on the front side of the shock. This quadrilateral structure would not be stable in a monolayer of identical repulsive particles, under equilibrium conditions. Glaser-Clark polygon analysis of the microstructure helped in identifying quadrilaterals. Voronoi analysis was used to characterize the defect fraction behind the shock, as an indication of shock-induced melting. Published by the American Physical Society 2025

Kananovich, Anton (ORCID:0000000225374952)↗
DOE OSTI2025

Clustering Algorithm for AM Parts using GSH and EDT with Autoencoder

SAND2025-10103O The Clustering Algorithm for AM Parts Using GSH and (EDT With Autoencoder is a software tool. It uses a clustering algorithm for additive manufacturing (AM) parts using generalized spherical harmonics (GSH) and Euclidean distance transform (EDT) with an autoencoder to quantify material microstructure. The tool offers improved sensitivity to microstructural changes compared to traditional approaches. The tool integrates multiple microstructural properties, such as grain morphology, crystallographic orientation, and material phase information, to provide a comprehensive analysis of material microstructures. Sandia National Laboratories is a multimission laboratory managed and operated by National Technology & Engineering Solutions of Sandia, LLC, a wholly owned subsidiary of Honeywell International Inc., for the U.S. Department of Energy’s National Nuclear Security Administration under contract DE-NA0003525.

Rodgers, Theron [Sandia National Lab. (SNL-CA), Li↗
DOE OSTI2025

Generalizable Image Segmentation for Microstructure Characterization Through Integrated SEM and EBSD Analysis

We demonstrate generalizable semantic segmentation using minimal ground truth data. Correlated scanning electron microscopy (SEM) images and electron backscatter diffraction (EBSD) measurements of frictionstir processed 316L stainless steel plates were used to train deep learning models for grain boundary segmentation. Secondary electron (SE) imaging taken at an accelerating voltage of 10 keV correlated to EBSD-derived grain boundaries produced the best performing model. Notably, an ensemble of three models trained on a single SE image produced accurate segmentation over a series of BSE images of samples manufactured under different processing parameters, with a resultant mean absolute error in grain size of 0.34 µm. The striking generalizability of the models likely results from the similar escape depths of the SE training input and the EBSD training output and the reduced probability of dislocation artifacts appearing in the image. This finding highlights the importance of considering the physical principles behind imaging in the development of robust segmentation models for microstructure characterization.

Taufique, Mohammad Fuad Nur↗
DOE OSTI2025

In-situ synchrotron X-ray study on microstructure and stress evolutions of electroplated copper upon self-annealing

Background: The self-annealing behavior of electroplated copper (Cu) at room temperature is gaining attention in the microelectronics industry due to its significant impact on reliability issues such as substrate warpage and electrical resistivity. Methods: In this study, in-situ analysis of the microstructure transition and stress relaxation of the electroplated copper upon self-annealing was conducted via synchrotron white X-ray nanodiffraction (beamline 21A, Taiwan Photon Source) and grazing-incidence X-ray diffraction (beamline 17B1, Taiwan Light Source). Significant Findings: Remarkable relaxations of deviatoric stress and absolute strain component along the [002] direction were closely related to the Cu grain growth and crystallographic reorientation at the early stage of selfannealing, and a complete stress/strain relaxation can be achieved with the cessation of microstructure transition. In conclusion, the in-situ synchrotron X-ray studies provided an insight into Cu self-annealing mechanism, offering valuable information for improving Cu interconnect reliability.

