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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 1,567 records · Page 87
All sourcesNASA NTRSDOE OSTI
DOE OSTI2015

Synthesis and characterization of electron doped La{sub 0.85}Te{sub 0.15}MnO{sub 3} thin film grown on LaAlO{sub 3} substrate by pulsed laser deposition technique

We report the structural, morphological and magneto-transport properties of electron doped La{sub 0.85}Te{sub 0.15}MnO{sub 3} (LTMO) thin film grown on (001) LaAlO{sub 3} single crystal substrate by pulsed laser deposition (PLD). X-ray diffraction (XRD) results confirm that the film has good crystalline quality, single phase, and c-axis orientation. The atomic force microscopy (AFM) results have revealed that the film consists of grains with the average size in a range of 20–30 nm and root-mean square (rms) roughness of 0.27nm. The resistivity versus temperature measurement exhibits an insulator to metal transition (MIT). We have noticed a huge value of magnetoresistance (∼93%) close to MIT in presence of 8T field. X-ray photoemission spectroscopy confirms the electron doping and suggests that Te ions could be in the Te{sup 4+} state, while the Mn ions stay in the Mn{sup 2+} and Mn{sup 3+} valence state.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗
DOE OSTI2015

Accounting for partiality in serial crystallography using ray-tracing principles

Serial crystallography generates partial reflections from still diffraction images. Partialities are estimated with EVAL ray-tracing simulations, thereby improving merged reflection data to a similar quality as conventional rotation data. Serial crystallography generates ‘still’ diffraction data sets that are composed of single diffraction images obtained from a large number of crystals arbitrarily oriented in the X-ray beam. Estimation of the reflection partialities, which accounts for the expected observed fractions of diffraction intensities, has so far been problematic. In this paper, a method is derived for modelling the partialities by making use of the ray-tracing diffraction-integration method EVAL. The method estimates partialities based on crystal mosaicity, beam divergence, wavelength dispersion, crystal size and the interference function, accounting for crystallite size. It is shown that modelling of each reflection by a distribution of interference-function weighted rays yields a ‘still’ Lorentz factor. Still data are compared with a conventional rotation data set collected from a single lysozyme crystal. Overall, the presented still integration method improves the data quality markedly. The R factor of the still data compared with the rotation data decreases from 26% using a Monte Carlo approach to 12% after applying the Lorentz correction, to 5.3% when estimating partialities by EVAL and finally to 4.7% after post-refinement. The merging R{sub int} factor of the still data improves from 105 to 56% but remains high. This suggests that the accuracy of the model parameters could be further improved. However, with a multiplicity of around 40 and an R{sub int} of ∼50% the merged still data approximate the quality of the rotation data. The presented integration method suitably accounts for the partiality of the observed intensities in still diffraction data, which is a critical step to improve data quality in serial crystallography.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗
DOE OSTI2015

Microstructural studies of AgNbO{sub 3} ceramic by using complex impedance spectroscopy

Lead-free piezoelectric silver niobate ceramic was synthesized by conventional solid state route. Room temperature X-ray diffraction pattern revealed that the sample crystallizes in single phase orthorhombic perovskite structure. Scanning electron micrographs of AgNbO{sub 3} ceramic showed that the average grain size is in the range 2–3 µm. The electrical properties were investigated by using impedance spectroscopy. Appearance of single semicircular arc in the Nyquist plot indicated the presence of grain contribution in the sample. Single RC parallel circuit model was employed to extract bulk capacitance (C{sub b}), resistance (R{sub b}) and electrical conductivity (σ{sub b}). The activation energy calculated from impedance and modulus data indicate that same types of charge carriers (oxygen vacancy movements) are responsible for conduction and relaxation.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗
DOE OSTI2016

