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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 307 records · Page 17
All sourcesNASA NTRSDOE OSTI
DOE OSTI2021

Advanced inorganic halide ceramic scintillators

Research in ceramic scintillators has steadily progressed alongside the research in bulk single crystal scintillator growth. As interest in faster scintillation material production with lower cost increases, more research on scintillating ceramics is needed. Research targeting optimization of optically transparent ceramics that can rival bulk-grown crystals grown may lower cost, increase yield, increase volume, and improve energy resolution in applications and systems currently using sodium iodide and alike. Ceramic scintillators that are dense (>5 g/cm 3 ), have high effective Z (>60), are bright (>40,000 photons/MeV), and are not sensitive to moisture as well as those that can be handled without protection are desired. Ultra-fast ceramic materials are also of interest. This paper presents an equipment design and technique to produce inorganic halide ceramic scintillators Cs 2 HfCl 6 (CHC) and Tl 2 HfCl 6 (THC). Improvements and optimization of CHC and THC ceramic scintillator fabrication are gauged by monitoring the energy resolution and peak position of 137 Cs full energy peak at 662 keV. With a 1-inch diameter CHC ceramic scintillator, energy resolution of 5.4% (FWHM) and light yield of 20,700 ph/MeV are achieved, while with a 16-mm diameter THC ceramic scintillator, energy resolution of 5.1% (FWHM) and light yield of 27,800 ph/MeV are achieved. Decay times of 0.6 μs (21%) and 3.0 μs (79%) are measured for CHC and 0.3 μs (13%) and 1.0 μs (87%) for THC. Here, both ceramic CHC and THC scintillators have similarly good proportionality data when compared to their single crystal counterparts.

36 MATERIALS SCIENCE↗
DOE OSTI2023

Floating zone crystal growth, structure, and properties of a cubic Li 5.5 La 3 Nb 1.5 Zr 0.5 O 12 garnet-type lithium-ion conductor

As a promising candidate for solid-state electrolytes in Li-ion batteries, the garnet-type Li-ion conductor series Li 5+x La 3 Nb 2-x Zr x O 12 (LLNZO) (0 ≤ x ≤ 2) exhibits high ionic conductivity at room temperature. However, no previous single-crystal growth or characterization has been reported for LLNZO compositions 0 ≤ x ≤ 1. To obtain a complete understanding of the trend in the structure–property relationship in this class of materials, we used the floating zone (FZ) method to grow a single crystal of Li 5.5 La 3 Nb 1.5 Zr 0.5 O 12 that was 4 mm in diameter and 10 mm in length. Using Laue neutron single-crystal diffraction, two distinct Li sites were observed: tetrahedral 24d and octahedral 96h sites. The maximum entropy method (MEM) based on neutron single-crystal diffraction data was used to map Li nuclear density and estimate that the bottleneck of Li transport exists between neighboring tetrahedral and octahedral sites, and that Li is delocalized between split octahedral sites. Room-temperature Li-ion conductivity in Li 5.5 La 3 Nb 1.5 Zr 0.5 O 12 measured with electrochemical impedance spectroscopy (EIS) was 1.37 × 10 -4 S cm -1 . The Li migration activation energy was estimated to be 0.50 eV from EIS and 0.47 eV from dielectric relaxation measurements. The Li-ion jump attempt rate was estimated to be 1.47 × 10 12 Hz while the time scale of successful migration is 10 -7 to 10 -6 s.

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

Synthesis and structure of carbon-doped H 3 S compounds at high pressure

Understanding of recently reported putative close-to-room-temperature superconductivity in C-S-H compounds at 267 GPa demands a reproducible synthesis protocol as well as knowledge of the compounds' structure and composition. Here, we synthesized C-S-H compounds with various carbon compositions at high pressures from elemental carbon C and methane CH 4 , sulfur S, and molecular hydrogen H 2 . Here, we focus on compounds synthesized using methane as these allow a straightforward determination of their structure and composition by combining single-crystal x-ray diffraction and Raman spectroscopy. We applied a two-stage synthesis of [(CH 4 ) x (H 2 S) (1-x) ] 2 H 2 compounds with various compositions by first reacting sulfur and mixed methane-hydrogen fluids and forming CH 4 -doped H 2 S crystals at 0.5-3 GPa and then by growing single crystals of the desired hydrogen-rich compound. Raman spectroscopy applied to this material shows the presence of CH 4 molecules incorporated into the lattice and allows the determination of the CH 4 content, while single-crystal x-ray diffraction results suggest that the methane molecules substitute H 2 S molecules. The structural behavior of these compounds is very similar to the previously investigated methane-free crystals demonstrating a transition from Al 2 Cu type I4/mcm molecular crystal to a modulated molecular structure at 20-30 GPa and back to the same basic I4/mcm structure in an extended modification with greatly modified Raman spectra. This latter phase demonstrates a distortion into a Pnma structure at 132-159 GPa and then transforms into a common Im$\bar{3}$m H 3 S phase at higher pressures; however, no structural anomaly is detected near 220 GPa, where a sharp upturn in T c has been reported.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗
DOE OSTI2022

