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At least 631 records · Page 35
All sourcesNASA NTRSDOE OSTI
DOE OSTI2024

In situ coherent x-ray scattering reveals polycrystalline structure and discrete annealing events in strongly coupled nanocrystal superlattices

Solution-phase bottom up self-assembly of nanocrystals into superstructures such as ordered superlattices is an attractive strategy to generate functional materials of increasing complexity, including very recent advances that incorporate strong interparticle electronic coupling. While the self-assembly kinetics in these systems have been elucidated and related to the product characteristics, the weak interparticle bonding interactions suggest the superstructures formed could continue to order within the solution long after the primary nucleation and growth have occurred, even though the mechanism of annealing remains to be elucidated. Here, we use a combination of Bragg coherent diffractive imaging and x-ray photon correlation spectroscopy to create real-space maps of supercrystalline order along with a real-time view of the strain fluctuations in aging strongly coupled nanocrystal superlattices while they remain suspended and immobilized in solution. By combining the results, we deduce that the self-assembled superstructures are polycrystalline, initially comprising multiple nucleation sites, and that shear avalanches at grain boundaries continue to increase crystallinity long after growth has substantially slowed. This multimodal approach should be generalizable to characterize a breadth of materials in their native chemical environments, thus extending the reach of high-resolution coherent x-ray characterization to the benefit of a much wider range of physical systems. Published by the American Physical Society 2024

36 MATERIALS SCIENCE↗
DOE OSTI2025

Li 21 Ge 8 P 3 S 34 : New Lithium Superionic Conductor with Unprecedented Structural Type

Abstract Lithium superionic conductors are pivotal for enabling all‐solid‐state batteries, which aim to replace liquid electrolytes and enhance safety. Herein, we report the discovery of an unprecedented lithium superionic conductor, Li 21 Ge 8 P 3 S 34 , featuring a novel structural type and a new composition in the Li–Ge–P–S system. This material exhibits high lithium ionic conductivity of approximately 1.0 mS cm −1 at 303 K with a low activation energy of 0.20(1) eV. It's unique crystal structure was elucidated using three‐dimensional electron diffraction (3D ED) and further refined through combined powder X‐ray and neutron diffraction analyses. The structure consists of alternating two‐dimensional slabs: one of corner‐sharing GeS 4 tetrahedra and the other of isolated PS 4 tetrahedra, enabling efficient lithium‐ion transport through a tetrahedrally interconnected network of 1D, 2D, and 3D diffusion pathways. This distinctive structural motif provides a novel design strategy for next‐generation solid electrolytes, broadening the structural landscape of lithium superionic conductors. With further advancements in compositional tuning and interfacial engineering, Li 21 Ge 8 P 3 S 34 could contribute to the development of high‐performance all‐solid‐state batteries.

Chemistry↗
DOE OSTI2023

A review of in situ/operando studies of heterogeneous catalytic hydrogenation of CO 2 to methanol

Repurposing CO 2 into chemicals, one of the Carbon Dioxide Removal (CDR) strategies, still faces significant challenges in conversion and energy efficiency due to the lack of effective catalysts and processes. Fundamental understanding through in situ/operando investigations of the reaction mechanisms and catalyst structures is pivotal for developing the efficient catalysts. This paper reviews the past and recent in situ/operando studies of methanol synthesis from heterogeneous CO 2 hydrogenation over a few typical catalysts including Cu-based, oxide-based, and noble-metal-based catalysts. With the development of high-pressure reactors, in situ/operando IR, X-ray absorption spectroscopy (XAS), X-ray diffraction (XRD), neutron diffraction and imaging have been used to reveal the surface intermediates and structures of working catalysts under CO 2 hydrogenation conditions. On the one hand, the combined operando techniques shed light on working mechanisms for some catalytic systems. On the other hand, due to the complexity of selective CO 2 hydrogenation reaction and limited sensitivity of current accessible operando techniques to the surface structure of catalysts, it is still murky about the exact nature of the active sites at the surface/interface and how different sites promote different reaction paths. Furthermore, it is concluded that new methodologies for differentiating signals from different sites, and the development of surface-sensitive techniques for high pressure reactions are needed for providing structural descriptors of highly active and selective CO 2 conversion catalysts.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2022

Engineering Nanostructured Interfaces of Hexagonal Boron Nitride-Based Materials for Enhanced Catalysis

