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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 19 records
All sourcesNASA NTRSDOE OSTI
DOE OSTI2024

Near-net shaping of high-density, complex, spatially-tailored ceramics for extreme environments

The purpose of this subcontract is for LLNL to collaborate with the Subcontractor (UCSB) in the areas of binder jet additive manufacturing (BJAM), hot pressing (HP), finite element modeling (FEM), and multi-material sintering studies. LLNL wants to further develop its hot pressing, AM, and modeling capabilities through LLNL’s Early Career Faculty Program. This work will focus on developing a method to hot press complex-shaped ceramic parts through the co-deposition of a structural/functional ceramic and sacrificial mold material in one assembly via multi-material binder jet printing. The method aims to produce dense, near-net shaped parts with applications relevant to a wide variety of fields including aerospace, defense, and energy.

36 MATERIALS SCIENCE↗
DOE OSTI2025

Additive manufacturing of carbon fiber-reinforced thermoset composites via in-situ thermal curing

Fiber-reinforced polymer composites are lightweight structural materials widely used in the transportation and energy industries. Current approaches for the manufacture of composites require expensive tooling and long, energy-intensive processing, resulting in a high cost of manufacturing, limited design complexity, and low fabrication rates. Here, we report rapid, scalable, and energy-efficient additive manufacturing of fiber-reinforced thermoset composites, while eliminating the need for tooling or molds. Use of a thermoresponsive thermoset resin as the matrix of composites and localized, remote heating of carbon fiber reinforcements via photothermal conversion enables rapid, in-situ curing of composites without further post-processing. Rapid curing and phase transformation of the matrix thermoset, from a liquid or viscous resin to a rigid polymer, immediately upon deposition by a robotic platform, allows for the high-fidelity, freeform manufacturing of discontinuous and continuous fiber-reinforced composites without using sacrificial support materials. This method is applicable to a variety of industries and will enable rapid and scalable manufacture of composite parts and tooling as well as on-demand repair of composite structures.

36 MATERIALS SCIENCE↗
DOE OSTI2026

Developing cathode infiltration processes for all-solid-state bilayer LLZO cells

To realize the bilayer architecture of lithium lanthanum zirconate (LLZO) for application in solid-state batteries (SSBs), the scaffold structure must be optimized, and effective cathode infiltration strategies must be established. In this study, we fabricate a modified bilayer LLZO using a sacrificial layer to enhance surface porosity, and systematically investigate various cathode infiltration techniques to fill the scaffold with oxide cathode active materials (CAM). Structural characterizations showed that the sacrificial layer significantly increased open surface porosity, enabling the surface of the scaffold to be filled with CAM. To further increase infiltration depth, applying vacuum or vibration was compared, with the full-depth infiltration achieved using a sonicator-based vibration. Full cells prepared using the modified bilayer LLZO and vibration-assisted technique demonstrated successful operation. This work demonstrates a practical and scalable approach for engineering bilayer LLZO structures and integrating oxide cathodes into porous scaffolds, offering a promising pathway toward high-performance solid-state batteries.

Bilayer↗
DOE OSTI2026

Hybrid Additive Manufacturing and Electric Field-Assisted Sintering of High-temperature Heat Exchangers via Sacrificial Channel Molds

A hybrid manufacturing approach, integrating additive manufacturing (AM) with powder methodology via electric field-assisted sintering (EFAS), was developed for the fabrication of high-temperature compact heat exchangers (CHX) from refractory metals. The methodology employed additively manufactured sacrificial channel molds (SCMs) as shapeholders for CHX channels, which were embedded in metal powders using EFAS. Following embedding, the SCMs were chemically dissolved to form the internal channel network. SCMs were fabricated using both digital light processing (DLP) and direct ink writing (DIW) from chemically reactive, calcium-based ceramic feedstocks with varying ratios of Al2O3 reinforcement. The microstructure, phase composition, and dissolution behavior of both as-printed and embedded SCMs were investigated. The shrinkage behavior of the SCMs embedded in refractory metals, as well as the interfacial characteristics between the SCMs and metal matrix, were studied. The results showed that the SCMs containing sufficient chemical reactive ceramics dissolved effectively before and after embedding. The as-printed SCMs retained the phase composition of their feedstocks, but the embedded SCMs containing calcium-based ceramics and Al2O3 exhibited the formation of calcium aluminates due to high temperature exposure during embedding. Most SCMs exhibited a cellular Al2O3 network filled with Ca-rich ceramics. Shrinkage after embedding was strongly dependent on SCM density, with lower density SCMs exhibiting greater shrinkage. A thin SCM-affected zone was observed at the metal matrix surface, characterized by increased porosity compared to the bulk matrix. This effect was attributed to infiltration of the SCM materials into powder particle boundaries under pressure, followed by their removal during dissolution. This study demonstrates the feasibility of manufacturing CHXs from hard-to-process refractory metals for use in harsh environments.

