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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 343 records · Page 19
All sourcesNASA NTRSDOE OSTI
DOE OSTI2017

The assembly of two isomorphous coordination compounds based on 1,4-cyclohexanedicarboxylic acid and 2,4-diamino-6-phenyl-1,3,5-triazine

The compounds [Co(e,a-cis-1,4-chdc)(phdat)]{sub n} (1) and [Cd(e,a-cis-1,4-chdc)(phdat)]{sub n} (2) have been synthesized under hydrothermal method by using 1,4-cyclohexanedicarboxylic acid (1,4-H{sub 2}chdc), 2,4-diamino-6-phenyl-1,3,5-triazine (phdat) as well as CoCl{sub 2}·6H{sub 2}O, CdCl{sub 2}·2.5H{sub 2}O respectively and characterized by IR spectra, X-ray single-crystal diffraction, powder X-ray single-crystal diffraction (PXRD), elemental analyses and thermogravimetric analyses (TGA). The results show the compounds 1 and 2 are isomorphous and exhibit paddle-wheel dinuclear Co{sub 2}(CO{sub 2}){sub 4}/Cd{sub 2}(CO{sub 2}){sub 4} units, which are further connected to 1D chain structures by μ{sub 4}:η{sup 1}:η{sup 1}:η{sup 1}:η{sup 1} 1,4-chdc{sup 2–} ligands and extended into a 3D structures via different hydrogen bonding and π…π stacking interactions. Furthermore, compound 1 exhibits antiferromagnetic behavior and compound 2 displays luminescent behavior at solid state. - Graphical abstract: Two isomorphous coordination compounds 1–2 have been synthesized and characterized by XRD, IR spectra and TGA etc. Compound 1 and 2 display antiferromagnetic behavior and luminescent behavior respectively. - Highlights: • Two novel polymers based on 1,4-cyclohexanedicarboxylic acid have been synthesized. • Compounds 1 and 2 feather 1D chain structure built up from paddle-wheel SBUs. • The magnetism of 2 is investigated. • The electrochemical property and luminescent property of 1 are investigated.

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

Structure of diopside, enstatite, and magnesium aluminosilicate glasses: A joint approach using neutron and x-ray diffraction and solid-state NMR

Neutron diffraction with magnesium isotope substitution, high energy x-ray diffraction, and 29 Si, 27 Al, and 25 Mg solid-state nuclear magnetic resonance (NMR) spectroscopy were used to measure the structure of glassy diopside (CaMgSi 2 O 6 ), enstatite (MgSiO 3 ), and four (MgO) x (Al 2 O 3 ) y (SiO 2 ) 1–x–y glasses, with x = 0.375 or 0.25 along the 50 mol. % silica tie-line (1 – x – y = 0.5) or with x = 0.3 or 0.2 along the 60 mol. % silica tie-line (1 – x – y = 0.6). The bound coherent neutron scattering length of the isotope 25 Mg was remeasured, and the value of 3.720(12) fm was obtained from a Rietveld refinement of the powder diffraction patterns measured for crystalline 25 MgO. The diffraction results for the glasses show a broad asymmetric distribution of Mg–O nearest-neighbors with a coordination number of 4.40(4) and 4.46(4) for the diopside and enstatite glasses, respectively. As magnesia is replaced by alumina along a tie-line with 50 or 60 mol. % silica, the Mg–O coordination number increases with the weighted bond distance as less Mg 2+ ions adopt a network-modifying role and more of these ions adopt a predominantly charge-compensating role. 25 Mg magic angle spinning (MAS) NMR results could not resolve the different coordination environments of Mg 2+ under the employed field strength (14.1 T) and spinning rate (20 kHz). The results emphasize the power of neutron diffraction with isotope substitution to provide unambiguous site-specific information on the coordination environment of magnesium in disordered materials.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2025

The structures of mcgovernite and carlfrancisite reconsidered: static disorder or ordered defects and twinning?

