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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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All sourcesNASA NTRSDOE OSTI
DOE OSTI2024

Disorder and diffuse scattering in single-chirality (TaSe 4 ) 2 ⁢I crystals

The quasi-one-dimensional chiral compound (TaSe 4 ) 2 I has been extensively studied as a prime example of a topological Weyl semimetal. Upon crossing its phase transition temperature $T$ CDW ≈263K, (TaSe 4 ) 2 I exhibits incommensurate charge density wave (CDW) modulations described by the well-defined propagation vector ∼(0.05,0.05,0.11), oblique to the TaSe 4 chains. Although optical and transport properties greatly depend on chirality, there is no systematic report about chiral domain size for (TaSe 4 ) 2 I. In this study, our single-crystal scattering refinements reveal a bulk iodine deficiency, and Flack parameter measurements on multiple crystals demonstrate that separate (TaSe 4 ) 2 I crystals have uniform handedness, supported by direct imaging and helicity-dependent terahertz emission spectroscopy. Our single-crystal x-ray scattering and calculated diffraction patterns identify multiple diffuse features and create a real-space picture of the temperature-dependent (TaSe 4 ) 2 I crystal structure. Further, the short-range diffuse features are present at room temperature and decrease in intensity as the CDW modulation develops. These transverse displacements, along with electron pinning from the iodine deficiency, help explain why (TaSe 4 ) 2 I behaves as an electronic semiconductor at temperatures above and below $T$ CDW , despite a metallic band structure calculated from density functional theory of the ideal structure.

36 MATERIALS SCIENCE↗
DOE OSTI2019

Fixed-Angle Reflectance from Uranium Compounds and U-Bearing Minerals: Experimental Challenges to Determine the Optical Constants n and k

Fixed-angle reflectance spectroscopy using a commercial Fourier transform infrared (FTIR) spectrometer was employed to derive the optical constants n and k of several uranium compounds. This technique relies upon measurement of the quantitative reflectance R(?) spectra from a polished surface across a broad spectral range (in this case, the mid- and far-IR covering ca. 7500 to 50 cm-1) followed by application of the Kramers-Kronig transformation (KKT). Near-normal fixed-angle measurements as used in this technique require continuous reflectance spectra to as low a wavenumber value as possible. Here, we discuss some of the many challenges in measuring the far-IR and very far-IR (terahertz) spectra using an interferometric instrument, particularly those stemming from small sample sizes, typically just millimeters on a face for crystalline samples, as well as limitations due to optical components and diffraction. We apply this method to single-crystal UO2 and its mineralogical form uraninite, as well as other U-bearing minerals such as autunite [Ca(UO2)2(PO4)2·8-12H2O] and the dehydrated form of autunite, meta-autunite. In addition to the specular reflectance spectra, x-ray diffractometry was used as a confirmatory technique to analyze the surface composition of the species. Deriving the infrared optical constants for such U-bearing species (as well as other solids) will enable nondestructive detection under a variety of environmental and compositional conditions.

Uranium Minerals, infrared spectroscopy, optical c↗
DOE OSTI2015

Structure of compound Pr{sub 5}Mo{sub 3}O{sub 16+δ} exhibiting mixed electronic—ionic conductivity

The structure of Pr{sub 5}Mo{sub 3}O{sub 16+δ} single crystals is studied by X-ray diffraction, EDXS microanalysis, transmission microscopy, and XANES spectroscopy. It is found that in the structure Pr and Mo cations mutually replace each other, atomic positions of oxygen are split into several additional positions, and structural voids accommodate interstitial oxygen atoms (which make the main contribution to the conductivity). The disorder of the oxygen sublattice is responsible for the continuity of the framework of the ways of migration of oxygen ions.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗
DOE OSTI2015

Quantification of water in majoritic garnet

Majoritic garnet, characterized by an excess of silicon (>3 Si per formula unit), is considered one of the major phases of the Earth’s transition zone from 410-660 km depth. Quantifying the H 2 O content of nominally anhydrous mantle minerals is necessary to evaluate their water storage capacity from experiments and modeling the Earth’s deep water cycle. We present mineral-specific infrared absorption coefficients for the purpose of quantifying the amount of water incorporated into majorite as hydroxyl point defects. A suite of majoritic garnet samples with varying proportions of Si, Fe, Al, Cr and H 2 O was synthesized at conditions of 18-19 GPa and 1500-1800°C. Single-crystals were characterized using X-ray diffraction, electron microprobe analysis, secondary Ion Mass spectrometry (SIMS), IR, Raman and Mössbauer spectroscopy. We utilize SIMS and Raman spectroscopy in combination with IR spectroscopy to provide IR absorption coefficients for water in majoritic garnets with the general mineral formula (Mg,Fe) 3 (Si,Mg,Fe,Al,Cr) 2 [SiO4] 3 . Furthermore, the IR absorption coefficient for majoritic garnet in the OH stretching region is frequency-dependent and ranges from 10 470 ± 3100 Lmol-1cm-2 to 23 400 ± 2300 Lmol -1 cm -2 .