Cu Self-annealing↗
DOE OSTI2025

Reactive Carbide‐Based Synthesis and Microstructure of NASICON Sodium Metal All Solid‐State Electrolyte

Reactive carbide precursor-based synthesis of NASICON-type NZSP (Na 1+x Zr 2 Si x P 3-x O 12 ) solid-state electrolyte (SSE) is demonstrated, in contrast to the established oxide-based approach. Exothermic decomposition of ZrC and SiC in air homogenizes microstructure, yielding 98% compact density after conventional sintering at 1200 °C. Quantitative stereology demonstrates that significant microstructural differences are present. Compacts of carbide-derived Carb-NZSP are 98% dense with a secondary zirconium oxide (ZrO 2 ) volume fraction of 0.2% ± 0.3%, versus 93% dense and 3% ± 1% for oxide-derived baseline. For Carb-NZSP, the secondary glassy phosphate phase is agglomerated, while for baseline, it is dispersed and percolated. Electrochemical testing combined with post-mortem analysis demonstrates how microstructural control of secondary phases is critical for dendrite suppression: Carb-NZSP critical current density (CCD) is 3.1 ± 0.8 mA cm −2 at 0.1 mAh cm −2 , versus 1.0 ± 0.7 mA cm −2 at 0.1 mAh cm −2 . Cryogenic focused ion beam (cryo-FIB) analysis demonstrates that in both materials, the porous 2D sheet-like sodium metal dendrites propagate around and subsume NZSP grains, likely following a path enriched with glassy phase and with porosity. Dendrites also flow around isolated zirconia particles. Phase field simulation reveals deflection of dendrites by mechanically tough zirconia, while brittle glassy phase accelerates dendrite growth, especially when finely distributed.

36 MATERIALS SCIENCE↗
DOE OSTI2025

Homogenization of Dendritic Structures and the High-Temperature Strength of the Refractory High-Entropy Alloy MoNbTaVW

MoNbTaVW, a pioneering refractory high-entropy alloy (RHEA), is renowned for its exceptional strength at elevated temperatures. Like most RHEAs, it solidifies into a dendritic microstructure with steep concentration gradients, necessitating heat treatment for equilibration. Steep concentration gradients typically complicate mechanical property analysis and modeling, key challenges for high-throughput alloy discovery. This study examines the effects of high-temperature homogenization (1800 °C for 8 hours) on the microstructure and mechanical properties of MoNbTaVW across temperatures up to 1200 °C. Postmortem microstructural analysis, coupled with chemical, crystallographic, and mechanical assessments, revealed that yield strength was surprisingly insensitive to homogenization, with less than a 3 pct difference between as-cast and heat-treated materials. Nanoindentation confirmed minimal nanohardness changes across the dendritic structure at room temperature. However, homogenization significantly enhanced high-temperature work hardening, producing higher peak compressive strength. Both as-cast and homogenized MoNbTaVW exhibited room-temperature strengths of 1400 MPa, exceeding previously reported values. These findings demonstrate that high-temperature treatment enables microstructural homogenization without compromising strength, a unique behavior among RHEAs. In conclusion, while not universally applicable, this insight highlights the importance of understanding microstructural development in experimental alloys and offers a pathway to design alloys that achieve homogeneous-like properties without heat treatment.

Rietema, C. J. [Lawrence Livermore National Labora↗
DOE OSTI2024

Characterization of build parameters and microstructure in low heat input WAAM of Ni-based superalloy Haynes 282

Conference paper for 2024 10th International Conference on Advances in Materials, Manufacturing & Repair for Power Plants. Ni-based superalloy Haynes 282 is a prime candidate for advanced power generation systems due to its superior fabricability, weldability, and high-temperature performance. Additive manufacturing offers potential cost and time savings for gas turbine components. Wire-arc direct energy deposition can create large components but often requires post-processing treatments, such as hot isostatic pressing (HIP), to address porosity. This study explores a low heat-input, high deposition rate GMAW process to achieve fully dense Haynes 282 without HIP. Twenty-one blocks were deposited, varying travel and wire feed speeds. Initial analysis (visual inspection, microstructural examination, and CT) revealed the impact of build parameters on internal porosity and defects. Scanning electron microscopy provided insights into structural heterogeneity and microstructural properties. Related journal article can be found at https://doi.org/10.31399/asm.cp.am-epri-2024p0001.

