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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 1,747 records · Page 97
All sourcesNASA NTRSDOE OSTI
DOE OSTI2012

Purification, crystallization and preliminary X-ray diffraction analysis of the carbohydrate-binding region of the Streptococcus gordonii adhesin GspB

The carbohydrate-binding region of the bacterial adhesin GspB from Streptococcus gordonii strain M99 (GspB{sub BR}) was expressed in Escherichia coli and purified using affinity and size-exclusion chromatography. Separate sparse-matrix screening of GspB{sub BR} buffered in either 20 mM Tris pH 7.4 or 20 mM HEPES pH 7.5 resulted in different crystallographic behavior such that different precipitants, salts and additives supported crystallization of GspB{sub BR} in each buffer. While both sets of conditions supported crystal growth in space group P2{sub 1}2{sub 1}2{sub 1}, the crystals had distinct unit-cell parameters of a = 33.3, b = 86.7, c = 117.9 {angstrom} for crystal form 1 and a = 34.6, b = 98.3, c = 99.0 {angstrom} for crystal form 2. Additive screening improved the crystals grown in both conditions such that diffraction extended to beyond 2 {angstrom} resolution. A complete data set has been collected to 1.3 {angstrom} resolution with an overall R{sub merge} value of 0.04 and an R{sub merge} value of 0.33 in the highest resolution shell.

59 BASIC BIOLOGICAL SCIENCES↗
DOE OSTI2011

Crystallization and Preliminary Diffraction Analysis of Truncated Human Pleckstrin

Pleckstrin is a major substrate of protein kinase C in platelets and leukocytes and appears to play an important role in exocytosis through a currently unknown mechanism. Pleckstrin function is regulated by phosphorylation, which is thought to cause dissociation of pleckstrin dimers, thereby facilitating phosphoinositide interactions and membrane localization. Evidence also exists suggesting that phosphorylation causes a subtle conformational change in pleckstrin. Structural studies of pleckstrin have been initiated in order to characterize these structural changes and ultimately advance understanding of pleckstrin function. Here, the crystallization and preliminary X-ray diffraction analysis of a truncated version of pleckstrin consisting of the N-terminal PH domain, the protein kinase C phosphorylation sites and the DEP domain (NPHDEP) are reported. In addition, the oligomeric state and phospholipid-binding properties of NPHDEP were analyzed. This work demonstrates that NPHDEP behaves as a monomer in solution and suggests that all three pleckstrin domains contribute to the dimerization interface. Furthermore, based on the binding properties of NPHDEP, the C-terminal PH domain appears to increase the specificity of pleckstrin for phosphoinositides. This work represents a significant step towards determining the structure of pleckstrin.

59 BASIC BIOLOGICAL SCIENCES↗
DOE OSTI2012

Crystallization and preliminary X-ray diffraction analysis of Val57 mutants of the amyloidogenic protein human cystatin C

Human cystatin C (hCC) is a low-molecular-mass protein (120 amino-acid residues, 13 343 Da) found in all nucleated cells. Its main physiological role is regulation of the activity of cysteine proteases. Biologically active hCC is a monomeric protein, but all crystallization efforts have resulted in a dimeric domain-swapped structure. Recently, two monomeric structures were reported for cystatin C variants. In one of them stabilization was achieved by abolishing the possibility of domain swapping by the introduction of an additional disulfide bridge connecting the two protein domains (Cys47-Cys69). In the second structure, reported by this group, the monomeric hCC fold was preserved by stabilization of the conformationally constrained loop (L1) by a single-amino-acid substitution (V57N). To further assess the influence of changes in the sequence and properties of loop L1 on the dimerization propensity of cystatin C, two additional hCC mutants were obtained: one with a residue favoured in {beta}-turns (V57D) and another with proline (V57P), a residue that is known to be a structural element that can rigidify but also broaden turns. Here, the expression, purification and crystallization of V57D and V57P variants of recombinant human cystatin C are described. Crystals were grown by the vapour-diffusion method. Several diffraction data sets were collected using a synchrotron source at the Advanced Photon Source, Argonne National Laboratory, Chicago, USA.

