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DOE OSTI2023

Fracture‐Resistant and Thermally Insulating Ultrahigh‐Temperature Carbide Foams

Dense ultrahigh‐temperature ceramics (UHTCs) carbides are recognized as potential materials for thermal protection systems (TPS) owing to properties beyond existing structural materials’ capabilities. Recent advances in UHTCs have enabled the development of multiscale porous microstructures. Herein, it is highlighted that the porosity in UHTCs are no longer treated as a defect but as a functional property specifically tailored for thermal insulation. It is a promising solution to design and fabricate bulk UHTC foams via a freeze‐drying (FD) approach followed by calibrated pressureless spark plasma sintering. Herein, monolithic TaC and HfC UHTC foams and their composite show the partial solid–solution formation of (Ta, Hf)C with porosity ≥50%. TaC–HfC foam (≈80–92 N) shows an intermediate load‐bearing capability compared to monolithic TaC (≈120–135 N) and HfC (≈28–35 N) foams, with no evident cracking on the sample surface. The thermal conductivity of partial solid‐solution TaC–HfC foam increases up to fivefold compared to parent UHTC foams. In the results, solid solutions’ efficacy and pores’ unidirectionality in providing thermal insulation to TaC–HfC while maintaining its high‐load bearing capability are illustrated. In conclusion, the developed technique establishes a new paradigm shift in UHTCs, expanding their potential for TPS in extreme environments.

36 MATERIALS SCIENCE↗

NASA NTRS1992

The Earth Observing System (EOS) nickel-hydrogen battery

Information is given in viewgraph form on the Earth Observing System (EOS) nickel hydrogen battery. Information is given on the life evaluation test, cell characteristics, acceptance and characterization tests, and the battery system description.

Bennett, Charles W.↗

DOE OSTI2026

Equilibrium and non-equilibrium effects in high pressure phase transformations of carbon

The behavior of carbon in the range 1–100 GPa and 1–10 kK is central to problems in planetary interiors, inertial confinement fusion targets, and high-pressure synthesis of carbon-based materials, but experiments in this regime are difficult and often provide only indirect constraints on phase behavior. As a result, phase boundary loci, structure, and limits of metastability at high pressure remain uncertain. In this work, machine-learning enhanced atomistic simulations are used to address this knowledge gap. We determine the melt line up to 100 GPa, the graphite-diamond phase boundary up to the melt line, and analyze structure of the coexisting phases. We show that the coexisting liquid evolves smoothly with pressure without evidence for a first-order liquid–liquid transition. Orientation-resolved graphite melting simulations indicate that basal-plane interfaces develop a dewetting layer and undergo layer-by-layer melting, producing kinetic hysteresis and an apparent orientation dependence of the melt line. Non-equilibrium quenches from the melt are used to construct a kinetically limiting graphite–diamond phase boundary for rapid quenches from above the melt line, and show that graphite is metastable at pressures of up to ≈ 25 GPa. These results provide bounds on equilibrium and metastable behavior in carbon relevant for interpreting high-pressure experiments and for designing synthesis pathways to specific carbon microstructures.

Lyu, Yanjun [Department of Materials Science and E↗

NASA NTRS2012

General Purpose Data-Driven System Monitoring for Space Operations

Modern space propulsion and exploration system designs are becoming increasingly sophisticated and complex. Determining the health state of these systems using traditional methods is becoming more difficult as the number of sensors and component interactions grows. Data-driven monitoring techniques have been developed to address these issues by analyzing system operations data to automatically characterize normal system behavior. The Inductive Monitoring System (IMS) is a data-driven system health monitoring software tool that has been successfully applied to several aerospace applications. IMS uses a data mining technique called clustering to analyze archived system data and characterize normal interactions between parameters. This characterization, or model, of nominal operation is stored in a knowledge base that can be used for real-time system monitoring or for analysis of archived events. Ongoing and developing IMS space operations applications include International Space Station flight control, spacecraft vehicle system health management, launch vehicle ground operations, and fleet supportability. As a common thread of discussion this paper will employ the evolution of the IMS data-driven technique as related to several Integrated Systems Health Management (ISHM) elements. Thematically, the projects listed will be used as case studies. The maturation of IMS via projects where it has been deployed or is currently being integrated to aid in fault detection will be described. The paper will also explain how IMS can be used to complement a suite of other ISHM tools, providing initial fault detection support for diagnosis and recovery