Here, the minerals mcgovernite and carlfrancisite possess an extraordinary rhombohedral unit cell [mcgovernite: a = b = 8.206 Å and c = 204.118 Å, with the complex formula unit M 2+ 19 Zn 3 (OH) 21 (AsO 3 )(AsO 4 ) 3 (SiO 4 ) 3 (M = Mn, Mg, Zn); carlfrancisite similar]. Hawthorne [(2018), Mineral. Mag. 82, 1101–1118] reported a single-crystal study using a centrosymmetric model ($R\bar{3}c$) containing disorder on three cationic sites and an AsIII lone-pair site for both mcgovernite and carlfrancisite. A solution of the structure of mcgovernite from high-resolution synchrotron powder diffraction data suggests a reinterpretation of the crystal structures of mcgovernite and carlfrancisite as noncentrosymmetric R3c with ordered planar defects which allows for merohedral twinning.

carlfrancisite↗
DOE OSTI2017

Designing pseudocubic perovskites with enhanced nanoscale polarization

A crystal-chemical framework has been proposed for the design of pseudocubic perovskites with nanoscale ferroelectric order, and its applicability has been demonstrated using a series of representative solid solutions that combined ferroelectric (K 0.5 Bi 0.5 TiO 3 , BaTiO 3 , and PbTiO 3 ) and antiferroelectric (Nd-substituted BiFeO 3 ) end members. The pseudocubic structures obtained in these systems exhibited distortions that were coherent on a scale ranging from sub-nanometer to tens of nanometers, but, in all cases, the macroscopic distortion remained unresolvable even if using high-resolution X-ray powder diffraction. Different coherence lengths for the local atomic displacements account for the distinctly different dielectric, ferroelectric, and electromechanical properties exhibited by the samples. The guidelines identified provide a rationale for chemically tuning the coherence length to obtain the desired functional response.

36 MATERIALS SCIENCE↗
DOE OSTI2019

Using powder XRD and pair distribution function to determine anisotropic atomic displacement parameters of orthorhombic tridymite and tetragonal cristobalite

Determination of the crystal structures of low-temperature tridymite and cristobalite using single-crystal XRD has been challenging because they generally occur as metastable fine-grained crystals in the geological environment. Therefore, using powder diffraction and scattering techniques is critical to study the low-temperature crystals. Synchrotron powder X-ray diffraction (XRD), pair distribution function (PDF) and transmission electron microscopy were used to investigate the structure of orthorhombic tridymite with C 222 1 symmetry and tetragonal cristobalite with P 4 1 2 1 2 symmetry, including their anisotropic atomic displacement parameters (ADPs). Rietveld refinement was used to determine the unit-cell parameters, fractional coordinates and isotropic atomic displacement parameters ( U iso ) of the tridymite and cristobalite. The PDF method was used to determine ADPs for each atom. The results suggest that the crystal structure with high quality ADP values can be obtained using the combined methods of XRD and PDF analyses. The method can be used for characterizing crystals that are not suitable for single-crystal XRD.

Lee, Seungyeol (ORCID:0000000201751389)↗
DOE OSTI2020

Dehydration synthesis and crystal structure of terbium oxychloride, TbOCl

Terbium oxychloride, TbOCl, was synthesized via a simple heat-treatment of TbCl3·6H2O. The structure was determined using X-ray powder diffraction (XRD) data. The TbOCl compound crystallizes within the tetragonal P4/nmm space group, and its crystal structure is composed of alternating layers of (TbO)n and n Cl- anions. The unit cell parameters, volume, and density were compared to the literature data of other isostructural rare-earth oxychlorides in the P4/nmm space group and showed a good agreement when fitted to the calculated trendlines.

oxychloride, rare-earth oxyhalide, powder diffract↗
DOE OSTI2020

In situ temperature profile measurements with high-energy X-rays as a probe of optical floating zone crystal growth environment