36 MATERIALS SCIENCE↗
DOE OSTI2014

Experimental Report: ORNL Proposal ID IPTS 8937

Neutron scattering experiment was performed using fine-resolution Fermi chopper spectrometer “SEQUOIA” installed at the Spallation Neutron Source, ORNL. Although this spectrometer is designed to measure inelastic neutron scattering spectra, during experiments a signal of elastic scattering is also recorded. The coherent nuclear component of this elastic scattering provides Bragg diffraction pattern of a sample, i.e., CeNi single crystal in our case. Therefore, it is possible to follow the CeNi structural variations as a function of pressure and to register structural phase transition. Measurements were performed at the temperature of 15 K under pressure of zero (ambient pressure at 15 K), 400, 800, and 2200 bars.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗
DOE OSTI2020

Crystallization of ApoA1 and ApoE4 Nanolipoprotein Particles and Initial XFEL-Based Structural Studies

Nanolipoprotein particles (NLPs), also called “nanodiscs”, are discoidal particles with a patch of lipid bilayer corralled by apolipoproteins. NLPs have long been of interest due to both their utility as membrane-model systems into which membrane proteins can be inserted and solubilized and their physiological role in lipid and cholesterol transport via high-density lipoprotein (HDL) and low-density lipoprotein (LDL) maturation, which are important for human health. Serial femtosecond crystallography (SFX) at X-ray free electron lasers (XFELs) is a powerful approach for structural biology of membrane proteins, which are traditionally difficult to crystallize as large single crystals capable of producing high-quality diffraction suitable for structure determination. To facilitate understanding of the specific role of two apolipoprotein/lipid complexes, ApoA1 and ApoE4, in lipid binding and HDL/LDL particle maturation dynamics, and to develop new SFX methods involving NLP membrane protein encapsulation, we have prepared and crystallized homogeneous populations of ApoA1 and ApoE4 NLPs. Crystallization of empty NLPs yields semi-ordered objects that appear crystalline and give highly anisotropic and diffuse X-ray diffraction, similar to fiber diffraction. Several unit cell parameters were approximately determined for both NLPs from these measurements. Thus, low-background, sample conservative methods of delivery are critical. Here we implemented a fixed target sample delivery scheme utilizing the Roadrunner fast-scanning system and ultra-thin polymer/graphene support films, providing a low-volume, low-background approach to membrane protein SFX. This study represents initial steps in obtaining structural information for ApoA1 and ApoE4 NLPs and developing this system as a supporting scaffold for future structural studies of membrane proteins crystalized in a native lipid environment.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
NASA NTRS1987

Laser induced OMCVD growth of AlGaAs on GaAs

A major factor limiting the efficiency of the GaAs-GaAlAs solar cell is the rate of recombination at the GaAs-AlGaAs interface. Evidence has been previously reported which indicates that recombination at this interface can be greatly reduced if the AlGaAs layer is grown at lower than normal temperatures. The authors examine the epitaxial growth of AlGaAs on GaAs using a horizontal OMCVD reactor and an excimer laser operating in the UV (lambda = 193 nm) region. The growth temperatures were 450 and 500 C. The laser beam was utilized in two orientations: 75 deg angle of incidence and parallel to the substrate. Film composition and structure were determined by Auger electron spectroscopy (AES) and transmission electron microscopy (TEM). Auger analysis of epilayers grown at 500 C with the laser impinging show no carbon or oxygen contamination of the epitaxial layers or interfaces. TEM diffraction patterns of these same epilayers exhibit single crystal (100) zone axis patterns.

