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DOE OSTI2025

Gas-solid reaction-based selective lithium leaching strategy for efficient LiFePO 4 recycling

As the electric-vehicle market continues to expand, LiFePO 4 (LFP) batteries, valued for their intrinsic safety and cost-effectiveness, are being increasingly utilized. However, this widespread adoption highlights the urgent need for innovative and environmentally friendly recycling methods for spent LFP batteries due to their relatively low material value and the environmental challenges associated with traditional recycling processes. Here, in this study, we present a novel selective lithium leaching technique that involves a gas–solid reaction with chlorine gas. This method achieves a remarkable leaching efficiency of 99.8 % and a selectivity of 98.8 % at 200 °C within just 10 min, without generating acidic wastewater. The resulting LiCl solution was successfully converted into Li 2 CO 3 with an excellent purity of 99.5 %, while producing NaCl solution as the only byproduct. Notably, the olivine structure of the LFP was preserved as FePO 4 after lithium leaching. The regenerated LFP demonstrated excellent performance, retaining 94.1 % of its capacity after 150 cycles, while the lithium-leached FePO 4 delivered a reversible capacity exceeding 150 mAh/g. This approach not only enhances the efficiency of LFP recycling but also paves the way for more sustainable battery technologies.

36 MATERIALS SCIENCE↗

NASA NTRSDate not supplied

Seeding Method for Velocimetry and Visualization of Supersonic Retropropulsion Nozzle Plumes

In the current work, the “Venturi seeder” method for nozzle plumes is improved and studied to determine suitability for particle image velocimetry. This seeding method involves independently pressurizing the primary flow path and a separate seed liquid reservoir, connecting them at the throat of a Venturi contraction upstream of the nozzle. The pressure differential at the throat causes the liquid to enter the nozzle channel where it is atomized into particles by strong shearing forces. This new seeding system was characterized by conducting a series of diagnostics using different exit nozzle pressure ratios and seed reservoir pressures. Shadowgraph imaging confirmed the nozzle plumes to be underexpanded jets. A particle sizing device determined that generated DEHS oil particles had median aerodynamic diameters of 0.67, 0.69, and 0.73 μm for seed liquid reservoir pressure supplies of 0.67, 0.60, and 0.93 MPa and primary flow path pressures of 0.67, 0.76, and 0.93 MPa measured downstream of the Venturi throat, respectively. These diameters were within the threshold for acceptable response time in typical gas flows (≤ 1 μm). PIV experiments were conducted on the nozzle plume for all presented cases; mean axial and transverse velocities appeared as expected for the underexpanded jet structure, including the Mach disk and re-acceleration regions. Additional sizing analysis based on the particle response times across the normal shock again showed particle diameters to be well less than 1 μm for all cases. The results suggest that this method is an inexpensive and relatively simple solution to the problem of seeding nozzle plumes. The method will be used in testing of supersonic retropropulsion models in the Unitary Plan Wind Tunnel at The NASA Langley Research Center in 2022.

particle image velocimetry↗

DOE OSTI2025

NiAl–MoO 2 S 2 Nanoparticles: Structural Evolution and Mechanistic Insights into High-Performance Selenium Oxyanion Removal across Diverse pH Conditions

Advancing sorbent materials for the selective removal of toxic oxyanions from water requires synthetic control, tunable chemistry, and an atomic-level understanding of structure–function relationships. Here, we report the synthesis and detailed characterization of NiAl–MoO 2 S 2 , a novel layered double hydroxide (LDH) nanomaterial designed for the efficient sequestration of selenium oxoanions (SeO 3 2– and SeO 4 2– ) from complex aqueous environments. The material is synthesized through a room-temperature ion-exchange process, wherein interlayer NO 3 – anions in NiAl–LDH are replaced with MoO 2 S 2 2– clusters, forming high-surface-area, flower-like nanoparticles. Comprehensive structural analysis using the synchrotron X-ray pair distribution function, X-ray absorption spectroscopy, and X-ray photoelectron spectroscopy reveals a distinct chemical transformation of intercalated [MoO 2 S 2 ] 2– into [Mo 2 O 2 S 6 ] 2– -like clusters, generating redox-active interlayers that drive selenium capture. This tailored interfacial chemistry underpins the material’s exceptional sorption performance, achieving distribution coefficients (K d ) ≥ 10 6 mL/g and maximum capacities of 343 mg/g for SeO 4 2– and 514 mg/g for SeO 3 2– , outperforming state-of-the-art inorganic sorbents. Importantly, NiAl–MoO 2 S 2 maintains high selectivity and capacity across acidic, neutral, and alkaline pH, efficiently removing selenium from ppm to sub-10 ppb trace levels, even in the presence of competing ions typical of natural and industrial waters. The selenium uptake proceeds via reductive precipitation coupled with the oxidation of molybdenum and sulfide within the LDH framework. This study highlights the power of strategic synthetic modification and interlayer functionalization in LDHs to unlock new structural motifs and redox chemistries, offering a scalable route to advanced materials for environmental remediation.