36 - MATERIALS SCIENCE↗
DOE OSTI2025

Transitory Topochemical Tailoring of a van der Waals Superconductor

Topochemical intercalation is widely used to access metastable phases with novel electronic properties, but the reverse reaction (deintercalation) typically restores the original state, limiting practical use. Here, in this study, we present a topochemical approach that employs a sacrificial intercalant that thermally decomposes to irreversibly lock in the new electronic state. Using 2-aminobutane as the sacrificial intercalant, we convert the van der Waals (vdW) material 1T-TiSe 2 into a superconductor and the vdW superconductor 2H-NbSe 2 into a nonsuperconducting metal, while preserving the ability to exfoliate the resulting crystals. We find that this transitory intercalation increases the electron density in both materials and partially suppresses the CDW in TiSe 2 . By tuning the thermolysis temperature, we can systematically vary the carrier density in TiSe 2 , enabling us to map its phase diagram. The superconductivity in TiSe 2 is retained in exfoliated flakes, although with a lower critical temperature. This transitory topochemical strategy enables access to new electronic states with precisely tuned carrier densities that are otherwise inaccessible through direct solid-state synthesis.

36 MATERIALS SCIENCE↗
DOE OSTI2026

Electrochemical Nutrient Recovery for the Food–Energy–Water Nexus at Municipal Wastewater Facilities: Multivariate Analyses of Seasonal Sampling and Reactor Performance

Digester-equipped municipal wastewater facilities generate recycle streams with high nutrient loads that increase energy consumption and can cause environmental pollution. The reduction of these loads through electrochemical nutrient recovery (ENR) could enhance the food–energy–water nexus by producing fertilizer (struvite). This study investigated the recovery process through a 1 year sampling of recycle streams and the implementation of nutrient recovery. Time series analyses showed that P (as orthophosphate) concentration was time-variant in digester effluent streams, while N (as ammonia) concentration was time-variant in only the aerobic system. Furthermore, these two nutrient concentrations did not correlate in any of the recycle streams. Subsequent multivariate screening analyses identified anode type, NH 4 + concentration, cathodic potential, P concentration, and temperature as most significant for ENR. Finally, the optimum conditions of cathodic potential, anode area-to-volume ratio, and temperature applied to a real recycle stream resulted in 95% P recovery with 0.03 kWh/kg P. This energy consumption is significantly lower than process energy for conventional P fertilizers (1.1 kWh/kg P) and chemical recovery processes at scale (1.7–12.9 kWh/kg P). Overall, this study recommended specific process controls for nutrient recovery, expanded the variables evaluated for ENR, and demonstrated the ability to significantly impact energy demand associated with P-based fertilizers.

36 MATERIALS SCIENCE↗
DOE OSTI2025

Dual-Wavelength Simultaneous Patterning of Degradable Thermoset Supports for One-Pot Embedded 3D Printing

Vat photopolymerization (VP) techniques have enabled the fabrication of complex geometries while balancing high precision and fast processing times. 3D printed objects are traditionally built layer-by-layer with newly cured layers being structurally supported by previous ones. Fabricating unsupported features such as overhangs and arches risks misalignment and sagging, limiting the range of accessible designs. To overcome this issue, support structures are fabricated along with the primary object as temporary scaffolds that provide stability and conserve print fidelity. For VP specifically, patterning dissolvable sacrificial supports is attractive to avoid manual removal after printing. In this study, we demonstrate a base-degradable thermoset to pattern print supports in a one-pot formulation along with the primary structural material. Efficient printing is enabled using a dual-wavelength negative imaging (DWNI) DLP printer that patterns the degradable thermoset with visible light and the permanent network with UV light, which are simultaneously projected using a single digital micromirror device (DMD). Printed objects undergo thermal postprocessing to enhance the final conversion of the primary material, after which thermoset supports are degraded in a basic, aqueous solution. This approach provides a robust method for the dual-wavelength patterning of sacrificial thermoset supports, broadening the range of accessible 3D printable materials and geometries.