Two-dimensional single crystal diamond refractive x-ray lens

The next generation light sources such as diffraction-limited storage rings and high repetition rate x-ray free-electron lasers will generate x-ray beams with significantly increased brilliance. These future machines will require X-ray optical components that are capable of handling higher instantaneous and average power densities while tailoring the properties of the x-ray beams for a variety of scientific experiments. Single crystal diamond is one of the best bulk materials for this application, because it is radiation hard, has a suitable uniform index of refraction and the best available thermal properties. In this paper we report on fabrication and experimental testing of a two-dimensional (2D) single crystal diamond compound refractive X-ray lenses (CRL). These lenses were manufactured using femto-second laser cutting and tested at the Advanced Photon Source of Argonne National Laboratory.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗
DOE OSTI2024

Coupled Gel/Seeded Growth of Cs2AgBiBr6 Single Crystals for Radiation Detection

Abstract— The all-inorganic lead free Cs2AgBiBr6 perovskite represents a highly promising environment-friendly radiation detector material. The first attempt to grow Cs2AgBiBr6 single crystals using the unique gel growth method is reported in this study. This technique enables controlled reagent diffusion in a gel medium at room temperature, fostering the growth of visible single crystals. It offers advantages over conventional methods, leading to fewer equilibrium and non-equilibrium defects and simplified execution. Interestingly, the as-grown crystals exhibited variations in size and colors within the gel matrix, indicating the influence of Bi solutes in Bi-poor and Bi-rich Cs2AgBiBr6 crystals. Once the crystals were confirmed by powder xray diffraction, a series of comprehensive material characterizations was performed. The resistivity of Cs2AgBiBr6 single crystals was measured at 1.12x107 Ω•cm. Trap density analysis yielded a value of 2.82 x1010 cm-3. The charge carrier mobility was determined to be 32.9 cm2V-1S-1, suggesting the suitability for radiation detector applications. Additional growth optimization is going on and further characterization will be reported during the presentation. Our work helps accelerate the development of lead-free perovskite materials toward radiation detector applications.

James, Ralph B.↗
DOE OSTI2019

Comparative Study of Magnetocaloric Effect in La{sub 0.67}Ca{sub 0.20}Sr{sub 0.13}MnO{sub 3} Manganite Prepared by Sol-Gel Method and Spark Plasma Sintering

The La{sub 0.67}Ca{sub 0.20}Sr{sub 0.13}MnO{sub 3} nanoparticles and bulks were prepared by using sol-gel method (SGM) and spark plasma sintering (SPS), respectively. The X-ray diffraction analysis indicates each sample crystal in a single rhombohedral perovskite structure (space group R 3-bar c). The Curie temperature is slightly improved and the phase transition is sharpened after processing with SPS. The enhancement of magnetocaloric effect (MCE) is also observed in the samples prepared by SPS. For a field change of 3 T, the maximum isothermal entropy change is improved by 32 and 117% when different sintering temperatures and sintering pressures are applied. The magnetic phase transition and MCE can be well described by the Landau theory. The present studies suggest that the perovskite bulks prepared by SPS could be useful for the application of magnetic refrigeration.

77 NANOSCIENCE AND NANOTECHNOLOGY↗
DOE OSTI2016

Crystal structure of the kinase domain of human protein tyrosine kinase 6 (PTK6) at 2.33 Å resolution

Human Protein tyrosine kinase 6 (PTK6) (EC:2.7.10.2), also known as the breast tumor kinase (BRK), is an intracellular non-receptor Src-related tyrosine kinase expressed in a majority of human breast tumors and breast cancer cell lines, but its expression is low or completely absent in normal mammary glands. In the recent past, several studies have suggested that PTK6 is a potential therapeutic target in cancer. To understand its structural and functional properties, the PTK6 kinase domain (PTK6-KD) gene was cloned, overexpressed in a baculo-insect cell system, purified and crystallized at room temperature. X-ray diffraction data to 2.33 Å resolution was collected on a single PTK6-KD crystal, which belonged to the triclinic space group P1. The Matthews coefficient calculation suggested the presence of four protein molecules per asymmetric unit, with a solvent content of ∼50%.The structure has been solved by molecular replacement and crystal structure data submitted to the protein data bank under the accession number 5D7V. This is the first report of apo PTK6-KD structure crystallized in DFG-in and αC-helix-out conformation. - Highlights: • We report the first crystal structure of the kinase domain of human PTK6. • >95% pure recombinant protein was purified in two-steps protocol: affinity chromatography followed by gel filtration. • Kinase activity of the crystal construct is comparable to the full length enzyme. • This apo PTK6-KD is in DFG-in and αC-helix-out conformation.