Hexagonal boron nitrides (h-BNs) are attractive two-dimensional (2D) nanomaterials that consist of alternating B and N atoms and layered honeycomb-like structures similar to graphene. They have exhibited unique properties and promising application potentials in the field of energy storage and transformation. Recent advances in utilizing h-BN as a metal-free catalyst in the oxidative dehydrogenation of propane have triggered broad interests in exploring h-BN in catalysis. However, h-BN-based materials as robust nanocatalysts in heterogeneous catalysis are still underexplored because of the limited methodologies capable of affording h-BN with controllable crystallinity, abundant porosity, high purity, and defect engineering, which played important roles in tuning their catalytic performance. Here, in this account, our recent progress in addressing the above issues will be highlighted, including the synthesis of high-quality h-BN-based nanomaterials via both bottom-up and top-down pathways and their catalytic utilization as metal-free catalysts or as supports to tune the interfacial electronic properties on the metal nanoparticles (NPs). First, we will focus on the large-scale fabrication of h-BN nanosheets (h-BNNSs) with high crystallinity, improved surface area, satisfactory purity, and tunable defects. h-BN derived from the traditional approaches using boron trioxide and urea as the starting materials generally contains carbon/oxygen impurities and has low crystallinity. Several new strategies were developed to address the issues. Using bulk h-BN as the precursor via gas exfoliation in liquid nitrogen, single- or few-layered h-BNNS with abundant defects could be generated. Amorphous h-BN precursors could be converted to h-BN nanosheets with high crystallinity assisted by a magnesium metallic flux via a successive dissolution/precipitation/crystallization procedure. The as-fabricated h-BNNS featured high crystallinity and purity as well as abundant porosity. An ionothermal metathesis procedure was developed using inorganic molten salts (NaNH 2 and NaBH 4 ) as the precursors. The h-BN scaffolds could be produced on a large scale with high yield, and the as-afforded materials possessed high purity and crystallinity. Second, utilization of the as-prepared h-BN library as metal-free catalysts in dehydrogenation and hydrogenation reactions will be summarized, in which they exhibited enhanced catalytic activity over the counterparts from the previous synthesis method. Third, the interface modulation between metal NPs with the as-prepared defects’ abundant h-BN support will be highlighted. The h-BN-based strong metal–support interaction (SMSI) nanocatalysts were constructed without involving reducible metal oxides via the ionothermal procedure we developed by deploying specific inorganic metal salts, acting as robust nanocatalysts in CO oxidation. Under conditions simulated for practical exhaust systems, promising catalytic efficiency together with high thermal stability and sintering resistance was achieved. Across all of these examples, unique insights into structures, defects, and interfaces that emerge from in-depth characterization through microscopy, spectroscopy, and diffraction will be highlighted.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2024

High-Pressure Melting Experiments of Fe 3 C and a Thermodynamic Model of Fe-C Liquids for the Earth's Core

Melting experiments of Fe 3 C were conducted to 85 GPa in laser-heated diamond anvil cells with in situ X-ray diffraction and post-experiment textural observation. From the determined pressure-temperature conditions of the melting curve for Fe 3 C, together with literature data on the melting point of diamond and eutectic point of the system Fe-Fe 3 C/Fe 7 C 3 under high pressures, we established a self-consistent thermodynamic model for high-pressure melting of the system Fe-C including the mixing parameters for liquids. The results show that mixing of Fe and C liquids is negatively nonideal from 1 bar to the pressure at the center of the Earth. The departure from ideal mixing becomes progressively larger with increasing pressure, which leads to greatly stabilized liquids under core pressures. The modeled carbon content in eutectic melts under core pressures is 3.3–4.4 wt%. From the Gibbs free energy, we derived an internally consistent parameters for Fe-C outer cores which included the crystallizing points at their bottoms, isentropic thermal profiles, and densities and longitudinal seismic wave speeds (Vp). While the addition of carbon in excess of the eutectic melt composition effectively reduces the density of iron liquid, the Vp of iron liquid is not greatly changed. Therefore, the low density and high Vp of PREM relative to pure iron cannot be reconciled by an Fe-C liquid. Therefore, the Earth's core cannot be approximated by the system Fe-C and should include another light element.

58 GEOSCIENCES↗
DOE OSTI2022

HP-PdF2-type FeCl2 as a potential Cl-carrier in the deep Earth

Here, we report for the first time the formation of a HP-PdF 2 -type FeCl 2 phase (space group Pa$\bar{3}$), through high pressure-temperature (P-T) reactions in the hydrous systems (Mg 0.6 Fe 0.4 )SiO 3 –H 2 O–NaCl and FeO2H–NaCl in a laser-heated diamond-anvil cell up to 108 GPa and 2000 K. Applying single-crystal X-ray diffraction (XRD) analysis to individual submicrometer-sized grains, we have successfully determined the crystal structure of the as-synthesized FeCl 2 phase, in agreement with our theoretical structure search results. In situ high P-T XRD data revealed the substitution of Cl for OH(O) in such a cubic Pa$\bar{3}$ structure, demonstrating that this topology is a potential host for both H and Cl in the deep Earth. The chemical analysis of the recovered sample showed that the post-perovskite phase contains considerable amounts of Na 2 O and Fe 2 O 3 . The coexistence of the cubic FeCl 2 phase and post-perovskite suggests that the lowermost mantle could be a potential reservoir of Cl. The possible presence of volatiles such as H and Cl in the deep lower mantle would impact the composition and iron valence state of the post-perovskite phase.