The ability of optical floating zone (OFZ) furnaces to rapidly produce large single crystals of complex emerging materials has had a transformative effect on many scientific fields that require samples of this type. However, the crystal growth process within the OFZ furnace is not well understood owing to the challenges involved in monitoring the high-temperature crystal growth process. Novel beamline-compatible optical furnaces that approximate the inhomogeneous growth environment within an OFZ furnace have been fabricated and tested in high-energy synchrotron beamlines. In this paper, it is demonstrated that temperature profiles can be effectively extracted from powder diffraction data collected on polycrystalline ceramic rods heated at their tip. Furthermore, these measured temperature profiles can be accurately reproduced using a heat-transfer model that accounts for solid-state thermal conduction, partial sample lamp power absorption, convective air cooling and radiative cooling, allowing key thermal parameters such as thermal conductivity to be extracted from experimental data.

36 MATERIALS SCIENCE↗
DOE OSTI2019

Improved calibration of area detectors using multiple placements

Calibration of area detectors from powder diffraction standards is widely used at synchrotron beamlines. From a single diffraction image, it is not possible to determine both the sample-to-detector distance and the wavelength, but, with images taken from multiple positions along the beam direction and where the relative displacement is known, the sample-to-detector distance and wavelength can both be determined with good precision. Finally, an example calibration using the GSAS-II software package is presented.

46 INSTRUMENTATION RELATED TO NUCLEAR SCIENCE AND ↗
DOE OSTI2022

Machine-learning enabled thermodynamic model for the design of new rare-earth compounds

We employ a descriptor based machine-learning approach to assess the effect of chemical alloying on formation-enthalpy of rare-earth intermetallics. Application of machine-learning approaches in rare-earth intermetallic design have been sparse due to limited availability of reliable datasets. In this work, we developed an ‘in-house’ rare-earth database with more than 600 + compounds, each entry was populated with formation enthalpy and related atomic features using high-throughput density-functional theory (DFT). The SISSO (sure independence screening and sparsifying operator) based machine-learning method with meaningful atomic features was used for training and testing the formation enthalpies of rare earth compounds. The complex lattice function coupled with the machine-learning model was used to explore the effect of transition metal alloying on the energy stability of Ce based cubic Laves phases (MgCu 2 type). The SISSO predictions show good agreement with high-fidelity DFT calculations and X-ray powder diffraction measurements. Our study provides quantitative guidance for compositional considerations within a machine-learning model and discovering new metastable materials. The electronic-structure of Ce-Fe-Cu based compound was also analyzed to get an in-depth understanding of the electronic origin of phase stability. The interpretable analytical models in combination with density-functional theory and experiments provide a fast and reliable design guide for discovering technologically useful materials.

36 MATERIALS SCIENCE↗
DOE OSTI2014

Magnetic structure of Sr 2 CuWO 6

Magnetic structure of the double perovskite Sr2CuWO6 was determined from neutron powder diffraction data. At 3 K the material is magnetically long-range ordered into a collinear antiferromagnetic structure described by a propagation vector k = (0, 1/2, 1/2) with the Cu-II moments of 0.57(1) mu(B) parallel to the a-axis. The result is in agreement with our previous prediction (Vasala et al 2014 Phys. Rev. B 89 134419) based on electronic structure calculations, showing that the three-dimensional magnetic long-range order is caused by relatively strong antiferromagnetic next-nearest-neighbor interactions.

double-perovskite oxide↗
DOE OSTI2015

Small-angle scattering of particle assemblies

Small-angle scattering formulae for crystalline assemblies of arbitrary particles are derived from powder diffraction theory using the decoupling approximation. To do so, the pseudo-lattice factor is defined, and methods to overcome the limitations of the decoupling approximation are investigated. Further, approximated equations are suggested for the diffuse scattering from various defects of the first kind due to non-ideal particles, including size polydispersity, orientational disorder and positional fluctuation about their ideal positions. Calculated curves using the formalism developed herein are compared with numerical simulations computed without any approximation. For a finite-sized assembly, the scattering from the whole domain of the assembly must also be included, and this is derived using the correlation function approach.