Active and passive defects in tetragonal tungsten bronze relaxor ferroelectrics

Tetragonal tungsten bronze (TTB) based oxides constitute a large family of dielectric materials which are known to exhibit complex distortions producing incommensurately modulated superstructures as well as significant local deviations from their average symmetry. The local deviations produce diffuse scattering in diffraction experiments. The structure as well as the charge dynamics of these materials are anticipated to be sensitive to defects, such as cation or oxygen vacancies. In this work, in an effort to understand how the structural and charge dynamical properties respond to these two types of vacancy defects, we have performed measurements of dielectric susceptibilities and single crystal diffraction experiments of two types of TTB materials with both ‘filled’ (Ba 2 NdFeNb 4 O 15 and Ba 2 PrFeNb 4 O 15 ) and ‘unfilled’ (Sr 0.5 Ba 0.5 Nb 2 O 6 ) cation sublattices. We also perform these measurements before and after oxygen annealing, which alters the oxygen vacancy concentrations. Surprisingly, we find that many of the diffuse scattering features that are present in the unfilled structure are also present in the filled structure, suggesting that the random fields and disorder that are characteristic of the unfilled structure are not responsible for many of the local structural features that are reflected in the diffuse scattering. Furthermore, oxygen annealing clearly affected both color and dielectric properties, consistent with a diminishment of the oxygen vacancy concentration, but had little effect on observed diffuse patterns.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗
DOE OSTI2025

Regioisomer-Specific Crystallization of Diglycidyl Ether of Bisphenol F Epoxy Resin

Diglycidyl ether of bisphenol F (DGEBF) is a common industrial epoxy resin, desired for its possible replacement of the bisphenol A (BPA) analogue DGEBA due to potential health hazards of BPA. During curing, crystallization of the DGEBF resin can cause inaccurate resin-to-hardener ratios, resulting in incomplete crosslinking; therefore, understanding the crystallization of DGEBF is important for proper industrial control of the material. Here, in this work, we utilized a combination of single-crystal x-ray diffraction, Raman spectroscopy, and 1 H-NMR to investigate the crystallization of DGEBF. We observed crystallization of two DGEBF regioisomers: ortho-ortho’-DGEBF and ortho-para’-DGEBF, and report their crystal structures. Notably, para-para’-DGEBF crystallization is not observed, indicating crystallization of this regioisomer does not occur under ambient conditions. Density functional theory calculations were performed to describe the phonon modes of the ortho-ortho’- and ortho-para’-DGEBF structures, corroborating Raman signatures for the respective isomers. Using a phonon mode analysis, we identify the presence of three specific optical vibrational modes at 631.3, 344.1, and 345.6 cm -1 that are unique to the para monomer. This work offers insights into the crystallization behavior of DGEBF resins under ambient conditions and may inform potential industrial application of this material.

Neu, Jennifer [Oak Ridge National Laboratory (ORNL↗
DOE OSTI2021

Topological approach to electron correlations at fractional quantum Hall effect

Highlights: • Braids in 2D electron systems in magnetic field acquire a cyclotron metrics. • Commensurability of 2D braids with Wigner crystal of electrons leads to FQHE. • Homotopy invariants define the hierarchy of FQHE universal in all 2D Hall systems. • Composite fermions illustrate multiloop braids in the simplest homotopy case. • Correlations in FQHE reveal long-range quantum entanglement of all electrons. The classification of homotopy invariants in interacting multi-electron 2D systems at quantizing magnetic fields is presented, explaining the topologically protected correlations occurring at integer and fractional quantum Hall effects. The long-range quantum entanglement is essential for homotopy correlated phases in contrast to the binary entanglement for conventional phases with local order parameters. The classification of homotopy long-range correlated phases induced by the Coulomb interaction of electrons has been derived in terms of homotopy invariants, which are universal and robust against local disorder and single-particle crystal field, as illustrated by experimental observations in various materials with different microscopic structure, like GaAs 2DES, graphene monolayer and bilayer and in Chern topological insulators. The homotopy phases are demonstrated to be topologically protected and immune to single-particle perturbations, temperature chaos and variation of the electron interaction strength. The nonzero repulsive interaction between electrons is shown, however, to be essential for the definition of the homotopy invariants, which disappear in gaseous systems.

