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Search indexed NASA NTRS and DOE OSTI research on propulsion, heat transfer, battery materials and energy systems. Follow report and document links to the original sources.

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At least 19 records
All sourcesNASA NTRSDOE OSTI
DOE OSTI2020

Large Single Crystals of V 1– x Mo x O 2 from a Two-Step Chemical Vapor Transport Synthesis

This article details the synthesis of single crystals with the chemical formulas V 1-x Mo x O 2 ( 0 ≤ x ≤ 0.6) using the chemical vapor transport method at high temperatures (850 to 950 °C). These compounds are of interest due to the special relationship between their structure and electronic properties. Understanding this relationship will help guide future efforts in designing energy-saving devices. While some of these compounds have been synthesized before, this is the first time their synthesis has been reported for such a wide range of compounds in the form of bulk single crystals. The single crystal form is required for detailed characterization of the compounds. The materials were characterized chemically and structurally in order to validate the precise chemical compositions that were reported. Characterization methods included x-ray diffraction, inductively-coupled plasma atomic emission spectroscopy, and electron dispersive spectroscopy. The synthesis method is tunable, and the introduction of multiple steps both overcome the previous chemical challenges precluding synthesis of high molybdenum content crystals and allow for the creation of larger single crystals that were otherwise possible. The crystals synthesized this way are suitable for specialized measurements for determining the precise physical properties and atomic structure.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗
DOE OSTI2017

Growth and structural characterization of large superconducting crystals of La 2 - x Ca 1 + x Cu 2 O 6

Large crystals of La 2 - x Ca 1 + x Cu 2 O 6 (La-Ca-2126) with x = 0:10 and 0.15 have been grown and converted to bulk superconductors by high-pressure oxygen annealing. The superconducting transition temperature, T c , is as high as 55 K; this can be raised to 60 K by post-annealing in air. Here we present structural and magnetic characterizations of these crystals using neutron scattering and muon spin rotation techniques. While the as-grown, non-superconducting crystals are single phase, we nd that the superconducting crystals contain 3 phases forming coherent domains stacked along the c axis: the dominant La-Ca-2126 phase, very thin (1.5 unit-cell) intergrowths of La 2 CuO 4 , and an antiferromagnetic La 8 Cu 8 O 20 phase. We propose that the formation and segregation of the latter phases increases the Ca concentration of the La-Ca-2126, thus providing the hole-doping that supports superconductivity.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗
DOE OSTI2016

Preparation of Gd(OH){sub 3} large single crystals by solid KOH assisted hydrothermal method and their luminescent and magnetic properties

Highlights: • Gd(OH){sub 3} large single crystals were prepared by solid KOH assisted hydrothermal method. • The possible growth mechanism of Gd(OH){sub 3} large single crystals was proposed. • The Gd(OH){sub 3} samples emitted a strong narrow-band ultraviolet B (NB-UVB) light. • The Gd(OH){sub 3} samples showed good paramagnetic properties. - Abstract: Large single crystals of gadolinium hydroxide [Gd(OH){sub 3}] in the length of several millimeters were successfully prepared by using solid KOH assisted hydrothermal method. Gd(OH){sub 3} samples were characterized by X-ray diffraction (XRD), 4-circle single-crystal diffraction, Fourier transform infrared (FTIR) spectroscopy and X-ray photoelectron spectroscopy (XPS). FESEM image shows hexagonal prism morphology for the Gd(OH){sub 3} large crystals. The possible growth mechanism of Gd(OH){sub 3} large single crystals was proposed. The photoluminescence and magnetic properties of Gd(OH){sub 3} species were investigated.

36 MATERIALS SCIENCE↗
DOE OSTI2024

Quantification of Dynamic Scattering Effects in Molecular Crystals using Large Angle Rocking Beam Electron Diffraction

Electron crystallography provides a pathway to solve structure of small crystals (< 1um) in size, and thus overcomes difficult synthesis constraints involved in growing large crystals. Generally, electron diffraction data is collected in the form of integrated intensity using continuous rotation or by precession. The measured intensities in 3D are utilized for structure solution. Using this approach, structure solution of difficult crystals, such as small crystals of zeolites, metal-organic frameworks, molecular crystals, and proteins , can be solved by electron diffraction. However, electron structure solutions are regularly reported with higher Rvalues than x-ray or neutron diffraction. While similar structures are found despite the high R-values, the differences in the measure intensity and theory calculated intensity limit information that can be extracted by electron diffraction. Previous work demonstrated that including multiple-scattering effects significantly reduce the R-values . Thus, it is critical to be able to quantify the dynamical diffraction effects in molecular crystals.