assembly↗
DOE OSTI2025

Spotlight: efficient automated global optimization in rietveld analysis of diffraction data

Performing reliable Rietveld analysis on tens or hundreds of powder diffraction datasets from parametric or time-resolved experiments often poses a bottleneck in extracting meaningful results from the data. While automated analysis of data has recently been demonstrated, high temperature annealing studies, during which phase transformations occur and lattice parameters may change due to repartitioning of elements, are prime examples where automation by a simple phase identification from a database of room temperature structures or automation by sequential refinements is likely to fail. To enable reliable, efficient, automated Rietveld analysis, we present a Python package named Spotlight , building on established Rietveld packages such as MAUD, GSAS , or GSAS-II , which extends the refinement of best fit parameters to a global optimization using an ensemble of optimizers leveraging hierarchical parallel execution on high-performance computing clusters. Spotlight further enables the efficient design of refinement plans through the iterative automated machine-learning of a surrogate for the refinement on which the global optimizations are performed until results from the surrogate converge to the response surface data. We demonstrate Spotlight with the analysis of uranium molybdenum and Ti–6Al–4V datasets, as well as in two open-source tutorials analyzing aluminium oxide and lead sulphate.

36 MATERIALS SCIENCE↗
DOE OSTI2026

Thermal neutron imaging detector with wavelength shifting fiber and digital readout

Here, we developed a large area, digital thermal neutron imaging detector. The detector uses a 6 LiF/ZnS(Ag) neutron-sensitive scintillator combined with wavelength shifting fiber technology. The signals from fiber channels are amplified, integrated, and digitized using individual analog-to-digital converters for each channel. The neutron position is determined from the digitized signal using a least-squares gaussian-fitting algorithm. The detector size was 77 × 38 cm 2 (2926 cm 2 ), it provided 1.3 mm resolution, and its resolution can further be improved. The detector was designed for a powder diffraction neutron scattering beamline and provided substantial improvement of d-space resolution compared with existing detectors. This detector may have broader applications due to its large area and high spatial resolution extended over its large area.

6LiF/ZnS(Ag) scintillator↗
DOE OSTI2014

Piezo-/dielectric properties of perovskite-structure high-temperature relaxor ferroelectrics: The Pb(Lu{sub 1/2}Nb{sub 1/2})O{sub 3}–Pb(Zn{sub 1/3}Nb{sub 2/3})O{sub 3}–PbTiO{sub 3} ternary ceramics

Graphical abstract: - Highlights: • Pb(Zn{sub 1/3}Nb{sub 2/3})O{sub 3}-based ternary ferroelectric ceramics were prepared by solid-state synthesis method. • Morphotropic phase boundary region has been determined by XRD, di-/piezoelectric properties. • The compositions near MPB region exhibit excellent piezoelectric properties. - Abstract: A new compositional system of relaxor ferroelectrics was investigated based on the high piezoelectricity Pb(Zn{sub 1/3}Nb{sub 2/3})O{sub 3}–PbTiO{sub 3} ferroelectric perovskite family. Compositions were fabricated near an estimated morphotropic phase boundary (MPB) of the Pb(Lu{sub 1/2}Nb{sub 1/2})O{sub 3}–Pb(Zn{sub 1/3}Nb{sub 2/3})O{sub 3}–PbTiO{sub 3} (PLZNT) ternary system by a two-step synthetic process. Their structures have been analyzed by means of X-ray diffraction technique. On the basis of X-ray powder diffraction, the morphotropic phase boundary (MPB) region for the ternary system was obtained. The Curie temperature T{sub C} of ternary system varied from 240 °C to 330 °C and the coercive fields E{sub c}s > 10 kV/cm. The values of piezoelectric coefficients d{sub 33} vary in the range of 260–450 pC/N with different PZN contents. It is worth noting that the optimum compositions were located at MPB region but near the tetragonal phase. The new PLZNT ceramics exhibit wider range of T{sub C}s and E{sub c}s, making it a promising material for high-powder ultrasound transducers using in a large temperature range.