71 CLASSICAL AND QUANTUM MECHANICS, GENERAL PHYSIC↗
DOE OSTI2020

Cryo-quenched Fe–Ni–Cr alloy decorative steel single crystals II: Alloy phases, structure, hardness, tensile, tribological, magnetic and electronic properties

We have previously reported (Boatner et al., J. Alloys Compd. 691 (2017) 666–671) on the discovery, formation, processing, and application of a new decorative ternary steel alloy and on its use in a wide range of practical applications including: custom and commercial knives, art objects, jewelry, electronics, and furniture. This decorative property results when polished single crystals of the 70 wt%Fe-15 wt%Ni-15 wt% Cr austenitic alloy are cryo-quenched into the martensitic phase resulting in the formation of a three-dimensional raised pattern of mixed austenitic/martensitic laths. These laths propagate across large dimensions of the material due to the absence of grain boundaries in the single crystal. The macroscopic optically reflective 3-D decorative pattern reproduces the structural symmetry inherent in the single-crystal orientation. This pattern results solely from the metallurgical phase properties of the ternary alloy and is completely distinct from the properties of Damascus steels or more modern so-called pattern-welded steels. Here we use X-ray diffraction, nanoindentation, hardness measurements/scratch testing, tribological measurements, and alloy resistivity and magnetization methods to obtain a more fundamental and comprehensive study of the effects of the austenitic/martensitic phase transition on the structural and physical properties of the 70 wt%Fe-15 wt%Ni-15 wt% Cr alloy. These results reveal new insight into irreversible phenomena that are associated with the inhibited phase transition on heating of the two-phase, mixed austenitic/martensitic structure that is formed subsequent to cryo-quenching the alloy crystal to 77 K.

36 MATERIALS SCIENCE↗
DOE OSTI2023

Optimization of La 2–x Sr x CuO 4 Single Crystal Film Growth via Molecular Beam Epitaxy

Atomic layer-by-layer molecular beam epitaxy (ALL-MBE) combined with ozone is one of the best methods to fabricate single-crystal thin films of complex oxides. Cuprate such as La 2-x Sr x CuO 4 (LSCO) is a representative complex-oxide high-temperature superconductor (HTS) material. Our group utilizes this method to produce high-quality single-crystal HTS films with atomically smooth surfaces and interfaces. In addition, ALL-MBE enables us to engineer multilayer heterostructures with atomic precision. This allows the fabrication of tunnel junctions, various nanostructures, and other HTS devices of interest for superconducting electronics. We have synthesized over three thousand LSCO thin films in the past two decades. These films’ structural and electronic properties have been studied and characterized by various methods. Here, we distill the extensive experience we accumulated into a step-by-step protocol to fabricate atomically perfect LSCO films. The recipe includes substrate preparation, ozone generation and distillation, source calibration, the in situ monitoring of the film synthesis, post-growth annealing, and ex situ characterization. It discloses a reproducible way to fabricate single-crystal LSCO films for basic research and HTS electronic applications.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗
DOE OSTI2025

Understanding the Effect of Sample Geometry on Temperature Distribution during Optical Floating Zone Crystal Growth in Vacuum Environment through Heat Transfer Modeling

Optical floating zone furnaces (OFZ) have had a transformative impact on fundamental science due to their ability to rapidly produce large single crystals of a wide variety of complex materials. However, a quantitative understanding of the OFZ growth environment is generally lacking due to the difficulty of measuring the local sample temperatures during OFZ growth, as well as to the general lack of information about the temperature-dependent physical parameters needed to model heat transfer. To overcome these challenges, we apply a physics-based heat transfer model, parametrized by measurements from synchrotron experiments and a machine-learning (ML) algorithm, to simulate the temperature distributions of samples heated in an OFZ furnace in a vacuum environment. This model is used to quantitatively understand how the sample maximum temperature and temperature gradient (key parameters that influence the success of crystal growth) are affected by the rod size, rod shape, and heat-zone position on the rod. The results of this study can be applied to make informed decisions on how crystal growth parameters can be tuned to modify temperature profiles and to optimize crystal growth outcomes even when data on internal sample temperature profiles (e.g., those obtained through in situ synchrotron experiments) are not accessible.