60 APPLIED LIFE SCIENCES↗
DOE OSTI2021

Microstructural Analysis of Cadmium Whiskers on Long-Term-Used Hardware

A survey of cadmium plated field return hardware showed ubiquitous cadmium whisker growth. The most worn and debris-covered hardware showed the densest whisker growth. Whiskers were often found growing in agglomerates of nodules and whiskers. The hardware was rinsed with alcohol to transfer whiskers and debris from the hardware to a flat stub. Fifty whiskers were studied individually by scanning electron microscopy (SEM), including energy dispersive spectroscopy (EDS) and electron backscatter diffraction (EBSD). Most of the whiskers were single crystal, though three were found to contain grain boundaries at kinks. The whiskers ranged from 5 to 600 μm in length and 80 pct showed a $<\bar{1} 2 \bar{1} 0>$ type growth direction. This growth direction facilitates the development of low energy side faces of the whisker, (0001) and {1010}.

36 MATERIALS SCIENCE↗
DOE OSTI2015

First stage of reaction of molten Al with MgO substrate

The Al/MgO couple was produced in vacuum (~ 5 × 10{sup −} {sup 4} Pa) by contact heating from RT up to 1000 °C and holding at that temperature for 1 h of a small 4 × 4 × 4 mm aluminium (5 N) sample placed on the [100] MgO single crystal substrate. TEM observations backed with electron diffraction analysis indicated that the interaction between liquid aluminium and MgO starts from a redox reaction producing a continuous layer of MgAl{sub 2}O{sub 4} spinel on the substrate surface. Its growth is controlled by solid state out-diffusion of magnesium and oxygen towards the surface being in contact with liquid metal. The thickening of spinel layer is accompanied by its cracking and infiltration with aluminium. The above process enables local dissolution of the MgO substrate and formation in it of a thin region of interpenetrating metallic channels walled with spinel. The removal of dissolved magnesium through open aluminium channels towards the drop and to vacuum locally produces areas of aluminium enriched with dissolved oxygen, which results in the nucleation of α-Al{sub 2}O{sub 3} at spinel clad walls. The growth of α-Al{sub 2}O{sub 3} is controlled only by the dissolution rate of MgO by aluminium, liquid state diffusion of Mg to drop/vacuum and oxygen to the front of the of α-Al{sub 2}O{sub 3} crystallites growing into MgO substrate. - Highlights: • New unique evidence of first stages of interaction of liquid Al with MgO substrates • Interaction of liquid Al with MgO starts with the formation of a layer MgAl{sub 2}O{sub 4}. • Growth of MgAl{sub 2}O{sub 4} is slow as controlled by solid state out-diffusion of Mg and O. • MgAl{sub 2}O{sub 4} serves as a nucleation site for Al{sub 2}O{sub 3} and consumed by it soon after. • Growth of Al{sub 2}O{sub 3} is fast as controlled by diffusion in liquid state.

36 MATERIALS SCIENCE↗
DOE OSTI2026

Cs X Si 15 P 21 ( X = Sn or Pb): Polar Noncentrosymmetric Si–P Frameworks Stabilized by Covalent X –P Bonding

Metal silicon phosphides composed of earth-abundant Si and P tend to exhibit semiconducting properties and adopt diverse crystal structures with relatively small additions of structure-directing elements. The potential of silicon phosphide materials in nonlinear optical applications has been hindered by the inability to systematically produce noncentrosymmetric structures with such a flexible framework. Here, in this work, two isostructural compounds with a novel noncentrosymmetric structure were made possible by the inclusion of elements with stereochemically active lone pairs (Sn 2+ and Pb 2+ ). The structures were determined through single-crystal and synchrotron powder X-ray diffraction. Analysis of chemical bonding in real space through the electron localization function revealed stereochemically active Pb 2+ and Sn 2+ species in a trigonal pyramidal coordination with {Pb/Sn}–P bonds. Such covalent bonding between Pb and P is quite uncommon in extended solids and has been reported in a few rare instances. Band structure calculations and linear optical measurements confirm the semiconducting nature of Cs X Si 15 P 21 ( X = Sn or Pb). The synthesis was optimized to yield high-purity polycrystalline samples. The nonlinear optical properties show promising second-harmonic generation (SHG) coefficients from the Kurtz–Perry method. First-principles calculations of the nonlinear optical properties support the experimentally determined SHG values and provide moderate values of birefringence, suggesting Cs X Si 15 P 21 could be phase-matchable and practical nonlinear optical materials in the mid-IR region.