Adsorption↗

DOE OSTI2025

Direct Conversion of MnO2 into Atomic Mn Sites for Oxygen Reduction

Development of platinum group metal (PGM)-free catalysts has been investigated to replace the platinum group metal catalyst in future inexpensive polymer electrolyte membrane (PEM) fuel cells. Usually, synthetic methods for these PGM-free catalysts involve introducing transition-metal salts or molecules. Herein, we demonstrate a facile synthetic method to prepare PGM-free Mn-N-C catalysts by directly converting manganese oxides into highly active MnN4 sites. Typically, MnO2 is used as a Mn source. Ammonium chloride and benzimidazole are introduced during high-temperature treatment to enhance catalytic activity and stability further. Ammonia generated from the decomposition of ammonium chloride can improve the intrinsic ORR activity of MnNx moieties through chemical or electronic effects by introducing additional nitrogen groups. The Mn-N-C catalyst exhibits promising ORR activity, achieving a half-wave potential of 0.83 V in 0.5 M H2SO4, outperforming most PGM-free ORR catalysts. The robust carbon structure resulting from organic-molecule treatment is also verified by electrochemical and physical characterization, thereby improving the catalyst's durability.

Yang, Xiaoxuan↗

DOE OSTI2025

Mechanistic Insights into Visible-Light-Induced ATRA Reactions Powered by the Symbiotic Relationship between Cu(II)/Cu(I) Phenanthroline Complexes

As photoredox catalysis continues to yield promising chemical transformations, there is an increased need to understand how specific photocatalysts function to improve reaction efficiencies while expanding their scope. Copper-phenanthroline-based photocatalysts such as Cu II (dap)Cl 2 (dap = 2,9-di(p-anisyl)-1,10-phenanthroline) and [Cu I (dap) 2 ]Cl were both found to be equally capable of olefin activation through electrophilic atom transfer radical addition (ATRA) reactions. Although these molecular catalysts have proven successful, many intermediates suggested in the proposed catalytic cycles have never been detected. One undetermined aspect in this chemistry is related to how one equivalent of Cu II (dap)Cl 2 generates half of an equivalent of [Cu I (dap) 2 ] + during the photocatalytic sequence. To this end, we initially used more synthetically accessible model systems, namely, [Cu I (dpp) 2 ]Cl and Cu II (dpp)Cl 2 (dpp = 2,9-diphenyl-1,10-phenanthroline), to glean detailed mechanistic insights into this unusual symbiotic relationship. We directly detected several intermediates involved in the ATRA photocatalytic cycle using these model chromophores in conjunction with electronic spectroscopy, infrared matrix-assisted laser desorption electrospray ionization (IR-MALDESI) mass spectrometry, electronic structure calculations, EPR spin-trap experiments, and 1 H NMR spectroscopy. We found that the unique ligand lability and coordinating properties of acetonitrile enable both the in situ oxidation of [Cu I (dpp) 2 ] + by tosyl chloride into Cu II (dpp)Cl 2 and the visible-light-induced homolysis of the Cu II –Cl bond, which initiates the conversion to the Cu I species [Cu I (dpp) 2 ][Cu I Cl 2 ]. Here, the combined findings from the present study of the catalytic cycle demonstrate that the symbiotic relationship between Cu II (dpp)Cl 2 and [Cu I (dpp) 2 ] + , as well as between Cu II (dap)Cl 2 and [Cu I (dap) 2 ] + , is the critical factor enabling the ATRA photoreaction by departing from either photocatalyst.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