3D printing↗
DOE OSTI2025

Measurement of post-disruption runaway electron kinetic energy and pitch angle during final loss instability in DIII-D

Post-disruption runaway electron (RE) kinetic energy K and pitch angle sin$\vartheta$ are critical parameters for determining resulting first wall material damage during wall strikes, but are very challenging to measure experimentally. During the final loss instability, confined RE K and sin$\vartheta$ are reconstructed during center-post wall strikes for both high impurity (high-Z) and low impurity (low-Z) plasmas by combining soft x-ray, hard x-ray, synchrotron emission, and total radiated power measurements. Deconfined (wall impacting) RE sin$\vartheta$ is then reconstructed for these shots by using time-decay analysis of infra-red imaging. Additionally, deconfined RE K and sin$\vartheta$ are reconstructed for a low-Z downward loss shot by analyzing resulting damage to a sacrificial graphite dome limiter. The damage analysis uses multi-step modeling simulating plasma instability, RE loss orbits, energy deposition, and finally material expansion (MARS-F, KORC, GEANT-4, and finally COMSOL). Overall, mean kinetic energies are found to be in the range $\langle$$K$$\rangle$ $≈ 3-4$ MeV for confined REs. KORC simulations indicate that the final loss instability process does not change individual RE kinetic energy K. In conclusion, confined RE pitch angles are found to be fairly low initially pre-instability, $\langle$sin$\vartheta$$\rangle$ $≈ 0.1 – 0.2$, but appear to increase roughly 2x, to $\langle$sin$\vartheta$$\rangle$ $≈ 0.3 – 0.4$ for both confined and deconfined REs during instability onset in the low-Z case; this increase is not observed in the high-Z case.

70 PLASMA PHYSICS AND FUSION TECHNOLOGY↗
DOE OSTI2024

Large Area Transfer of Bismuth‐Based Layered Oxide Thin Films Using a Flexible Polymer Transfer Method

Magnetic and ferroelectric oxide thin films have long been studied for their applications in electronics, optics, and sensors. The properties of these oxide thin films are highly dependent on the film growth quality and conditions. To maximize the film quality, epitaxial oxide thin films are frequently grown on single-crystal oxide substrates such as strontium titanate (SrTiO 3 ) and lanthanum aluminate (LaAlO 3 ) to satisfy lattice matching and minimize defect formation. However, these single-crystal oxide substrates cannot readily be used in practical applications due to their high cost, limited availability, and small wafer sizes. One leading solution to this challenge is film transfer. In this demonstration, a material from a new class of multiferroic oxides is selected, namely bismuth-based layered oxides, for the transfer. A water-soluble sacrificial layer of Sr 3 Al 2 O 6 is inserted between the oxide substrate and the film, enabling the release of the film from the original substrate onto a polymer support layer. The films are transferred onto new substrates of silicon and lithium niobate (LiNbO 3 ) and the polymer layer is removed. These substrates allow for the future design of electronic and optical devices as well as sensors using this new group of multiferroic layered oxide films.

36 MATERIALS SCIENCE↗
DOE OSTI2024

Advanced Functional Materials ZnO@ZIF-8 Heterostructures for Neuromorphic Synaptic Devices