Crystallography↗
DOE OSTI2012

BaGa{sub 2}GeX{sub 6}(X=S, Se): New mid-IR nonlinear optical crystals with large band gaps

New middle infrared nonlinear optical crystals of BaGa{sub 2}GeX{sub 6}(X=S, Se) have been synthesized. The structures of both BaGa{sub 2}GeS{sub 6} and BaGa{sub 2}GeSe{sub 6} were found to be isomorphous exhibiting a three-dimensional framework constructed by the parallel alignment of Ga or Ge tetrahedron groups along the c-aix. The ultraviolet transmittance spectrum indicates the short-wavelength absorption edges of BaGa{sub 2}GeS{sub 6} and BaGa{sub 2}GeSe{sub 6} are 380 nm and 440 nm, respectively. The IR transmittance spectrum shows that the absorption edge of the BaGa{sub 2}GeS{sub 6} crystal is 13.7 {mu}m. Second-harmonic generation of the powder samples was measured with a 2.05 {mu}m laser using the Kurtz and Perry technique, which showed that BaGa{sub 2}GeS{sub 6} and BaGa{sub 2}GeSe{sub 6} are phase-matched materials, and their measured SHG coefficient is {approx}2.1 and {approx}3.5 times as large as the coefficient of AgGaS{sub 2}, or 26.3 pm/V and 43.7 pm/V. - Graphical abstract: The structure of BGGS viewed along the a and c axis and an as-grown crystal. Highlights: Black-Right-Pointing-Pointer Mid-IR NLO crystals of BaGa{sub 2}GeX{sub 6}(X=S, Se) with wide band-gap have been discovered. Black-Right-Pointing-Pointer The structures were constructed by the parallel alignment of Ga or Ge tetrahedra. Black-Right-Pointing-Pointer They are phase-matchable material with their SHG coefficient of 26.3 and 43.7 pm/V.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2012

Three-dimensional photonic crystals by large-area membrane stacking

We designed and analyzed a “mesh-stack” three-dimensional photonic crystal of a 12.4% bandgap with a dielectric constant ratio of 12:1. The mesh-stack consists of four offset identical square-lattice air-hole patterned membranes in each vertical period that is equal to the in-plane period of the square lattice. This design is fully compatible with the membrane-stacking fabrication method, which is based on alignment and stacking of large-area single-crystal membranes containing engineered defects. A bandgap greater than 10% is preserved as long as the membranes are subjected to in-plane misalignment less than 3% of the square period. By introducing a linear defect with a nonsymmorphic symmetry into the mesh-stack, we achieved a single-mode waveguide over a wide bandwidth.

36 MATERIALS SCIENCE↗
DOE OSTI2018

Chemical Vapor Synthesis of Titanium Aluminides by Reaction of Aluminum Subchloride and Titanium Tetrachloride

A new process for developing titanium aluminides (TiAls) using chemical vapor synthesis was investigated in a laboratory experiment. Aluminum subchloride (AlCl) was used as the reducing agent in the reaction with TiCl{sub 4} and the source of aluminum for Ti-Al alloy. Two types of products, with large crystals and fine particles, were fabricated. The large crystals were determined to be TiAl, with small amounts of Ti and Ti{sub 3}Al phases. The composition of fine particles, on the other hand, varied in wide range.

36 MATERIALS SCIENCE↗
DOE OSTI2016

Projection x-ray topography system at 1-BM x-ray optics test beamline at the advanced photon source

Projection X-ray topography of single crystals is a classic technique for the evaluation of intrinsic crystal quality of large crystals. In this technique a crystal sample and an area detector (e.g., X-ray film) collecting intensity of a chosen crystallographic reflection are translated simultaneously across an X-ray beam collimated in the diffraction scattering plane (e.g., [1, 2]). A bending magnet beamline of a third-generation synchrotron source delivering x-ray beam with a large horizontal divergence, and therefore, a large horizontal beam size at a crystal sample position offers an opportunity to obtain X-ray topographs of large crystalline samples (e.g., 6-inch wafers) in just a few exposures. Here we report projection X-ray topography system implemented recently at 1-BM beamline of the Advanced Photon Source. A selected X-ray topograph of a 6-inch wafer of 4H-SiC illustrates capabilities and limitations of the technique.