DOE OSTI2025

Mechanism of O 2 Activation and Cysteine Oxidation by the Unusual Mononuclear Cu(I) Active Site of the Formylglycine-Generating Enzyme

The formylglycine-generating enzyme (FGE) catalyzes the selective oxidation of a peptidyl-cysteine to form formylglycine, a critical cotranslational modification for type I sulfatase activation and a useful bioconjugation handle. Previous studies have shown that the substrate peptidyl-cysteine binds to the linear bis-thiolate Cu(I) site of FGE to form a trigonal planar tris-thiolate Cu(I) structure that activates O 2 for the oxidation of the C β –H of the cysteine substrate via an unknown mechanism. Here, we employed a combination of stopped-flow kinetic, spectroscopic (UV–vis absorption, XAS, and EPR), and computational (DFT/TD-DFT calculations) methods to observe and characterize the key intermediates in this reaction for FGE from Streptomyces coelicolor. Our results define the reaction coordinate of FGE, which involves H-atom abstraction from the C β –H bond of the cysteine substrate by a reactive Cu(II)–O 2 •– species to form the now experimentally observed Cu(I)–OOH intermediate bound to a peptidyl-thioaldehyde, which proceeds to oxidize one of the protein-derived cysteine residues to a sulfenate that is end-on O-coordinated to Cu(I). These results provide fundamental insights into how the unusual mononuclear Cu(I) site of FGE activates O 2 for cysteine oxidation and stores oxidizing equivalents during catalysis by employing a Cu(I)–sulfenate intermediate with an end-on O-coordination that is unprecedented in biology.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

DOE OSTI2025

Development of interatomic potential and effect of ordering on defect properties in CrMnV

Developing materials that can withstand extreme environments, such as high radiation doses and elevated temperatures, is crucial for next-generation particle accelerators, including the 2.4 MW Long-Baseline Neutrino Facility. High-Entropy Alloys have emerged as promising candidates for beam window materials due to their superior mechanical strength, corrosion resistance, and radiation tolerance. In this study, we focus on the Cr–Mn–V alloy system, developing and employing machine-learning interatomic potentials (MLIPs) to investigate the formation of an ordered phase and its influence on defect properties. Using hybrid Monte Carlo-Molecular Dynamics simulations, we observe the formation of a B2-ordered phase at lower temperatures, consistent with Density Functional Theory (DFT) predictions. Ordered structures display a bimodal distribution of migration energies and reduced mean square displacement values, indicating suppressed vacancy diffusion. Our results also show that the migration energy barrier varies based on the atomic species, with Mn and V exhibiting the highest and lowest average barriers, respectively. These findings suggest that atomic ordering inhibits defect mobility, potentially enhancing the radiation resistance of CrMnV alloys. The validated MLIP provides a reliable framework for simulations that are faster than traditional DFT while maintaining the accuracy required to study defect and ordering properties.

36 MATERIALS SCIENCE↗

NASA NTRS2007

A Support Database System for Integrated System Health Management (ISHM)

The development, deployment, operation and maintenance of Integrated Systems Health Management (ISHM) applications require the storage and processing of tremendous amounts of low-level data. This data must be shared in a secure and cost-effective manner between developers, and processed within several heterogeneous architectures. Modern database technology allows this data to be organized efficiently, while ensuring the integrity and security of the data. The extensibility and interoperability of the current database technologies also allows for the creation of an associated support database system. A support database system provides additional capabilities by building applications on top of the database structure. These applications can then be used to support the various technologies in an ISHM architecture. This presentation and paper propose a detailed structure and application description for a support database system, called the Health Assessment Database System (HADS). The HADS provides a shared context for organizing and distributing data as well as a definition of the applications that provide the required data-driven support to ISHM. This approach provides another powerful tool for ISHM developers, while also enabling novel functionality. This functionality includes: automated firmware updating and deployment, algorithm development assistance and electronic datasheet generation. The architecture for the HADS has been developed as part of the ISHM toolset at Stennis Space Center for rocket engine testing. A detailed implementation has begun for the Methane Thruster Testbed Project (MTTP) in order to assist in developing health assessment and anomaly detection algorithms for ISHM. The structure of this implementation is shown in Figure 1. The database structure consists of three primary components: the system hierarchy model, the historical data archive and the firmware codebase. The system hierarchy model replicates the physical relationships between system elements to provide the logical context for the database. The historical data archive provides a common repository for sensor data that can be shared between developers and applications. The firmware codebase is used by the developer to organize the intelligent element firmware into atomic units which can be assembled into complete firmware for specific elements.