Space Propulsion↗

NASA NTRSDate not supplied

Evaluating Crystallinity in Thermoplastic Composites for Aerospace Applications

Polymer matrix composites (PMCs) offer many benefits for the aerospace industry due to their potential for weight reduction when compared to metal or ceramic based materials. Most PMCs currently in flight use thermoset matrices, however, thermoplastic resins are being explored as alternatives due to their ability to be remelted, which is of particular interest due to the potential for in-situ repair and faster production. Most thermoplastic resins are semicrystalline polymers. The properties of semicrystalline thermoplastics are directly influenced by their crystallinity, which can vary due to many factors including thermal treatments, environmental conditions, and mechanical deformation. Within thermoplastic PMC parts, crystallinity gradients can arise due to variations in part geometry, across part thicknesses, and along bonded joints. Monitoring the crystallinity of thermoplastic composites is key to ensuring these materials meet the high demands required for aerospace. Several different analytical techniques exist that can be used to characterize the bulk crystallinity of thermoplastic materials. However, many existing methods lack the specificity required to identify the subtle variations in crystallinity that may play a significant role in the performance and durability of PMC parts. Because of this, a significant amount of work is still required to fully characterize and understand the crystallinity profiles of thermoplastic PMCs and the resulting impact to material properties. This talk discusses the use of multiple techniques such as Differential Scanning Calorimetry, Polarized Light Optical Microscopy, and Fourier-Transform Infrared Spectroscopy to characterize the crystallinity in carbon fiber/thermoplastic composites. Samples of different crystallinity profiles were manufactured using various cooling procedures. This work aims to provide the fundamental data necessary to understand the effects of crystallinity on thermoplastic PMCs, which is key to advancing their use in aerospace applications.

Thermoplastics↗

NASA NTRS2009

General Purpose Data-Driven System Monitoring for Space Operations

Modern space propulsion and exploration system designs are becoming increasingly sophisticated and complex. Determining the health state of these systems using traditional methods is becoming more difficult as the number of sensors and component interactions grows. Data-driven monitoring techniques have been developed to address these issues by analyzing system operations data to automatically characterize normal system behavior. The Inductive Monitoring System (IMS) is a data-driven system health monitoring software tool that has been successfully applied to several aerospace applications. IMS uses a data mining technique called clustering to analyze archived system data and characterize normal interactions between parameters. This characterization, or model, of nominal operation is stored in a knowledge base that can be used for real-time system monitoring or for analysis of archived events. Ongoing and developing IMS space operations applications include International Space Station flight control, satellite vehicle system health management, launch vehicle ground operations, and fleet supportability. As a common thread of discussion this paper will employ the evolution of the IMS data-driven technique as related to several Integrated Systems Health Management (ISHM) elements. Thematically, the projects listed will be used as case studies. The maturation of IMS via projects where it has been deployed, or is currently being integrated to aid in fault detection will be described. The paper will also explain how IMS can be used to complement a suite of other ISHM tools, providing initial fault detection support for diagnosis and recovery.

Satellites↗

NASA NTRS1986

Parametric tests of a 40-Ah bipolar nickel-hydrogen battery

A series of tests were performed to characterize battery performance relating to certain operating parameters which include charge current, discharge current, temperature, and pressure. The parameters were varied to confirm battery design concepts and to determine optimal operating conditions.

Cataldo, R. L.↗

DOE OSTI2026

Rinse-Free, Sodium-Efficient Synthesis of O3-Type Layered Oxide Materials Enabled by Acetate Precursors

Sodium-ion batteries (SIBs) are a sustainable alternative to lithium-ion systems for global electrification, with O3-type layered oxide cathodes offering high specific capacity and feasibility of scalable synthesis. Industrial co-precipitation synthesis of these cathodes typically uses transition metal sulfates, requiring extensive water rinsing to remove Na 2 SO 4 impurities, a process that consumes significant water and risks residual inactive phases if incomplete. Here, this work introduces a rinse-free, resource-efficient approach using metal acetate precursors. Residual sodium acetate in non-rinsed precursors decomposes during sintering to generate Na 2 CO 3 in situ, partially substituting an external sodium resource (e.g., NaOH and Na 2 CO 3 ) and reducing its consumption by ∼18–20%. Phase-pure O3-Na 1.0 Ni 1/3 Fe 1/3 Mn 1/3 O 2 (NFM111) cathodes synthesized via this method exhibit microstructure and electrochemical performance comparable to rinsed sulfate-derived counterparts, with initial capacities of 141 mAh g −1 at C/20 (7.5 mA g −1 ). By eliminating rinsing and minimizing sodium reagent use, this acetate-based route enhances sustainability and scalability of layered oxide production for SIBs.