43 PARTICLE ACCELERATORS↗
DOE OSTI2023

Make Selenium Reactive Again: Activating Elemental Selenium for Synthesis of Metal Selenides Ranging from Nanocrystals to Large Single Crystals

The inertness of elemental selenium is a significant obstacle in the synthesis of selenium-containing materials at low reaction temperatures. Over the years, several recipes have been developed to overcome this hurdle; however, most of the methods are associated with the use of highly toxic, expensive, and environmentally harmful reagents. As such, there is an increasing demand for the design of cheap, stable, and nontoxic reactive selenium precursors usable in the low-temperature synthesis of transition metal selenides with vast applications in nanotechnology, thermoelectrics, and superconductors. Herein, a novel synthetic route has been developed for activating elemental selenium by using a solvothermal approach. By comprehensive 77 Se NMR, Raman, and infrared spectroscopies and gas chromatography–mass spectrometry, we show that the activated Se solution contained HSe – , [Se–Se] 2– , and Se 2– ions, as well as dialkyl selenide (R 2 Se) and dialkyl diselenide (R–Se–Se–R) species in dynamic equilibrium. This also corresponded to the first observation of naked Se 2 2– in solution. The versatility of the developed Se precursor was demonstrated by the successful synthesis of (i) the polycrystalline room-temperature modification of the β-Ag 2 Se thermoelectric material; (ii) large single crystals of superconducting β-FeSe; (iii) CdSe nanocrystals with different particle sizes (3–10 nm); (iv) nanosheets of PtSe 2 ; and (v) mono- and dibenzyl selenides and diselenides at room temperature. In conclusion, The simplicity and diversity of the developed Se activation method holds promise for applied and fundamental research.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2023

Unraveling the convoluted and dynamic interphasial mechanisms on Li metal anode

Accurate understanding of the chemistry of solid-electrolyte interphase (SEI) is key to developing new electrolytes for high-energy batteries using lithium metal (Li-0) anodes(1). SEI is generally believed to be formed by the reactions between Li-0 and electrolyte(2,3). However, our new study shows this is not the whole story. Through synchrotron-based X-ray diffraction and pair distribution function analysis, we reveal a much more convoluted formation mechanism of SEI, which receives considerable contributions from electrolyte, cathode, moisture and native surface species on Li-0, with highly dynamic nature during cycling. Using isotope labelling, we traced the origin of LiH to electrolyte solvent, moisture and a new source: the native surface species (LiOH) on pristine Li-0. When lithium accessibility is very limited as in the case of anode-free cells, LiOH develops into plate-shaped large crystals during cycling. Alternatively, when the lithium source is abundant, as in the case of Li||NMC811 cells, LiOH reacts with Li-0 to form LiH and Li2O. While the desired anion-derived LiF-rich SEI is typically found in the concentrated electrolytes or their derivatives, we found it can also be formed in low-concentration electrolyte via the crosstalk effect, emphasizing the importance of formation cycle protocol and opening up opportunities for low-cost electrolyte development.

Polzin, Bryant J.↗
DOE OSTI2022

Growth mechanisms of large, faceted crystals grown from solutions

Here, the paper describes optical techniques and methods used to study growth mechanisms and phenomena occurring on multiple faces of real bulk crystals grown from aqueous and organic solutions. Using examples of ionic KDP and molecular trans-stilbene crystals, it shows how in-situ and ex-situ surface observations can be applied to identify growth structures characteristic for the dislocation, two-dimensional (2D), and 3D cluster deposition mechanisms. Results are analyzed and applied to understanding of defects origins and methods for their elimination in practical growth of large, high optical quality crystals.

2D growth mechanism↗
DOE OSTI2025

Unveiling nano-scale crystal deformation using coherent X-ray dynamical diffraction

Visualization of internal deformation fields in crystalline materials helps bridge the gap between theoretical models and practical applications. Applying Bragg coherent diffraction imaging under X-ray dynamical diffraction conditions provides a promising approach to the longstanding challenge of investigating the deformation fields in micron-sized crystals. Here, we present an automatic differentiation-based reconstruction method that integrates dynamical scattering theory to accurately reconstruct deformation fields in large crystals. Using this forward model, our simulated and experimental results demonstrate that three-dimensional local strain information inside a large crystal can be accurately reconstructed under coherent X-ray dynamical diffraction conditions with Bragg coherent X-ray diffraction imaging. These findings open an avenue for extending the investigation of local deformation fields to microscale crystals while maintaining nanoscale resolution, leveraging the enhanced coherence and brightness of advanced X-ray sources.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