Metal-Organic Frameworks have shown great promise for memristive synaptic devices because of their adaptable electrical properties and inherent porosity, which help in efficient ion transport and storage of functional molecules. However, the limited conductivity and sensitivity to moisture associated with most MOF materials hinder their use in electronic applications. In this study, MOFs derived from metabolites have been synthesized, using ZnO as a self-sacrificial metallic source to grow Zeolitic Imidazolate Framework-8 (ZIF-8), forming ZnO@ZIF-8 heteronanostructures for neuromorphic applications. These hybrids ZnO@ZIF-8 act as promising candidates for advanced electronic applications. Through systematic investigations, including a comparison of ZnO@ZIF-8 bilayer devices with ZnO single-layer counterparts, a significant discovery emerged. The bilayer synaptic devices outperformed their single layer counterparts in electrical characteristics, as evidenced by Current-Voltage curve analysis and Long-Term Potentiation/Long Term Depression (LTP/LTD) measurements. Additionally, the ZnO layer thickness (10, 30, 50 nm) has been emphasized and the effects of annealing at 300°C in a vacuum were carefully studied for Neuromorphic Synaptic Devices. Remarkably, the 10 nm ZnO layer exhibited the lowest set voltage and a consistent On/Off ratio. This work marks a significant advancement in understanding bilayer synaptic devices, highlighting the crucial role of ZIF-8 in shaping the future of neuromorphic systems

Kolleboyina, Jayaramulu↗
DOE OSTI2025

Ambient Rare Earth Metal Electrodeposition in Nitrogen-Coordinated Silylamide Electrolyte

The transition to a sustainable, low-carbon economy demands energy-efficient and environmentally benign methods for rare earth metal (REM) production. Furthermore, while high-temperature molten salt electrolysis remains energy-intensive, corrosive, and environmentally unfriendly, emerging room-temperature processes based on conventional ionic liquids are also hindered by high viscosity and chemical instability. In this study, a nitrogen-coordinated, water-, oxygen-, and fluorine-free silylamide-based electrolyte is presented as a promising system for room-temperature REM electrodeposition. Derived from commercially available lithium silylamide precursors, the system enables facile synthesis, broad electrochemical stability, and tunable metal–ligand interactions. Electrochemical analysis reveals high voltammetric stripping reversibility, stable cathodic and anodic potentials, and selective neodymium (Nd) deposition at appreciable current densities (>1 mA/cm 2 ), with minimal parasitic reactions. Bulk experiments produced high-purity Nd with reproducible performance across multiple batches. Scaled deposition yielded over 1 g of Nd with near-theoretical mass efficiency (0.40 mg/C) and >90% purity. Using sacrificial dysprosium (Dy) and Nd metal anodes, the system maintained constant Nd loading during extended deposition and enabled cathodic codeposition of stripped anode material, demonstrating the electrolyte’s dual functionality for REM electrorefining. Collectively, this silylamide platform offers a compelling combination of electrochemical robustness, chemical resilience, and process scalability for sustainable ambient REM recovery.

36 - MATERIALS SCIENCE↗
DOE OSTI2024

Covalent Triazine-Based Frameworks with Ru-tda Based Catalyst Anchored via Coordination Bond for Photoinduced Water Oxidation

Light-induced water splitting (hν-WS) for the production of hydrogen as a solar fuel is considered a promising sustainable strategy for the replacement of fossil fuels. An efficient system for hν-WS involves a photoactive material that, upon shining light, is capable of separating and transferring charges to catalysts for the hydrogen and oxygen evolution processes. Covalent triazine-based frameworks (CTFs) represent an interesting class of 2D organic light-absorbing materials that have recently emerged thanks to their tunable structural, optical and morphological properties. Typically, catalysts (Cat) are metallic nanoparticles generated in situ after photoelectroreduction of metal precursors or directly drop-casted on top of the CTF material to generate Cat-CTF assemblies. Here, in this work, the synthesis, characterization and photocatalytic performance of a novel hybrid material, Ru-CTF, is reported, based on a CTF structure featuring dangling pyridyl groups that allow the Ru-tda (tda is [2,2':6',2'“-terpyridine]-6,6'”-dicarboxylic acid) water oxidation catalyst (WOC) unit to coordinate via covalent bond. The Ru-CTF molecular hybrid material can carry out the light-induced water oxidation reaction efficiently at neutral pH, reaching values of maximum TOF of 17 h -1 and TONs in the range of 220 using sodium persulfate as a sacrificial electron acceptor.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2025

Pick-and-Place Transfer of Arbitrary-Metal Electrodes for van der Waals Device Fabrication