crystal structure↗
DOE OSTI2019

An Entropically Stabilized Fast-Ion Conductor: Li 3.25 [Si 0.25 P 0.75 ]S 4

We report on a family of lithium fast ion conductors, Li 3+x [Si x P 1–x ]S 4 , that exhibit an entropically stabilized structure type in a solid solution regime (0.15 < x < 0.33) with superionic conductivity above 1 mS·cm –1 . Exploration of the influence of aliovalent substitution in the thermodynamically unstable β-Li 3 PS 4 lattice using a combination of single crystal X-ray and powder neutron diffraction, the maximum entropy method, and impedance spectroscopy reveals that substitution induces structural splitting of the localized Li sites, effectively stabilizing bulk β-Li 3 PS 4 at room temperature and delocalizing lithium ion density. The optimal material, Li 3.25 [S i0.25 P 0.75 ]S 4 , exhibits inherent entropic site disorder and a frustrated energy landscape, resulting in a high conductivity of 1.22 mS·cm –1 that represents an increase of three orders of magnitude compared to bulk β-Li 3 PS 4 and one order of magnitude higher than the nanoporous form. The enhanced ion conduction and lowered activation barrier with increasing site disorder as a result of aliovalent “tuning” reveals an important strategy toward the design of fast ion conductors that are vital as solid state electrolytes.

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

Trickier than It Looks: Isomerization between Five- and Six-Coordinated Zinc in Heterometallic Li 2 Zn 2 Molecule

This report describes the synthesis and characterization of two hetero bi metallic Li–Zn coordination isomers [Li 2 Zn 2 (tbaoac) 6 ] (tbaoac = tert -butyl acetoacetato) that have been isolated separately by the same stoichiometric reaction run in different organic solvents. The 6-coordinated zinc isomer ( 6-Zn ) was synthesized in acetone with high yield, while the 5-coordinated one ( 5-Zn ) was readily obtained from ethanol. The 5-Zn isomer has a low solubility in organic solvents such as alkanes and haloalkanes, while its 6-Zn counterpart exhibits a good solubility in almost all common solvents. Two isomeric molecules feature similar centrosymmetric tetranuclear cyclic assemblies, which are different in their arrangement of tbaoac ligands. While all ligands act as μ 2 -type in the structure of 5-Zn , the two tbaoac groups chelating Li appear as μ 3 -type in 6-Zn , thus providing an additional coordination for Zn ions. However, the real structural transformation between these isomers was shown to be more complex than simply making or breaking a couple of Zn–O bonds. X-ray single-crystal structure analysis, powder X-ray diffraction, multinuclear NMR, DART mass spectrometry, ICP-OES analysis, and TGA have been employed for the characterization of the isomers. The combination of powder X-ray diffraction and 1 H NMR investigation revealed that 6-Zn isomer can be quantitatively transformed to 5-Zn in ethanol, while the reverse conversion instantly takes place in acetone.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2015

Synthesis, Structure, and Rigid Unit Mode-like Anisotropic Thermal Expansion of BaIr 2 In 9

This Article reports the synthesis of large single crystals of BaIr 2 In 9 using In flux and their characterization by variable-temperature single-crystal and synchrotron powder X-ray diffraction, resistivity, and magnetization measurements. The title compound adopts the BaFe 2 Al 9 -type structure in the space group P6/mmm with room temperature unit cell parameters a = 8.8548(6) angstrom and c = 4.2696(4) A. BaIr 2 In 9 exhibits anisotropic thermal expansion behavior with linear expansion along the c axis more than 3 times larger than expansion in the ab plane between 90 and 400 K. This anisotropic expansion originates from a rigid unit mode-like mechanism similar to the mechanism of zero and negative thermal expansion observed in many anomalous thermal expansion materials such as ZrW 2 O 8 and ScF 3 .