36 MATERIALS SCIENCE↗
DOE OSTI2026

Ambient Aging of Epitaxial and Polycrystalline Rhenium Thin Films

Extending the lifetime of superconducting qubits requires materials that are resistant to surface oxide formation. Rhenium has emerged as one such promising material. Because grain boundaries can promote material degradation, this project compares epitaxial (single-crystal, no grain boundaries) and polycrystalline (many grain boundaries) rhenium thin films after three years of ambient environmental exposure. Epitaxial rhenium remained free of undesired particles, while polycrystalline rhenium developed higher-oxide surface particles. Epitaxial rhenium demonstrated greater resistance to aging and oxidation, making it a more promising candidate for superconducting qubits. Surface characterization using scanning electron microscopy, energy dispersive x-ray spectroscopy, and x-ray photoelectron spectroscopy revealed localized oxygen and nitrogen enrichment together with a Re⁷⁺ oxidation state in the polycrystalline surface particles, consistent with the proposed formation of ammonium perrhenate. Ongoing cleaning and XPS depth profiling will further determine the identity and origin of the surface crystallites.

Wiacek, Wiktoria [William Rainey Harper Coll.]↗
DOE OSTI2026

Ambient Aging of Epitaxial and Polycrystalline Rhenium Thin Films

Extending the lifetime of superconducting qubits requires materials that are resistant to surface oxidation. Rhenium has emerged as one such promising candidate that forms a sub-nanometer oxide. Grain boundaries are known to promote material degradation, and thus, we compare epitaxial (single crystal, no grain boundaries) and polycrystalline (many grain boundaries) rhenium thin films after three years of ambient environmental exposure. Epitaxial rhenium remained free of undesired particles, while polycrystalline rhenium developed surface oxide crystallites. Surface characterization using scanning electron microscopy, energy dispersive x-ray spectroscopy, and x-ray photoelectron spectroscopy reveals localized oxygen and nitrogen enrichment, together with a Re⁷⁺ oxidation state in the polycrystalline surface particles, consistent with the proposed formation of ammonium perrhenate. Epitaxial rhenium demonstrated greater resistance to aging and oxidation, making it a more promising candidate for superconducting qubits. Ongoing cleaning and XPS depth profiling will further determine the identity and origin of the surface crystallites.

Wiacek, Wiktoria [Fermilab]↗
DOE OSTI2026

Ambient Aging of Epitaxial and Polycrystalline Rhenium Thin Films

Extending the lifetime of superconducting qubits requires materials that are resistant to surface oxidation. Rhenium has emerged as one such promising candidate that forms a sub-nanometer oxide. Grain boundaries are known to promote material degradation, and thus we compared epitaxial (single crystal, no grain boundaries) and polycrystalline (many grain boundaries) rhenium thin films after three years of ambient environmental exposure. Epitaxial rhenium remained free of undesired particles, while polycrystalline rhenium developed surface oxide crystallites. Surface characterization using scanning electron microscopy, energy dispersive x-ray spectroscopy, and x-ray photoelectron spectroscopy reveals localized oxygen and nitrogen enrichment together with a Re⁷⁺ oxidation state in the polycrystalline surface particles, consistent with the proposed formation of ammonium perrhenate. Epitaxial rhenium demonstrated greater resistance to aging and oxidation, making it a more promising candidate for superconducting qubits. Ongoing cleaning and XPS depth profiling will further determine the identity and origin of the surface crystallites.

Wiacek, Wiktoria [William Rainey Harper Coll.]↗
DOE OSTI2021

Radiation Effects in III-V Solar Cells Grown by Dynamic Hydride Vapor Phase Epitaxy

The recent development of hydride vapor phase epitaxy (HVPE) is potentially promising as a route to lower the cost of high-efficiency III-V solar cells for space applications. HVPE produces the same materials and device structures as the industry-standard organometallic vapor phase epitaxy (OMVPE) process, and although HVPE has shown promising device efficiencies, it lags the OMVPE growth technique in technical maturity. For example, there are no reports of the performance of HVPE-grown devices in radiation environments. There is an expectation that high-quality (that is, single crystal and low-defect) III-V materials will behave similarly regardless of the growth method. However, it is important to verify assumptions as facts. In this project, we produced materials and devices using both HVPE and OMVPE at NREL and irradiated them using 1 MeV electrons to ascertain the effect of radiation on the materials. We also performed initial work on producing more radiation-hard structures, including devices with the pn junction at the front of the device, and devices with a graded doping profile, both of which help with radiation tolerance. Measurements of the devices post radiation exposure showed that the open-circuit voltage (V OC ) of the HVPE-grown solar cells degraded least on a percent basis, although they also started from a lower baseline than the OMVPE-grown devices. All solar cells reached approximately the same V OC after irradiation, indicating that the dose used was sufficient to degrade all device equally. The short-circuit current in the HVPE devices did degrade more than the other solar cells, and this was attributed to a higher-than-expected doping density in the base layer of that cell. The results of these experiments, while by no means comprehensive, do not show any material difference in the radiation effects in OMVPE- and HVPE-grown materials and devices.