acetate vs. sulfate↗

DOE OSTI2026

Sintering effects on NpO 2 grain size and morphology: The role of precursor Np phase

Neptunium dioxide (NpO 2 ) is a key phase in nuclear material processing as a target material for the production of plutonium-238 ( 238 Pu) and has been historically synthesized via the calcination of a Np oxalate precursor. Alternative synthesis methods for NpO 2 are now more prevalent, necessitating their study and comparison with the more common oxalate route. The purpose of this work was to investigate the microstructural properties of NpO 2 synthesized from a nitrate-based Np precursor phase via the assessment of NpO 2 particle size and morphology as a function of calcination temperature and time. Scanning electron microscopy (SEM) was used to probe the primary grain size and morphology of NpO 2 after calcination at temperatures ranging from 700 to 1100 °C and hold times ranging from 1 to 10 h. Post-image analysis using ImageJ software enabled the quantification of mean particle diameter. This analysis indicated that particle diameter increases with both increasing calcination temperature and hold time. Primary particles were shown to be clumped in irregular patterns into the overall rough, blocky aggregates, but this macroscopic morphology was not affected by calcination time or temperature. Although trends in primary grain size of NpO 2 were consistent with available literature from other Np precursor phases, the macroscopic morphology of the NpO 2 aggregates was quite different than reported for other precursors. Through comparison with historical literature on Np oxalate, this work emphasizes the importance of Np precursor on the physical properties of NpO 2 .

38 RADIATION CHEMISTRY, RADIOCHEMISTRY, AND NUCLEA↗

DOE OSTI2026

Uncovering Hidden Entanglement in Twin Beams

Proper characterization of quantum correlations in multimode optical quantum states is critical for applications in quantum information science. However, standard entanglement measurements can lead to incomplete state reconstruction and characterization. Here, we implement a resonator-based detection system that reveals entanglement between sideband modes of twin beams, achieving full tomography and retrieving often ignored quantum correlations. Unlike standard spectral measurements such as homodyne detection, resonator detection can independently address the sidebands of each beam, thereby accessing these hidden correlations. Additionally, we show how phase shifts between the carrier and the sideband modes of the involved fields redistribute information and modify the observation of entanglement for different witnesses. The ability of the resonant detection to independently address sideband modes of entangled states can contribute to enhancing the capacity for secure communication and quantum networking protocols.

Rincon Celis, Raul [University of Sao Paulo, Brazi↗

DOE OSTI2026

Mechanical and durability properties of ultra-high-performance concrete of spent nuclear fuel dry storage systems: a review

Dry storage systems are used for interim storage of spent nuclear fuel (SNF). However, with the growing need to extend the operational periods of these systems, there are concerns about the degradation of their concrete overpacks, which could compromise the system's structural integrity and safety during hazardous events. Traditional concrete mixtures used in SNF dry storage systems have remained largely unchanged since their inception and often use conventional ingredients. These materials are susceptible to degradation mechanisms such as chemical attacks, alkali-silica reactions (ASR), and freeze–thaw cycles, which can lead to a loss of strength and durability over time. To address these challenges, this paper reviews the application of ultra-high-performance concrete (UHPC) as a promising alternative for spent nuclear fuel dry storage system overpacks. UHPC offers superior mechanical properties, exceptional durability, and reduced susceptibility to degradation mechanisms compared to conventional concrete. This paper focuses on the role of supplementary cementitious materials (SCMs) such as silica fume, fly ash, and metakaolin in enhancing UHPC performance for SNF storage applications. These SCMs have been shown to significantly improve the material’s microstructure, strength, and resistance to environmental stressors typically encountered in SNF storage environments. Moreover, incorporating SCMs supports sustainable construction by reducing cement consumption and associated carbon emissions. The review brings together existing research and experimental data, providing insights for engineers and researchers on developing UHPC mixtures that meet the rigorous demands of spent nuclear fuel dry storage systems, extending their service life and minimizing inspection intervals.