Wilt, David M.↗
DOE OSTI2026

Oxide-nitride heteroepitaxy for low-loss dielectrics in superconducting quantum circuits

Superconducting qubits show great promise for the realization of fault-tolerant quantum computing, but lossy, amorphous dielectrics limit current technology. Identifying highly crystalline and stoichiometric dielectrics with intrinsically low microwave loss is therefore a central materials challenge, yet experimentally validated platforms remain scarce. In this work, we integrate a crystalline dielectric into a heteroepitaxial TiN/$γ$-Al$_2$O$_3$/TiN trilayer grown via pulsed laser deposition. Correlative high-resolution imaging, diffraction, and spectroscopy measurements confirm the single-crystal quality and chemical integrity of all layers, with minimal defects and limited anion interdiffusion across the oxide-nitride interfaces. Using microwave lumped-element resonators with parallel-plate capacitors, we report the first direct measurement of the dielectric loss of epitaxial $γ$-Al$_2$O$_3$, for which we find a low intrinsic two-level system loss, $δ_{\text{TLS}}^0 = (2.8 \pm 0.1) \times 10^{-5}$. These results establish heteroepitaxial oxides on transition metal nitrides as an attractive materials platform for superconducting quantum circuits, particularly for integration into compact device architectures such as merged-element transmons and microwave kinetic inductance detectors.

Garcia-Wetten, David A. [Northwestern U.]↗
NASA NTRS1972

Evidence of crystal structure in some sputtered MoS2 films.

Electron diffraction patterns and electron micrographs of molybdenum disulfide films sputtered on single-NaCl-crystal and electropolished-aluminum substrates are presented as evidence that crystalline MoS2 films can be sputtered onto various substrates in thicknesses up to 2 microns. Applied to Falex test pins and V-blocks, some of these films exhibited a wear life as long as 65 minutes at 1000 lb jaw load.

Lavik, M. T.↗
DOE OSTI2018

Spectrometer of Synchrotron Radiation Based on Diffraction Focusing a Divergent Beam Formed by a Compound Refractive Lens

The results of the first experimental realization of a spectrometer based on the effect of diffraction focusing of X rays by a flat single crystal are discussed. A secondary X-ray source with a relatively high angular divergence and small sizes was formed at the focus of a compound refractive lens having 50 beryllium biconcave elements with a curvature radius of 50 μm. The silicon spectrometer crystal was cut in the form of a wedge of variable thickness, oriented perpendicular to the diffraction plane. The reflection 111 was used for energies of 8.3 and 12 keV. To simulate the experiment, a computer program was developed, which takes into account accurately and for the first time the focusing of radiation by the lens and its subsequent diffraction in the crystal. A calculated curve for a monochromatic beam has made it possible to determine the monochromator spectrum with high resolution from experimental data for a polychromatic beam. It is shown that monochromator resolution increases with an increase in the distance from the compound refractive lens to the crystal.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗
DOE OSTI2018

Effect of oxygen vacancies and Ag deposition on the magnetic properties of Ag/N co-doped TiO2 single-crystal films

Highlights: • Photochemical deposition method to prepare Ag-doped TiO{sub 2} samples. • TiO{sub 2} single crystal films are used for studying room temperature ferromagnetism origin. • Ag element is deposited on TiO{sub 2} single crystal films surface in the form of Ag particles. • Oxygen vacancies and Ag particles synergy influence the ferromagnetism in samples. - Abstract: We employ TiO{sub 2} single-crystal films as a substrate and use a photochemical deposition method to prepare Ag-doped and Ag/N co-doped TiO{sub 2} single-crystal films. We also investigate the optical and magnetic properties of the samples using various measurements. No diffraction peaks related to silver oxide appear in the X-ray diffraction (XRD) spectra, which implies the existence of Ag atoms in Ag-doped TiO{sub 2} single-crystal films. X-ray photoelectron spectroscopy (XPS) spectra indicate the existence of Ti{sup 4+} and Ag° in Ag/N co-doped TiO{sub 2} single-crystal films. It is found that Ag is deposited on a TiO{sub 2} single-crystal film surface in the form of Ag particles. Meanwhile, Ag particles can slightly enhance ferromagnetism in Ag-doped TiO{sub 2} single-crystal films compared with the TiO{sub 2} single-crystal film sample. Oxygen vacancies and Ag particle synergy influence ferromagnetism in Ag/N co-doped TiO{sub 2} single-crystal films.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗
DOE OSTI2015

Synthesis and characterization of BiFeO{sub 3} for photocatalytic degradation of azo dye