FROM↗

DOE OSTI2025

A bi-channel aided stitching of atomic force microscopy images

Microscopy is an essential tool in scientific research, enabling the visualization of structures at micro- and nanoscale resolutions. However, the field of microscopy often encounters limitations in field-of-view (FOV), restricting the amount of sample that can be imaged in a single capture. To overcome this limitation, image stitching techniques have been developed to seamlessly merge multiple overlapping images into a single, high-resolution composite. The images collected from microscope need to be optimally stitched before accurate physical information can be extracted from post analysis. However, the existing stitching tools either struggle to stitch images together when the microscopy images are feature sparse or cannot address all the transformations of images when performing image stitching. To address these issues, we propose a bi-channel aided feature-based image stitching method and demonstrate its use on Atomic Force Microscopy (AFM) generated Pantoea sp. YR343 biofilm and PTO thin film sample images as experimental data. The topographical channel image of AFM data captures the morphological details of the sample, and a stitched topographical image is desired for researchers. We utilize the amplitude and phase channels of AFM data to maximize the matching features and to estimate the position of the original topographical images and show that the proposed bi-channel aided stitching method outperforms the traditional direct stitching approach in AFM topographical image stitching task. Here, we demonstrated the application on AFM, but similar approaches could be employed of optical microscopy with brightfield and fluorescence channels. We believe this proposed workflow can serve as a valuable augmentation strategy for microscopy image stitching tasks and will benefit the experimentalist to avoid erroneous analysis and discovery due to incorrect stitching.

Atomic force microscopy↗

NASA NTRS2004

Disordered Zinc in Zn4Sb3 with Phonon-Glass and Electron-Crystal Thermoelectric Properties

By converting waste heat into electricity, thermoelectric generators could be an important part of the solution to today's energy challenges. The compound Zn4Sb3 is one of the most efficient thermoelectric materials known. Its high efficiency results from an extraordinarily low thermal conductivity in conjunction with the electronic structure of a heavily doped semiconductor. Previous structural studies have been unable to explain this unusual combination of properties. Here, we show through a comprehensive structural analysis using single-crystal X-ray and powder-synchrotron-radiation diffraction methods, that both the electronic and thermal properties of Zn4Sb3 can be understood in terms of unique structural features that have been previously overlooked. The identification of Sb3- ions and Sb-2(4-) dimers reveals that Zn4Sb3 is a valence semiconductor with the ideal stoichiometry Zn13Sb10. In addition, the structure contains significant disorder, with zinc atoms distributed over multiple positions. The discovery of glass-like interstitial sites uncovers a highly effective mechanism for reducing thermal conductivity. Thus Zn4Sb3 is in many ways an ideal 'phonon glass, electron crystal' thermoelectric material.

phases↗

NASA NTRS2002

Thermoelectric properties of Nb3SbxTe7-x compounds

Niobium antimony telluride, Nb3Sbx,Te7-x, was synthesized and tested for thermoelectric properties in the Thermoelectrics group at the Jet Propulsion Laboratory. The forty atoms per unit cell of Nb3Sb2Te5 and its varied mixture of atoms yield acomplicated structure, suggesting that Nb3Sb2Te5 and related compounds may exhibit low thermal conductivity and hence a higher ZT value. Nb3SbxTe7-x, compounds were synthesized and subsequently analyzed for their Seebeck voltage, heat conduction, and electrical resistivity. Results indicate that Nb3Sb2Te5 is a heavily doped semiconductor whose thermoelectric properties are compromised by compensating n-type and p-type carriers. Attempts to dope in favor of either carrier by varying the Sb:Te ratio yielded samples containing secondary metallic phases that dominated the transport properties of the resulting compounds.