Adam, Benjamin↗
DOE OSTI2026

Microstructure prediction for Ti-22Al-25Nb in laser powder bed fusion

This work presents a physics-informed framework for predicting solidification morphology and defect susceptibility in additively manufactured Ti–22Al–25Nb across a broad processing space. The framework integrates solidification microstructure selection (SMS) analysis with a single-track defect-based printability map to establish a unified methodology linking processing parameters to both interfacial morphology and manufacturability. Thermal gradients G and solidification rates R are first computed using the Thermo-Calc Additive Manufacturing (TC-AM) module, a finite-interface-dissipation (FID) phase-field (PF) model coupled with CALPHAD method is then employed to systematically distinguish planar and dendritic regimes as functions of $G$ and $R$. By superimposing the printability map onto the morphology projections, a comprehensive process–structure framework is obtained. Across most processing conditions, the predicted microstructure is predominantly dendritic, while planar growth emerges only under selected laser power $P$ and scan speed $v$ combinations. In addition to morphology classification, the framework quantifies the dendritic area fraction and introduces a width-based morphology descriptor to characterize the spatial extent of planar/dendritic regions within the melt pool. It provides mechanistic insight into the interplay between solidification physics and defect formation, offering practical guidance for parameter selection and microstructural control in Ti–22Al–25Nb additive manufacturing (AM).

36 MATERIALS SCIENCE↗
DOE OSTI2025

Fatigue Performance of an Improved Creep Strength 10%Cr Steel

The deployment of 9-12% Cr steels for elevated temperature applications up to 650 °C presents a cost-effective alternative to more expensive nickel-based alloys in steam turbine power generation. To enhance creep resistance at this temperature range, a novel ferritic-martensitic steel, designated CPJ7, was developed and fabricated at the National Energy Technology Laboratory. The alloy design aimed to mitigate the transformation of strengthening carbides into deleterious phases that degrade creep performance. Results have demonstrated that CPJ7 exhibits favorable creep and oxidation resistance at 650 °C. However, its fatigue performance remains unexplored. This study builds upon prior research by evaluating the low cycle fatigue behavior of CPJ7 and verifying that modifications beneficial to creep performance were not detrimental to the fatigue performance. The alloy was tested at both 650 °C and ambient temperature under fully reversed bending conditions (R = − 1) and a load ratio of 0.05. Furthermore, the alloy exhibits cyclic softening, a behavior consistent with other 9-10 wt.% Cr steels. Analysis of the microstructure and hysteresis loops further corroborate cyclic softening mechanisms typical of ferritic-martensitic steels. Overall, the fatigue performance of CPJ7 meets or exceeds that of P91 steel, demonstrating its potential for high-temperature structural applications.

9% Cr ferritic-martensitic steel↗
DOE OSTI2025

Additive manufacturing of high‐density silicon carbide ceramics through post‐processing spark plasma sintering

This research advances the field of additive manufacturing (AM) of silicon carbide (SiC) ceramics by integrating spark plasma sintering (SPS) to enhance material density, mechanical strength, and thermal properties. Traditional AM techniques struggle to achieve the high‐density SiC required for demanding applications, such as aerospace engineering, where high thermal conductivity and mechanical strength are paramount. Here, our study addresses these challenges by incorporating SPS as a post‐processing step, achieving near‐theoretical maximum densities and significantly reducing porosity, thereby resulting in outstanding thermal conductivity in SiC ceramics. We developed a specialized SiC ink optimized for 3D printing, ensuring structural integrity after deposition through tailored rheological properties. The application of SPS facilitates rapid, uniform sintering, essential for attaining superior density, mechanical properties, and thermal performance. Our experimental results, confirmed through scanning electron microscopy analysis, demonstrate significant microstructural properties, mechanical strength, and thermal conductivity, showcasing the effectiveness of integrating SPS in AM processes. This innovative approach not only expands the capabilities of AM in producing complex, high‐density ceramic structures but also broadens the potential applications of SiC in demanding environments.

36 MATERIALS SCIENCE↗