36 MATERIALS SCIENCE↗
DOE OSTI2023

The T 2 structure of polycrystalline cubic human insulin

The polymorphism of human insulin upon pH variation was characterized via X-ray powder diffraction, employing a crystallization protocol previously established for co-crystallization with phenolic derivatives. Two distinct rhombohedral ( R 3) polymorphs and one cubic ( I 2 1 3) polymorph were identified with increasing pH, corresponding to the T 6 , T 3 R 3 f and T 2 conformations of insulin, respectively. The structure of the cubic T 2 polymorph was determined via multi-profile stereochemically restrained Rietveld refinement at 2.7 Å resolution. This constitutes the first cubic insulin structure to be determined from crystals grown in the presence of zinc ions, although no zinc binding was observed. The differences of the polycrystalline variant from other cubic insulin structures, as well as the nature of the pH-driven phase transitions, are discussed in detail.

59 BASIC BIOLOGICAL SCIENCES↗
DOE OSTI2022

Magnetic moments and spin structure in single-phase B20 Co 1+x Si 1-x (x = 0.043)

Neutron powder diffraction (NPD) and x-ray magnetic circular dichroism (XMCD) spectroscopy are employed to investigate the magnetism and spin structure in single-phase B20 Co 1.043 Si 0.957 . The magnetic contributions to the NPD data measured in zero fields are consistent with the helical order among the allowed spin structures derived from group theory. The magnitude of the magnetic moment is (0.3 ± 0.1) μ B /Co according to NPD, while the surface magnetization probed by XMCD at 3 kOe is (0.18–0.31) μ B /Co. Both values are substantially larger than the bulk magnetization of 0.11 μ B /Co determined from magnetometry at 70 kOe and 2 K. Finally, these experimental data indicate the formation of a helical spin phase and the associated conical states in high magnetic fields.

36 MATERIALS SCIENCE↗
DOE OSTI2020

Consequences of long-term water exposure for bulk crystal structure and surface composition/chemistry of nickel-rich layered oxide materials for Li-ion batteries

Water exposure of layered nickel-rich transition metal oxide electrodes, widely used in high-energy lithium-ion batteries, has detrimental effects on the electrochemical performance, which complicates electrode handling and prevents implementation of environmentally benign aqueous processing procedures. Elucidating the degradation mechanisms in play may help rationally mitigate/circumvent key challenges. Here, the bulk structural consequences of long-term (>2.5 years) deuterated water (D2O) exposure of intercalation materials with compositions Li x Ni 0.5 Co 0.2 Mn 0.3 O 2 (NCM523) and Li x Ni 0.8 Co 0.1 Mn 0.1 O 2 (NCM811) are studied by neutron powder diffraction (NPD). Detailed inspection of the NPD data reveals gradual formation of a secondary crystalline phase in all exposed samples, not previously reported for this system. This unknown phase forms faster in liquid- compared to vapor-exposed compounds. Structural modelling of the NPD data shows a stable level of Li/Ni anti-site defects and does not indicate any significant changes in lattice parameters or hydrogen-lithium (D + /Li + ) exchange in the structure. Consequently, the secondary phase formation must take place via transformation rather than modification of the parent material. X-ray photoelectron spectroscopy data indicate formation of LiHCO 3 /Li 2 CO 3 at the surface and a Li-deficient oxide in the sub-surface region of the pristine compounds, and the presence of adsorbed water and transition metal hydroxides at the exposed sample surfaces.

25 ENERGY STORAGE↗