Van der Waals electrode integration is a promising strategy to create nearly perfect interfaces between metals and 2D materials, with advantages such as eliminating Fermi-level pinning and reducing contact resistance. However, the lack of a simple, generalizable pick-and-place transfer technology has greatly hampered the wide use of this technique. Here, we demonstrate the pick-and-place transfer of prefabricated electrodes from reusable polished hydrogenated diamond substrates without the use of any sacrificial layers due to the inherent low-energy and dangling-bond-free nature of the hydrogenated diamond surface. The technique enables transfer of arbitrary-metal electrodes and an electrode array, as demonstrated by successful transfer of eight different elemental metals with work functions ranging from 4.22 to 5.65 eV. We also demonstrate the electrode array transfer for large-scale device fabrication. The mechanical transfer of metal electrodes from diamond to van der Waals materials creates atomically smooth interfaces with no interstitial impurities or disorder, as observed with cross-section high-resolution transmission electron microscopy and energy-dispersive X-ray spectroscopy. As a demonstration of its device application, we use the diamond transfer technique to create metal contacts to monolayer transition metal dichalcogenide semiconductors with high-work-function Pd, low-work-function Ti, and semimetal Bi to create n- and p-type field-effect transistors with low Schottky barrier heights. We also extend this technology to air-sensitive materials (trilayer 1T’ WTe 2 ) and other applications such as ambipolar transistors, Schottky diodes, and optoelectronics. This highly reliable and reproducible technology paves the way for new device architectures and high-performance devices.

2D materials↗
DOE OSTI2024

High-resolution chemical patterns from negative tone resists for the integration of extreme ultraviolet patterns of metal-oxide resists with directed self-assembly of block copolymers

Extreme ultraviolet (EUV) lithography faces significant challenges in designing suitable resist materials that can provide adequate precision, while maintaining economically viable throughput. These challenges in resist materials have led to printing failures and high roughness in EUV patterns, compromising the performance of semiconductor devices. Integrating directed self-assembly (DSA) of block copolymers (BCPs) with EUV lithography offers a promising solution because, while the BCPs register to the EUV-defined chemical guiding pattern, the thermodynamically determined structures of the BCPs automatically rectify defects and roughness in the EUV pattern. Despite the superior resolution of metal-oxide EUV resists (MORs), their application to DSA is limited by the difficulty in converting them into chemical patterns that allow effective transfer of the rectified patterns of DSA films into inorganic materials. To address this challenge, this study introduces a novel strategy for fabricating chemical patterns using hydrogen silsesquioxane (HSQ), a high-resolution negative tone inorganic resist, as a model system for MORs. Initially, a sacrificial Cr pattern is generated from HSQ patterns via reactive ion etching. The sacrificial Cr pattern is converted into a chemical pattern by first grafting a water-soluble polyethylene oxide brush onto the substrate, then wet etching the Cr, and finally grafting nonpolar polystyrene brushes. Assembling polystyrene-block-poly(methyl methacrylate) on these patterns results in structures oriented and registered with the underlying pattern, achieving 24 nm full-pitch resolutions. In conclusion, this approach has the potential to integrate MOR patterns into the DSA process, thereby enabling the generation of high-quality sub-10 nm patterns with high-χ BCPs.

Atomic force microscopy↗
DOE OSTI2024

Reactive Fe anode for electrolytic reduction of solid metal oxide in molten LiCl-Li 2 O

Iron metal was investigated for use as a consumable anode for electrolytic reduction of solid metal oxides in molten LiCl-Li 2 O (2.0 - 2.4 wt%). Tests were performed where the potential of Fe anodes was increased incrementally from 0.1 to 1.0 V (vs Ni/NiO). Oxide formation on the anode started at a potential of 0.4 V and was identified as FeO via X-ray diffraction. In the absence of a pre-formed oxide layer, severe attack of the anode started at a potential of 0.7 V and was accompanied by an increase in Fe concentration in the salt. When an oxide layer was allowed to form on the anode, the Fe concentration did not increase in the salt. O 2 was detected in the headspace gas at an anode potential of 1.0 V only when an oxide layer was present on the anode. Finally, the results of this study support the idea that an inexpensive sacrificial anode could be an ideal replacement for expensive Pt that is currently widely used for this process.

36 MATERIALS SCIENCE↗