58 GEOSCIENCES↗
DOE OSTI2025

Effect of moisture ingression on material performance and particle generation in molten salts

This report summarizes activities conducted to understand and mitigate the negative consequences that moisture ingressions have upon the operations of pyroprocessing equipment. The objectives of the work conducted in FY25 were to characterize (1) the physicochemical properties of particles generated as a result of moisture ingressions, and (2) the corrosion of relevant structural materials with the introduction of moisture. Compositional and morphological analyses of the generated particles were conducted through a suite of characterization technologies, including X-ray diffraction, microscopy, and particle size analysis. The results gathered this year were compared to those obtained in FY24 when studies with oxygen ingressions were conducted on CeCl 3 -LiCl-KCl and UCl 3 -LiCl-KCl systems. Investigations involving performance evaluations of industrially relevant structural alloys were also conducted under moisture ingress conditions. In-line electrochemical monitoring of the bulk salt was augmented with microscopy of alloy samples to quantify the concentration and accumulation of corrosion products in the bulk salt. The results reported in this work provide a more holistic understanding of the effects of atmospheric ingressions on molten chloride salt chemistry such that effective redox control strategies may be implemented.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗
DOE OSTI2026

A Compact Cryogenic Environment for In Situ Neutron Diffraction Under Mechanical Loading

Understanding the deformation mechanisms of materials at cryogenic temperatures is crucial for cryogenic engineering applications. In situ neutron diffraction is a powerful technique for probing such mechanisms under cryogenic conditions. In this study, we present the development of a compact cryogenic environment (CCE) designed to facil-itate in situ neutron diffraction experiments under mechanical loading at tempera-tures as low as 77 K. The CCE features a polystyrene foam cryogenic chamber, alumi-num blocks serving as neutron-transparent cold sinks, a liquid nitrogen dosing system for cryogen delivery, a nitrogen gas flow control system for thermal management, a process controller for temperature control, and a pair of thermally isolated grip adapt-ers for mechanical testing. The CCE achieves reliable temperature control with mini-mal neutron attenuation. Utilizing this setup, we conducted three in situ neutron dif-fraction tensile tests on a 316L stainless steel at 77 , 173 , and 298 K, respectively. The results highlight the pronounced effects of cryogenic temperatures on the material's deformation mechanisms, underscoring both the significance of cryogenic deformation studies and the effectiveness of the CCE.

Yu, Dunji [ORNL] (ORCID:0000000189467851)↗
DOE OSTI2025

Massive compression for high data rate macromolecular crystallography (HDRMX): impact on diffraction data and subsequent structural analysis

New higher-count-rate, integrating, large-area X-ray detectors with framing rates as high as 17400 images per second are beginning to be available. These will soon be used for specialized macromolecular crystallography experiments but will require optimal lossy compression algorithms to enable systems to keep up with data throughput. Some information may be lost. Can we minimize this loss with acceptable impact on structural information? To explore this question, we have considered several approaches: summing short sequences of images, binning to create the effect of larger pixels, use of JPEG-2000 lossy wavelet-based compression, and use of Hcompress, which is a Haar-wavelet-based lossy compression borrowed from astronomy. We also explore the effect of the combination of summing, binning, and Hcompress or JPEG-2000. In each of these last two methods one can specify approximately how much one wants the result to be compressed from the starting file size. These provide particularly effective lossy compressions that retain essential information for structure solution from Bragg reflections.