A novel approach is reported to synthesize single phase BiFeO{sub 3} via. sol-gel auto combustion method using glycine as fuel. Synthesized powder was subjected to annealing at different temperatures, i.e. 400 °C, 450 °C, 500 °C, 550 °C, and 600°C. Crystal structure of BiFeO{sub 3} samples examined by X-ray diffraction indicates that the samples were single-phased with different particle sizes, as particle sizes are temperature dependent and crystallized in rhombohedral structure. As the temperature was increased, the diffraction peak intensity of BiFeO3 in the XRD spectra gradually enhanced and the diffraction peaks became sharper. The optical properties of the resultant BiFeO{sub 3} were characterized using UV-Vis spectrophotometer over the range of 350-800 nm. UV-vis spectra of all the samples indicate that optical band gap lies in the visible region in the range of 2.2-2.07 eV at all temperatures. Moreover, photocatalytic properties of the BiFeO{sub 3} powders were investigated by the photodegradation of Reactive Black-5 (RB-5)

36 MATERIALS SCIENCE↗
DOE OSTI2023

Synthesizing pseudo-Kossel lines from neutron transmission data. I. An analytical approach for recovering single-crystal orientation

The energy-dispersive neutron spectra transmitted through single crystals are characterized by sharp Bragg dips at specific wavelengths, where Bragg's law is being fulfilled for certain crystallographic planes. This phenomenon allows for developing methods for crystal-orientation determination techniques similar to electron backscatter diffraction and X-ray diffraction microscopy. This work presents a new procedure to recover the orientation matrix for single crystals using transmission spectra recorded during rotation of a crystal about an axis perpendicular to a polychromatic neutron beam. The proposed method consists of an initial transformation of the as-collected wavelength–rotation maps to a wavevector $\textit{K}$ space, resulting in linear pseudo-Kossel lines that are suitable for analysis and indexing using image-processing procedures. Further, simulated neutron transmission spectra through a copper crystal with known orientations were used to set and prove the numerical approach. This technique may be expanded for cases where the neutron beam intersects multiple single-crystal grains with different orientations.

36 MATERIALS SCIENCE↗
NASA NTRS1978

Catalysts for electrochemical generation of oxygen

Single crystal surfaces of platinum and gold and transition metal oxides of the spinel type were studied to find more effective catalysts for the electrolytic evolution of oxygen and to understand the mechanism and kinetics for the electrocatalysis in relation to the surface electronic and lattice properties of the catalyst. The single crystal studies involve the use of low energy electron diffraction (LEED) and Auger electron spectroscopy as complementary tools to the electrochemical measurements. Modifications to the transfer system and to the thin-layer electrochemical cell used to facilitate the transfer between the ultrahigh vacuum environment of the electron surface physics equipment and the electrochemical environment with a minimal possibility of changes in the surface structure, are described. The electrosorption underpotential deposition of Pb onto the Au(111), (100) and (110) single crystal surfaces with the thin-layer cell-LEED-Auger system is discussed as well as the synthesis of spinels for oxygen evolution studies.

Hagans, P.↗
DOE OSTI2026

Mechanism of the wurtzite to rocksalt phase transformation in cadmium sulfide single crystals shock compressed along the 𝑐-axis to elastic impact stresses of ∼ 5 GPa

Cadmium sulfide (CdS), which exhibits a wurzite (WZ) to rocksalt (RS) phase transformation at elevated stresses, is an ideal system to address the role of deformation on phase transformation mechanisms and kinetics. CdS has been shown to have very different elastic-inelastic behavior for shock propagation along the WZ 𝑐- and 𝑎-axes, and also exhibits significant differences in the time scale for the phase transformation when shocked along these different axes. As an important first step in examining the role of deformation in shock-induced phase transformations, here we present in situ, time-resolved x-ray diffraction (XRD) measurements in single-event, shock wave experiments on CdS single crystals shocked along the WZ 𝑐-axis to elastic impact stresses near or above ∼ 5 GPa, where a marked increase in the kinetics of this transformation has been reported. The XRD measurements are compared with forward diffraction simulations to evaluate different proposed phase transformation mechanisms and are shown to be consistent with a shearing mechanism that results in the RS [001] direction being aligned with the original WZ 𝑐-axis and the RS [110] direction being aligned with the original WZ 𝑎-axis. In order to reproduce all observed RS diffraction spots the forward diffraction simulations required three different RS crystalline domains, each with a [110] direction aligned with one of the three original WZ 𝑎-axes, and a significant mosaicity, particularly about the RS [001] direction (the direction of shock propagation). In conclusion, this large mosaicity is likely due to variations in the possible shearing mechanisms that connect the WZ and RS structures, which can create crystallites with up to ∼ ±10° of relative rotations about the RS [001] direction, as well as further rotation of these crystallites as they grow, merge, and coalesce.