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2019

New Family of Argyrodite Thioantimonate Lithium Superionic Conductors

We report on a new family of argyrodite lithium superionic conductors, as solid solutions Li 6+x MxSb 1–x S 5 I (M = Si, Ge, Sn), that exhibit superionic conductivity. These represent the first antimony argyrodites to date. Exploration of the series using a combination of single crystal X-ray and synchrotron/neutron powder diffraction, combined with impedance spectroscopy, reveals that an optimal degree of substitution (x), and substituent induces slight S 2– /I – anion site disorder—but more importantly drives Li + cation site disorder. The additional, delocalized Li-ion density is located in new high energy lattice sites that provide intermediate interstitial positions (local minima) for Li + diffusion and activate concerted ion migration, leading to a low activation energy of 0.25 eV. Excellent room temperature ionic conductivity of 14.8 mS·cm –1 is exhibited for cold-pressed pellets—up to 24 mS·cm –1 for sintered pellets—among the highest values reported to date. This enables all-solid-state battery prototypes that exhibit promising properties. Furthermore, even at -78 °C, suitable bulk ionic conductivity of the electrolyte is retained (0.25 mS·cm –1 ). Selected thioantimonate iodides demonstrate good compatibility with Li metal, sustaining over 1000 h of Li stripping/plating at current densities up to 0.6 mA·cm –2 . The significantly enhanced Li ion conduction and lowered activation energy barrier with increasing site disorder reveals an important strategy toward the development of superionic conductors.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2019

High-pressure polymorphism in L -threonine between ambient pressure and 22 GPa

The crystal structure of L -threonine has been studied to a maximum pressure of 22.3 GPa using single-crystal X-ray and neutron powder diffraction. The data have been interpreted in the light of previous Raman spectroscopic data by Holanda et al. (J. Mol. Struct. (2015), 1092, 160–165) in which it is suggested that three phase transitions occur at ca. 2 GPa, between 8.2 and 9.2 GPa and between 14.0 and 15.5 GPa. In the first two of these transitions the crystal retains its P2 1 2 1 2 1 symmetry, in the third, although the unit cell dimensions are similar either side of the transition, the space group symmetry drops to P2 1 . The ambient pressure form is labelled phase I, with the successive high-pressure forms designated I', II and III, respectively. Phases I and I' are very similar, the transition being manifested by a slight rotation of the carboxylate group. Phase II, which was found to form between 8.5 and 9.2 GPa, follows the gradual transformation of a long-range electrostatic contact becoming a hydrogen bond between 2.0 and 8.5 GPa, so that the transformation reflects a change in the way the structure accommodates compression rather than a gross change of structure. Phase III, which was found to form above 18.2 GPa in this work, is characterised by the bifurcation of a hydroxyl group in half of the molecules in the unit cell. Density functional theory (DFT) geometry optimisations were used to validate high-pressure structural models and PIXEL crystal lattice and intermolecular interaction energies are used to explain phase stabilities in terms of the intermolecular interactions.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2016

“Glass-like” thermal conductivity gradually induced in thermoelectric Sr{sub 8}Ga{sub 16}Ge{sub 30} clathrate by off-centered guest atoms