36 - MATERIALS SCIENCE↗

DOE OSTI2026

Kinetic control of phase evolution and defect-mediated recombination in AACVD-grown copper antimony sulphide thin films

Copper antimony sulphide (CAS) is a multinary chalcogenide semiconductor in which small deviations from stoichiometry can drive phase competition and strong defect-mediated modulation of optoelectronic properties. However, the systematic roles of copper precursor fraction and deposition time in governing phase evolution, off-stoichiometry, and recombination dynamics in aerosol-assisted chemical vapour deposition (AACVD)-grown undoped CAS thin films remain insufficiently understood. In this work, undoped CAS thin films were deposited by AACVD using Cu(dedtc)2 and Sb(dedtc)3 single-source precursors at 550 °C and a carrier gas flow rate of 150 sccm, while the Cu(dedtc)2 mole fraction (x = 0.15 – 0.55) and deposition time (1 – 2 hours) were systematically varied to probe how growth kinetics influence phase composition, microstructure, and defect-mediated optical properties without post-deposition annealing or extrinsic doping. Increasing copper precursor content drives phase evolution toward tetrahedrite-dominant CAS films at intermediate Cu(dedtc)2 mole fractions, with the film deposited at x = 0.35 exhibiting the strongest tetrahedrite character within the parameter space examined. The films are also copper-rich, antimony-poor, and sulphur-deficient, consistent with off-stoichiometric growth and intrinsic defect formation, plausibly including copper interstitials, Cu-on-Sb antisites, and sulphur vacancies. These growth-dependent compositional deviations are accompanied by tunable indirect optical bandgaps of approximately 1.60 – 2.18 eV and weak visible photoluminescence governed by defect-mediated recombination. Time-resolved photoluminescence reveals bi-exponential decay behaviour with lifetimes of approximately 0.1 – 3.6 ns, with emission dominated by slower donor–acceptor pair recombination and a smaller contribution from faster trap-assisted pathways. Collectively, these results establish an explicit kinetic process–structure–defect–property relationship for AACVD-grown CAS thin films and provide a growth–structure–property framework relevant to future optimization of CAS-based optoelectronic and energy materials.

36 MATERIALS SCIENCE↗

NASA NTRS1974

Storage battery comprising negative plates of a wedge shaped configuration

An improved silver-zinc battery particularly suited for use in an environment where battery operation is subjected to multiple charge/discharge cycling over extended periods is described. The battery seperator system, containing a highly absorbent material continguous with the surfaces of the plates and multiple semi-permeable membranes interposed between the plates, is also characterized.

Bogner, R. S.↗

DOE OSTI2025

Super-resolution imaging reveals resistance to mass transfer in functionalized stationary phases

Chemical separations are costly in terms of energy, time, and money. Separation methods are optimized with inefficient trial-and-error approaches that lack insight into the molecular dynamics that lead to the success or failure of a separation and, hence, ways to improve the process. We perform super-resolution imaging of fluorescent analytes in five different commercial liquid chromatography materials. Unexpectedly, we observe that chemical functionalization can block more than 50% of the material’s porous interior, rendering it inaccessible to small-molecule analytes. Only in situ imaging unveils the inaccessibility when compared to the industry-accepted ex situ characterization methods. Selectively removing some of the functionalization with solvent restores pore access without substantially altering the single-molecule kinetics that underlie the separation and agree with bulk chromatography measurements. Our molecular results determine that commercial “fully porous” stationary phases are over-functionalized and provide an alternative avenue to characterize and direct separation material design from the bottom-up.

Science & Technology - Other Topics↗

DOE OSTI2024

Isotropic negative thermal expansion in ZrW 2 O 8 and HfW 2 O 8 from 1100 to 1275°C

Abstract ZrW 2 O 8 (ZrO 2 •2WO 3 ) and HfW 2 O 8 (HfO 2 •2WO 3 ) have been the focus of thermal expansion studies due to their isotropic negative thermal expansion (NTE) measured previously at temperatures below 775°C. This work presents measurements of these materials at their thermodynamically stable temperature ranges of 1105 and 1257°C for ZrW 2 O 8 and 1105–1276°C for HfW 2 O 8 , where they were characterized with in situ, powder X‐ray diffraction. The linear coefficients of thermal expansion were measured to be −5.52 × 10 −6 and −4.87 × 10 −6 °C −1 for ZrW 2 O 8 and HfW 2 O 8 , respectively. The mechanism leading to this NTE is discussed. Powder samples were synthesized by a solution‐based process called the organic–inorganic steric entrapment method. In situ characterization in air was carried out at the National Synchrotron Light Source II using a hexapole lamp, optical furnace and the Advanced Photon Source using a quadrupole lamp, optical furnace to achieve elevated temperatures.