Crystal structure↗
DOE OSTI2019

Helical antiferromagnetic ordering in EuNi 1.95 As 2 single crystals

The Eu + 2 spins-7/2 in EuNi 2 As 2 with the body-centered tetragonal ThCr 2 Si 2 structure order antiferromagnetically below the Néel temperature T N = 15 K into a helical antiferromagnetic (AFM) structure with the helix axis aligned along the tetragonal c axis and the Eu ordered moments aligned ferromagnetically within the ab plane as previously reported from neutron diffraction measurements [T. Jin et al., Phys. Rev. B 99, 014425 (2019)]. Here we study the crystallographic, magnetic, thermal, and electronic transport properties of Bi-flux-grown single crystals using single-crystal x-ray diffraction, anisotropic magnetic susceptibility χ, isothermal magnetization M, heat capacity Cp, and electrical resistivity ρ measurements versus applied magnetic field H and temperature T. Vacancies are found on the Ni sites corresponding to the composition EuNi 1.95 (1) As 2. A good fit of the ρ (T) data by the Bloch-Grüneisen theory for metals was obtained. The χab (T) data below T N are fitted well by molecular field theory (MFT), and the helix turn angle kd and the Eu-Eu Heisenberg exchange constants are extracted from the fit parameters. The kd value is in good agreement with the neutron-diffraction result. The magnetic contribution to the zero-field heat capacity below T N is also fitted by MFT. The isothermal in-plane magnetization M ab exhibits two metamagnetic transitions versus H, whereas M c (T = 2 K ) is nearly linear up to H = 14 T, both behaviors being consistent with MFT. The M c (H, T) , ρ(H c , T) , and Cp (H c , T) data yielded a H c - T phase diagram separating the AFM and paramagnetic phases in good agreement with MFT. Anisotropic χ(T) literature data for the ThCr 2 Si 2 -type helical antiferromagnet EuRh 2 As 2 were also fitted well by MFT. A comparison is made between the crystallographic and magnetic properties of ThCr 2 Si 2 -type Eu M 2 Pn 2 compounds with M = Fe , Co, Ni, Cu, or Rh, and Pn = P or As, where only ferromagnetic and c -axis helical AFM structures are found.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗
DOE OSTI2019

Methods for operando coherent X-ray diffraction of battery materials at the Advanced Photon Source

Bragg coherent X-ray diffraction imaging has become valuable for visualization of the structural, morphological and strain evolution of crystals in operando electrode materials. As the electrode material particles (either in a single-crystal form or an aggregation form of single crystals) are evenly dispersed and randomly oriented in the electrode laminate, the submicrometer-sized coherent X-ray beam can be used to probe the local properties of electrode material crystals using two approaches. Coherent multi-crystal diffraction provides collective structural information of phase transitions in tens of crystals simultaneously as well as the individual behavior from single crystals, which are oriented at the Bragg condition in the X-ray illumination volume. Bragg coherent diffractive imaging enables one to monitor the evolution of the morphology and strain in individual crystals. This work explores and highlights the Bragg coherent X-ray diffraction measurements of battery electrode materials in operando conditions at the 34-ID-C beamline at the Advanced Photon Source. The experiment is demonstrated with NaNi 1/3 Fe 1/3 Mn 1/3 O 2 , a sodium-ion cathode material loaded in a half cell. Furthermore, the paper will discuss, in detail, the beamline setup, sample mounting and handling, alignment strategies and the data acquisition protocols.

73 NUCLEAR PHYSICS AND RADIATION PHYSICS↗
DOE OSTI2016

Direct and real time probe of photoinduced structure transition in colossal magnetoresistive material

Here, we report a direct and real time measurement of photoinduced structure phase transition in single crystal La 0.84 Sr 0.16 MnO 3 using femtosecond electron diffraction. The melting of orthorhombic lattice ordering under femtosecond optical excitation is found involving two distinct processes with different time scales, an initial fast melting of orthorhombic phase in about 4 ps and a subsequent slower transformation in 90 ps and longer timescales. Furthermore, the fast process is designated as the initial melting of orthorhombic phase induced by the Mn-O bond change that is most likely driven by the quenching of the dynamic Jahn-Teller distortion following the photo-excitation. We attribute the slow process to the growing of newly formed structure domain from the photo-excited sites to the neighboring non-excited orthorhombic sites.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