The origin of the “glass-like” plateau in thermal conductivity of inorganic type I clathrates has been debated for more than a decade. Here, it is demonstrated that the low temperature thermal conductivity of Sr{sub 8}Ga{sub 16}Ge{sub 30} can be controlled by the synthesis method: A flux-grown sample has a “glass-like” plateau in thermal conductivity at low temperature, while a zone-melted sample instead has a crystalline peak. A combination of flux-growth and zone-melting produces an intermediate thermal conductivity. In a comprehensive study of three single crystal samples, it is shown by neutron diffraction that the transition from crystalline peak to “glass-like” plateau is related to an increase in Sr guest atom off-centering distance from 0.24 Å to 0.43 Å. By modifying ab initio calculated force constants for the guest atom to an isotropic model, we reproduce both measured heat capacity and inelastic neutron scattering data. The transition from peak to plateau in the thermal conductivity can be modeled by a combined increase of Rayleigh and disorder scattering. Measurement of heat capacity refutes simple models for tunneling of Sr between off-center sites. Furthermore, the electronic properties of the same samples are characterized by Hall carrier density, Seebeck coefficient, and resistivity. The present comprehensive analysis excludes tunneling and charge carrier scattering as dominant contributors to the “glass-like” plateau. The increased guest atom off-centering distance controlled by synthesis provides a possible microscopic mechanism for reducing the low temperature thermal conductivity of clathrates.

71 CLASSICAL AND QUANTUM MECHANICS, GENERAL PHYSIC↗
DOE OSTI2019

Consequences of magnetic ordering in chiral M n 1 / 3 Nb S 2

We have investigated here the structural, magnetic, thermodynamic, and charge-transport properties of M n 1 / 3 Nb S 2 single crystals through x-ray and neutron diffraction, magnetization, specific heat, magnetoresistance, and Hall-effect measurements. M n 1 / 3 Nb S 2 displays a magnetic transition at T C ~ 45 K with highly anisotropic behavior expected for a hexagonal-structured material. Below T C , neutron diffraction reveals increased scattering near the structural Bragg peaks having a wider Q dependence along the c axis than the nuclear Bragg peaks. This indicates either a short-range ferromagnetic (FM) order with a domain size of ~250 nm along the c axis or a possible magnetic modulation with a large pitch length. The expectation of a significant Dzyaloshinskii-Moriya interaction in this chiral-structured magnet, along with the helical state discovered in isostructural C r 1 / 3 Nb S 2 , suggest either a long period helical state with q ~ 0.0025 Å - 1 , or FM regions separated by magnetic solitons, may be responsible for the apparent small size of the FM domains. Here, the domain length along the c axis is substantially larger than the pitch length of 48 nm found for the helimagnetic state in C r 1 / 3 Nb S 2 . Specific-heat-capacity measurements confirm a second-order magnetic phase transition with a substantial magnetic contribution that persists to low temperature. The low-temperature specific-heat capacity is consistent with a large density of low-lying magnetic excitations that are likely associated with topologically interesting magnetic modes. Changes to the magnetoresistance, the magnetization, and the magnetic neutron diffraction, which become more apparent below 20 K, imply a modification in the character of the magnetic ordering corresponding to the magnetic contribution to the specific-heat capacity. These determinations signify a more complex magnetic structure both at zero and finite fields for M n 1 / 3 Nb S 2 than for the well-investigated C r 1 / 3 Nb S 2 .

36 MATERIALS SCIENCE↗
DOE OSTI2016

Surface structure of coherently strained ceria ultrathin films

Cerium oxide, or ceria, is an important material for solid oxide fuel cells and water splitting devices. Although the ceria surface is active in catalytic and electrochemical reactions, how its catalytic properties are affected by the surface structure under operating conditions is far from understood. We investigate the structure of the coherently strained CeO 2 ultrathin films on yttria-stabilized zirconia (001) single crystals by specular synchrotron x-ray diffraction (XRD) under oxidizing conditions as a first step to study the surface structure in situ . An excellent agreement between the experiment data and the model is achieved by using a “stacks and islands” model that has a two-component roughness. One component is due to the tiny clusters of nanometer scale in lateral dimensions on each terrace, while the other component is due to slightly different CeO 2 thickness that span over hundreds of nanometers on neighboring terraces. We attribute the nonuniform thickness to step depairing during the thin film deposition that is supported by the surface morphology results on the microscopic level. Importantly, our model also shows that the polarity of the ceria surface is removed by a half monolayer surface coverage of oxygen. In conclusion, the successful resolution of the ceria surface structure using in situ specular synchrotron XRD paves the way to study the structural evolution of ceria as a fuel cell electrode under catalytically relevant temperatures and gas pressures.

36 MATERIALS SCIENCE↗