Materials Science↗

NASA NTRS2026

Influences of Introduced Yttrium Oxide Particles on Superalloy 718

Additive manufacturing has proven useful for introducing oxide particles into superalloys, to provide oxide dispersion strengthening (ODS) at high temperatures. This study screened how such an approach can influence microstructure and failure modes for superalloy 718. The objective of this study was to compare tensile and creep failure modes for additively manufactured superalloy 718 having introduced oxide particles. Fine yttrium-oxide (yttria) particles were introduced into 718 powder using two different powder mixing methods. Additive manufacturing by laser powder bed fusion was then used to prepare specimen blanks for each case, oriented parallel and transverse to the building direction. These were subsequently given consistent stress relief, hot isostatic pressurization, and final heat treatments, then subjected to tensile and creep tests at varied temperatures. Additively manufactured 718 without ODS (“no-ODS”) had nearly equiaxed grains at 50 μm in width. Roll-mixed ODS material had a bimodal grain size distribution, with fine grains at 9 μm and coarse grains at 66 μm in average width. The fine grains were elongated about 5x in the building direction. Acoustic-mixed ODS materials had grains at 10 μm in width that were elongated about 10x in the build direction. Compared to no-ODS, roll-mixed and acoustic mixed ODS materials did not show improved tensile strengths at room temperature, 760 °C, and 1093 °C. The tensile failure strains parallel to the building direction of roll-mixed ODS material were lowest in these tests. Flattened clumps of yttria had formed transverse to the building direction in roll-mixed material, which were easily cracked. Creep rupture response at 760 °C in the building direction was highest for acoustic-mixed material test. Creep tests at 1093 °C showed varied results, with low rupture lives associated with enhanced cavitation at grain boundaries and surface oxidation. Transverse to the building direction, all three materials had low failure strains in tests at 760 °C. The elongated grain boundaries failed readily in all transverse specimens tested at 760 °C and 1093 °C.

oxide dispersion strengthening↗

DOE OSTI2026

Development of large-scale, 3D Printed high temperature ceramic material

Through this collaborative effort, a new 3D printing platform for ceramics called laser-induced slip casting (LIS) was explored and developed for improving the processing and manufacture of silicon carbide (SiC), a high temperature ceramic material. This method prints layers of ceramic slips/slurries with subsequent selective-laser heating to dry each layer to build a 3D structure. The completed and dried part is then sintered. This manufacturing process is inherently lower cost than alternative ceramic printing methods such as binder jet technology or stereolithography when it comes to the feedstock material but is more expensive than robocasting or direct ink writing. However, it has the potential to make more controlled parts with less defects compared to robocasting. The largest cost is the heating source for the printer. With this technique, there is potential to make large ceramic parts in a near-net shape. Further, there is no known commercial manufacturing of 3D printed ceramics that creates a large range of different high-density ceramics at large scale. The goals and outcomes for the development of the new printing technology were: 1) assessing the technology with alumina by characterizing coupons, 2) printing and sintering of silicon carbide (SiC), and 3) characterization and properties testing of materials printed and a scale-up of SiC part(s). Through this collaborative project, it was sought to provide the best solution to achieving highly dense and near-net shaped ceramic parts at large scale and reduced cost. The goal was to produce high density sintered materials for applications in defense, energy generating systems, armor, and wear parts using 3D printing methods. Variables including powder particle sizes, dispersant molecular weights (MWs), binders, printing parameters, and post processing were explored as well as the characterization of the physical properties (add specifics here).

36 MATERIALS SCIENCE↗

DOE OSTI2026

Operando microscopy for neuromorphic hardware

Microscopy techniques can uncover the physical properties and dynamic behaviours of materials, driving the discovery of emergent phenomena and guiding the design of next-generation computing hardware. As artificial intelligence becomes pervasive, the demand for high-performance materials to support sustainable information technologies is growing. Here, this Review highlights state-of-the-art imaging from electron and X-ray to optical techniques to probe the dynamics of neuromorphic materials, including operando characterization of devices. We examine design principles for neuromorphic materials, along with obstacles that hinder their development. Emphasis is placed on spatially and temporally resolved approaches that capture state changes including phase transitions, ferroic switching and spin-wave propagation that emulate biological components such as neurons, synapses and their connectivity. We discuss challenges in operando characterization and the integration of artificial intelligence-driven analysis for feedback-guided material discovery. Finally, we outline opportunities for real-time imaging of neuromorphic systems, paving the way towards adaptive, brain-inspired hardware.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