thermoelectric power generation segmented↗

DOE OSTI2024

The role of Li doping in layered/layered Na x Li y Ni 0.4 Fe 0.2 Mn 0.4 O 2 intergrowth electrodes for sodium ion batteries

Here, the layered NaTMO 2 (TM = Ni, Fe, Mn) materials with the O3-type structure are attractive as positive electrodes for sodium ion batteries because of their high theoretical capacity. Additionally, Li doping in these materials has been shown to offer substantial enhancements to their electrochemical properties by promoting the formation of intergrowth structures, which are combinations of specific phases. However, the mechanism by which the intergrowth modifies the electrochemical properties is often unclear. Systematic variation of Li content in Na x Li y Ni 0.4 Fe 0.2 Mn 0.4 O 2 (NFM-Li y ) was conducted to identify its role in structural modification and electrochemical performance. Li contents of 0.15 and greater generate a layered/layered Na-O3/Li-O’3 intergrowth structure. 7 Li and 23 Na nuclear magnetic resonance and x-ray absorption spectroscopy identify that when the total solubility for alkali ions in the layered structure is exceeded, Li continues to form the Li-O’3 phase while the excess Na forms residual sodium compounds such as Na 2 O. Higher Li content is associated with improved capacity retention in the initial cycles from the superior stability of the mechanically linked NaO3/Li-O’3 structure that suppresses the P3 to OP2 phase transition during charge. However, high Li contents are associated with increased rates of parasitic side reactions that reduce long-term cycling stability. These side reactions are associated with the instability of the cathode-electrolyte interphase, which can be partially mitigated by atomic layer deposition (ALD) coating with alumina, which significantly enhances the capacity retention and Coulombic efficiency over many cycles. Overall, we find that the layered/layered Na-O3/Li-O’3 intergrowth structure is able to provide structural stability and suppress undesired phase transformations but is overwhelmed by the increased reactivity of the surface if not protected by surface coating.

25 ENERGY STORAGE↗

DOE OSTI2024

Strong Surface-Enhanced Coherent Phonon Generation in van der Waals Materials

Terahertz (THz) coherent phonons have emerged as promising candidates for the next generation of high-speed, low-energy information carriers in atomically thin phononic or phonon-integrated on-chip devices. However, effectively manipulating THz coherent phonons remains a significant challenge. Here, in this study, we investigated THz coherent phonon generation in exfoliated van der Waals (vdW) flakes of Fe 3 GeTe 2 , Fe 5 GeTe 2 , and FePS 3 . We successfully generated the THz A 1g coherent phonon mode in these vdW flakes. An innovative approach involved partially exfoliating vdW flakes on a gold substrate and partially on a silicon (Si) substrate to compare the THz coherent phonon generation between both sides. Interestingly, we observed a significantly enhanced THz coherent phonon in the vdW/gold area compared with that in the vdW/Si area. Frequency-domain Raman mapping across the vdW flakes corroborated these findings. Numerical simulations further indicated a stronger enhanced surface field in vdW/gold structures than in vdW/Si structures. Consequently, we attribute the observed enhancement in THz coherent phonon generation to the increased surface field on the gold substrate. This enhancement was consistent across the three different vdW materials studied, suggesting the universality of this strategy. Our results hold promise for advancing the design of THz phononic and phonon-integrated devices.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

DOE OSTI2024

Embracing disorder in quantum materials design

Many of the most exciting materials discoveries in fundamental condensed matter physics are made in systems hosting some degree of intrinsic disorder. While disorder has historically been regarded as something to be avoided in materials design, it is often of central importance to correlated and quantum materials. This is largely driven by the conceptual and theoretical ease to handle, predict, and understand highly uniform systems that exhibit complex interactions, symmetries, and band structures. In this Perspective, we highlight how flipping this paradigm has enabled exciting possibilities in the emerging field of high entropy materials, focusing primarily on high entropy oxide and chalcogenide quantum materials. These materials host high levels of cation or anion compositional disorder while maintaining unexpectedly uniform single crystal lattices. The diversity of atomic scale interactions of spin, charge, orbital, and lattice degrees of freedom are found to emerge into coherent properties on much larger length scales. Thus, altering the variance and magnitudes of the atomic scale properties through elemental selection can open new routes to tune global correlated phases, such as magnetism, metal–insulator transitions, ferroelectricity, and even emergent topological responses. The strategy of embracing disorder in this way provides a much broader pallet from which functional states can be designed for next-generation microelectronic and quantum information systems.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗

DOE OSTI2024

Embracing Disorder in Quantum Materials Design

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗

DOE OSTI2025

Tunable Few-Layer van der Waals Crystals and Heterostructures as Emerging Energy and Quantum Materials (Final Technical Report)

2D and layered (van der Waals) semiconductors offer extraordinary opportunities for manipulating optically excited charge carriers, many-body excitations, and non-charge based quantum numbers. To date, research has focused on a limited group of materials, mostly transition metal dichalcogenides in the monolayer limit. Other van der Waals semiconductors, and especially few-layer to multilayer crystals and their heterostructures, carry large potential for the discovery of phenomena of interest for future energy and information technologies. But they remain largely unexplored, often due to a lack of access to high-quality materials and approaches for measuring their properties at the relevant scales. The goal of this project was to develop an EPSCoR-State/National Laboratory Partnership that addresses the challenges of preparing high-quality van der Waals semiconductors and of probing their structure, composition, and especially their optoelectronic and photonic properties, near the atomic scale using electron microscopy techniques. A central component of the project was the development of advanced methods for electron microscopy and electron-excited spectroscopy, taking advantage of unique samples as well as leading capabilities and expertise at the partner institutions. Efforts to advance leading-edge techniques was supported by ancillary developments, such as precision sample preparation for electron microscopy/spectroscopy, coordinated chemical imaging, and analytical electron microscopy. Experiments in materials synthesis and technique development were closely linked to theory and computation. The results obtained under this project yielded multifaceted benefits to the involved partners and their institutions, DOE-BES, the wider scientific community, and society at large, particularly in the State of Nebraska through dividends from knowledge and human capital generated under the project.

36 MATERIALS SCIENCE↗

NASA NTRS1988

Surface compositional and structural aspects of Martian samples

There are many excellent reasons to examine the surface composition of a wide range of Martian samples. The existing spectral data indicate that many dust and soil particles have a thin Fe(+3) layer with a typical particle size in the 10 micrometer to 400 micrometer range. In view of the high CO2 content of the atmosphere, one might expect that surface carbonates should be present. In addition to chemisorbed material there will probably exist physisorbed atmospheric components of the atmosphere including oxygen, nitrogen and water vapor. The latter could possibly give rise to some hydrated minerals. Using ultra-high-vacuum/mass spectrographic techniques it should be possible to detect physisorbed and moderately strong chemisorbed species on the particle surfaces with a temperature programmed degassing procedure. In some instances such an approach is capable of helping distinguish between volcanic and impact generated materials by detecting the presence of fumerolic gases. Such gases typically condense on the exterior of the ejected particles. Additionally surface atomic and chemical compositions should be examined by a combination of modern surface analytical techniques. The combination we currently have in Buffalo at SUNY would appear to be one of the best available including ESCA (150 micrometer spot capability) Auger (SAM) with 300 A focussing for surface compositional surveys, SIMS for high sensitivity trace element detection and ISS for immediate surface layer analysis.

Cadenhead, D. A.↗

DOE OSTI2026

Weibel-mediated filamentary structures observed in the ICF context

Here, in light of novel and past experimental results, we demonstrate how Weibel-mediated filamentary structures can develop in the expanding plasma plume of a laser-irradiated foil. The transverse ballistic cooling that occurs during the quasi-spherical plasma expansion naturally drives an electron pressure anisotropy, resulting in the growth of electron current filaments. This effect competes with electron–ion Coulomb collisions, which tend to isotropize the electron distribution function. Based on theoretical and particle-in-cell modeling, we provide estimates of the dominant wavelength and amplitude of the self-generated magnetic fluctuations, which are found to explain experimental data obtained at the OMEGA and Laser Megajoule facilities.

70 PLASMA PHYSICS AND FUSION TECHNOLOGY↗