47 OTHER INSTRUMENTATION↗
DOE OSTI2024

Magneto-transport study on Sn-rich Sn 1–x Ge x thin films enabled by CdTe buffer layer

α-Sn, generally known as gray tin, has attracted significant scientific interest due to its potential to host novel topological phases. Studying the transport properties of α-Sn thin films grown on the InSb substrate has been challenging, as the InSb substrate also significantly contributes to the transport properties. In this article, we report a novel approach to epitaxially grow α-Sn thin films on an InSb substrate with a resistive buffer layer of CdTe. Thin films of α–Sn 1–x Ge x (x = 0, 0.025) alloy of 15 nm thickness have been grown using molecular beam epitaxy. The high quality of the samples has been determined through high-resolution x-ray diffraction. The CdTe buffer layer has high resistance and acts as an insulating virtual substrate, which significantly suppresses contribution from InSb. Magnetotransport measurements show clear Shubnikov–de Hass oscillations in α–Sn 1–x Ge x (x = 0, 0.025) thin films. A change in oscillation frequency is observed upon alloying with Ge, implying a modification in the electronic structure and demonstrating the effectiveness of the CdTe buffer layer approach. Furthermore, this work provides a new approach that enables the electronic transport characterization of the α–Sn 1–x Ge x alloy system, which enables the study of the topological quantum states using electronic transport and their device applications.

36 MATERIALS SCIENCE↗
DOE OSTI2023

Ultrafast X-Ray Scattering Reveals Composite Amplitude Collective Mode in the Weyl Charge Density Wave Material ( TaSe 4 ) 2 I

Here we report ultrafast x-ray scattering experiments of the quasi-1D charge density wave (CDW) material (TaSe 4 ) 2⁢ I following ultrafast infrared photoexcitation. From the time-dependent diffraction signal at the CDW sidebands we identify a 0.11 THz amplitude mode derived primarily from a transverse acoustic mode of the high-symmetry structure. From our measurements we determine that this mode interacts with the valence charge indirectly through another collective mode, and that the CDW system in (TaSe 4 ) 2 ⁢I has a composite nature supporting multiple dynamically active structural degrees of freedom.

36 MATERIALS SCIENCE↗
DOE OSTI2026

Predominant Proton Insertion during Electrochemical Cycling of ε-VOPO 4 in a Nonaqueous Ca-Ion Electrolyte

Calcium-ion batteries (CIBs) are promising for next-generation energy storage systems. However, many reported Ca-ion storage mechanisms lack direct structural evidence, raising concerns that the observed electrochemistry may instead originate from proton insertion. Herein, we investigate the electrochemical cycling of a VOPO 4 electrode in an aprotic Ca electrolyte with trace water to clarify the charge storage mechanism. While electrochemistry, elemental analysis, and X-ray absorption spectroscopy seem to support Ca-ion intercalation in the VOPO 4 electrode, X-ray diffraction and electron microscopy unequivocally show proton insertion as the predominant charge storage mechanism. The apparent variation of Ca content in the electrode with the state of charge is attributed to the formation and dissolution of Ca-containing precipitates on the surface of VOPO 4 particles. Our work demonstrates the propensity of proton participation in the intercalation reaction in Ca-ion batteries and the necessity of structural evidence in understanding reactions in multivalent electrochemical systems.

Wang, Jiwei [Binghamton University, NY (United Sta↗
DOE OSTI2025

Computing virtual dark-field X-ray microscopy images of complex discrete dislocation structures from large-scale molecular dynamics simulations

Dark-field X-ray microscopy (DFXM) is a novel diffraction-based imaging technique that non-destructively maps the local deformation from crystalline defects in bulk materials. While studies have demonstrated that DFXM can spatially map 3D defect geometries, it is still challenging to interpret DFXM images of the high-dislocation-density systems relevant to macroscopic crystal plasticity. This work develops a scalable forward model to calculate virtual DFXM images for complex discrete dislocation structure(s) (DDS) obtained from atomistic simulations. Our new DDS-DFXM model integrates a non-singular formulation for calculating the local strain from the DDS and an efficient geometrical optics algorithm for computing the DFXM image from the strain field. We apply the model to complex DDS obtained from a large-scale mol­ecular dynamics simulation of compressive loading on single-crystal silicon. Simulated DFXM images exhibit prominent contrast for dislocation features between the multiple slip systems, demonstrating the potential of DFXM to resolve features from dislocation multiplication. In conclusion, the integrated DDS-DFXM model provides a toolbox for DFXM experimental design and image interpretation in the context of bulk crystal plasticity for a range of measurements across shock plasticity and the broader materials science community.