14 SOLAR ENERGY↗
DOE OSTI2021

Hot-pressed 6 LiInSe 2 for use as a ceramic radiation detector

Lithium based chalcogenides have many uses in the nuclear science field. 6 LiInSe 2 (or LISe) has been researched extensively because of its ability to operate in both scintillator and semiconductor modes. Here, this makes it useful in applications including nuclear material detection for national security, space applications, and medical imaging. In some applications growth and fabrication costs are of concern, as it takes upwards of 40 days to synthesize a charge, grow a crystal and fabricate a detector. Ceramics are a solution for this long route of preparation. This research shows that using a 6 LiInSe 2 ceramic instead of a single crystal significantly decreases the time required to make a detector. In the present work, ceramic wafers can be formed using a mechanical press equipped with a heating attachment. The resulting ceramic wafer performs very similar to a slow-growth single crystal when used in the scintillator mode.

36 MATERIALS SCIENCE↗
DOE OSTI2020

Shock compression response of an insensitive high explosive single crystal: 1,1-diamino-2,2-dinitroethene (FOX-7)

Insensitive high explosives (IHEs) – that do not compromise performance – are of immense interest as a safer alternative to conventional high explosives, such as pentaerythritol tetranitrate (PETN) and cyclotrimethylenetrinitramine (RDX). Despite the strong interest in using IHEs, shock compression experiments on IHE single crystals have not been reported. To address this need, plate impact experiments were conducted to measure wave profiles in 1,1-diamino-2,2-dinitroethene (FOX-7) single crystals – a representative IHE crystal – shocked to 21 GPa longitudinal stress. Particle velocity histories, measured using laser interferometry, show a clear two-wave structure (elastic-inelastic response) at modest stresses (<3.8 GPa). Wave profiles at higher stresses show a single (overdriven) wave. Measured shock velocities and wave profiles provide accurate Hugoniot data to 21 GPa. The measured wave profiles to 21 GPa show no sign of energy release due to chemical decomposition and constitute the first demonstration of an IHE single crystal insensitivity under plane shock compression. Numerical simulations using a phenomenological material model developed for FOX-7 showed good agreement with the measured wave profiles. The experimental results and continuum simulations presented here constitute a significant first step in gaining insight into the shock compression response of IHE single crystals.

71 CLASSICAL AND QUANTUM MECHANICS, GENERAL PHYSIC↗
DOE OSTI2023

Machine-learning-assisted automation of single-crystal neutron diffraction

Neutron scattering is a powerful but expensive technique to study materials and discover new matter. Advanced detector technology has significantly improved the efficiency of neutron experiments, increasing the complexity of neutron data reduction and analysis. Machine learning (ML) brings new directions for neutron diffraction data reduction and experiment operation. Here, this work presents an ML-assisted data reduction and analysis method for precise recognition of Bragg peaks and the corresponding regions of interest; it can then automatically screen and align a measured crystal using the recognized peaks, and subsequently plan and optimize the data collection with user-provided information and uncertainty quantification values of detected peaks. This method shows robust performance in different complex sample environments and enables automated single-crystal neutron diffraction.

47 OTHER INSTRUMENTATION↗
DOE OSTI2023

Investigation of the High-Pressure Behaviors of Amblygonite by Single-Crystal X-ray Diffraction, Raman Spectroscopy, and DFT Calculations

In the present study, we extensively explored the high-pressure behaviors and vibrational properties of amblygonite LiAlPO 4 F with elevated pressures up to 34.3 GPa based on single-crystal X-ray diffraction measurements, Raman spectroscopy, and DFT calculations. The compressibility and elastic properties of amblygonite were determined first. Specifically, the obtained isothermal bulk modulus of LiAlPO 4 F is 128(4) GPa and the triclinic phase exhibited anisotropic compression with axial compressibility β c > β a > β b with a ratio of 1.11:1.00:1.20. The Raman spectra showed no indication of phase transformation and were used to obtained mode Grüneisen parameters. The average Grüneisen parameter for PO 4 tetrahedral sites was smaller than for the LiO 4 F sites. Our results provide new insights into the phase stability and elastic properties of lithium-fluorite granites at extreme conditions.

36 MATERIALS SCIENCE↗