X-ray imaging↗
DOE OSTI2020

Correlations between electronic order and structural distortions and their ultrafast dynamics in the single-layer manganite P r 0.5 C a 1.5 Mn O 4

Time-resolved x-ray diffraction experiments on the half-doped single-layered manganite Pr 0.5 Ca 1.5 Mn O 4 are used to monitor the ultrafast photoinduced dynamics of the structural distortion associated with the charge and orbital ordering (CO/OO). As in the nonlayered three-dimensional counterpart, the ordered phase melts in less than 100 fs after 800-nm photoexcitation and subsequently partially recovers due to thermal equilibration of electronic and vibrational systems. Photoexciting Pr 0.5 Ca 1.5 Mn O 4 below the transition temperature of a second structural phase transition that occurs around 146 K (deep inside the CO/OO phase) releases this structural transition, but progresses on a much slower timescale. Finally, this additional reduction of crystal symmetry, which we ascribe to a further tilt of the oxygen octahedra, can thus be considered to be only weakly coupled to CO/OO. Furthermore, static hard-x-ray and resonant soft-x-ray diffraction at the Mn L 2,3 edges experiments identify correlations between structural distortions and electronic order in thermal equilibrium.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗
DOE OSTI2023

FIRST RESULTS FROM Nb3Sn COATINGS OF 2.6 GHz Nb SRF CAVITIES USING DC CYLINDRICAL MAGNETRON SPUTTERING SYSTEM

A DC cylindrical magnetron sputtering system has been commissioned and operated to deposit Nb3Sn onto 2.6 GHz Nb SRF cavities. After optimizing the deposition conditions in a mock-up cavity, Nb-Sn films are deposited first on flat samples by multilayer sequential sputtering of Nb and Sn, and later annealed at 950 °C for 3 hours. X-ray diffraction of the films showed multiple peaks for the Nb3Sn phase and Nb (substrate). No peaks from any Nb-Sn compound other than Nb3Sn were detected. Later three 2.6 GHz Nb SRF cavities are coated with ~1 µm thick Nb3Sn. The first Nb3Sn coated cavity reached close to Eacc = 8 MV/m, demonstrating a quality factor Q0 of 3.2 × 108 at Tbath = 4.4 K and Eacc = 5 MV/m, about a factor of three higher than that of Nb at this temperature. Q0 was close to 1.1 × 109, dominated by the residual resistance, at 2 K and Eacc = 5 MV/m. The Nb3Sn coated cavities demonstrated Tc in the range of 17.9 ? 18 K. Here, we present the commissioning experience, system optimization, and the first results from the Nb3Sn fabrication on flat samples and SRF cavities.

Shakel, M.S.↗
DOE OSTI2023

FIRST RESULTS FROM Nb3Sn COATINGS OF 2.6 GHz Nb SRF CAVITIES USING DC CYLINDRICAL MAGNETRON SPUTTERING SYSTEM

A DC cylindrical magnetron sputtering system has been commissioned and operated to deposit Nb3Sn onto 2.6 GHz Nb SRF cavities. After optimizing the deposition conditions in a mock-up cavity, Nb-Sn films are deposited first on flat samples by multilayer sequential sputtering of Nb and Sn, and later annealed at 950 °C for 3 hours. X-ray diffraction of the films showed multiple peaks for the Nb3Sn phase and Nb (substrate). No peaks from any Nb-Sn compound other than Nb3Sn were detected. Later three 2.6 GHz Nb SRF cavities are coated with ~1 µm thick Nb3Sn. The first Nb3Sn coated cavity reached close to Eacc = 8 MV/m, demonstrating a quality factor Q0 of 3.2 × 108 at Tbath = 4.4 K and Eacc = 5 MV/m, about a factor of three higher than that of Nb at this temperature. Q0 was close to 1.1 × 109, dominated by the residual resistance, at 2 K and Eacc = 5 MV/m. The Nb3Sn coated cavities demonstrated Tc in the range of 17.9 ? 18 K. Here, we present the commissioning experience, system optimization, and the first results from the Nb3Sn fabrication on flat samples and SRF cavities.

Shakel, M. S.↗
DOE OSTI2023

Tetracopper σ‐Bound μ ‐Acetylide and ‐Diyne Units Stabilized by a Naphthyridine‐based Dinucleating Ligand

Abstract Reactions of a dicopper(I) tert ‐butoxide complex with alkynes possessing boryl or silyl capping groups resulted in formation of unprecedented tetracopper(I) μ ‐acetylide/diyne complexes that were characterized by NMR and UV/Vis spectroscopy, mass spectrometry and single‐crystal X‐ray diffraction. These compounds possess an unusual μ 4 ‐ η 1 : η 1 : η 1 : η 1 coordination mode for the bridging organic fragment, enforced by the rigid and dinucleating nature of the ligand utilized. Thus, the central π system remains unperturbed and accessible for subsequent reactivity and modification. This has been corroborated by addition of a fifth copper atom, giving rise to a pentacopper acetylide complex. This work may provide a new approach by which metal‐metal cooperativity can be exploited in the transformation of acetylide and diyne groups to a variety of substrates, or as a starting point for the controlled synthesis of copper(I) alkyne‐containing clusters.

Ríos, Pablo↗