43 PARTICLE ACCELERATORS↗
DOE OSTI2025

Shifting and tilting towards enhanced piezoelectricity in high-temperature ceramics: an average structure study of (1 − x )BiFe 2/8 Ti 3/8 Mg 3/8 O 3 – x PbTiO 3 through X-ray and neutron diffraction

A comprehensive report is provided of the average structure of a high Curie temperature ferroelectric ceramic, (1 − x)BiFe 2/8 Ti 3/8 Mg 3/8 O 3 –xPbTiO 3 (BFTM–xPT) when x = 0.25–0.375 at room temperature. Both neutron and synchrotron X-ray powder diffraction data were collected and combined Rietveld refinements were completed. These data revealed that, of the compositions studied, BFTM–xPT crystallizes as mixed phase material. At x = 0.25–0.275, the average structure of each phase is best described by space groups R3c and Cc. At 0.30 ≥ x ≥ 0.35, a morphotropic phase boundary is present and is best modelled by space groups P4mm and Cc, where space group Cc is the dominant phase. As the concentration of PbTiO 3 increases, the amount of octahedral tilting decreases and x = 0.375 exhibits a loss of octahedral tilting and crystallizes in space groups P4mm and Cm. In conclusion, an updated phase diagram at room temperature of this novel system is given and structural intricacies responsible for its piezoelectric properties are revealed.

high Curie temperature↗
DOE OSTI2013

X-ray and neutron diffraction study of the defect crystal structure of the as-grown nonstoichiometric phase Y{sub 0.715}Ca{sub 0.285}F{sub 2.715}

This work begins a series of papers aimed at studying the defect structure of nonstoichiometric phases R{sub 1-y}Ca{sub y}F{sub 3-y} with a tysonite-type (LaF{sub 3}) structure. In the single-crystal structure of Y{sub 0.715}Ca{sub 0.285}F{sub 2.715} with a tysonite-type small unit cell (sp. gr. P6{sub 3}/mmc, a = 3.9095(2) A, c = 6.9829(2) A; Z = 2; R{sub w} = 2.16%), the displacements of Y{sup 3+} cations and F{sup 2-} anions from 6{sub 3} symmetry axes were observed for the first time. The X-ray diffraction pattern shows weak satellites insufficient for structural calculations. The LaF{sub 3} structure type is stabilized up and down on the temperature scale due to anion vacancies and the symmetrizing effect of Ca{sup 2+} cations lying on 6{sub 3} symmetry axes. At 120 Degree-Sign C the fluoride-ion conductivity in the nonstoichiometric phase Y{sub 0.715}Ca{sub 0.285}F{sub 2.715} is five orders of magnitude higher than that in the stoichiometric phase {beta}-YF{sub 3}. The transition to a superionic state is caused by a deviation from stoichiometry and is not associated with reconstructive phase transformation.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗
DOE OSTI2012

On the ability of resonant diffraction gratings to differentiate a pulsed optical signal

The passage of an optical pulse through a resonant grating is considered. The conditions under which the resonant grating differentiates the envelope of the incident pulse are determined. It is shown that the necessary condition for computing the k-order derivative is the presence of k resonances in the transmission spectrum of the grating in the vicinity of the central frequency of the incident pulse. A method is described for constructing the stacked structure for computing the kth derivative on the basis of repetition of the structure for computing the first derivative. The results of numerical simulation of diffraction of the pulse from the analyzed structure for computing the first, second, and third derivative are presented.

71 CLASSICAL AND QUANTUM MECHANICS, GENERAL PHYSIC↗
DOE OSTI2010

X-ray diffraction analysis and scanning micro-Raman spectroscopy of structural irregularities and strains deep inside the multilayered InGaN/GaN heterostructure

High-resolution X-ray diffraction analysis and scanning confocal Raman spectroscopy are used to study the spatial distribution of strains in the In{sub x}Ga{sub 1-x}N/GaN layers and structural quality of these layers in a multilayered light-emitting diode structure produced by metal-organic chemical vapor deposition onto (0001)-oriented sapphire substrates. It is shown that elastic strains almost completely relax at the heterointerface between the thick GaN buffer layer and In{sub x}Ga{sub 1-x}N/GaN buffer superlattice. It is established that the GaN layers in the superlattice are in a stretched state, whereas the alloy layers are in a compressed state. In magnitude, the stretching strains in the GaN layers are lower than the compressive strains in the InGaN layers. It is shown that, as compared to the buffer layers, the layers of the superlattice contain a smaller number of dislocations and the distribution of dislocations is more randomly disordered. In micro-Raman studies on scanning through the thickness of the multilayered structure, direct evidence is obtained for the asymmetric gradient distributions of strains and crystal imperfections of the epitaxial nitride layers along the direction of growth. It is shown that the emission intensity of the In{sub x}Ga{sub 1-x}N quantum well is considerably (more than 30 times) higher than the emission intensity of the GaN barrier layers, suggesting the high efficiency of trapping of charge carriers by the quantum well.

36 MATERIALS SCIENCE↗
DOE OSTI2019

Study of Kinetics of Solid Phase Transition in Tetracosane С{sub 24}Н{sub 50} by High-Resolution Synchrotron X-Ray Powder Diffraction

Using the small-angle synchrotron X-ray diffraction method at the research facility “BELOK” of the Kurchatov synchrotron radiation source at the NRC Kurchatov Institute, it was shown that the first-order solid phase transition in tetracosane C{sub 24}H{sub 50} passes according to a heterogeneous mechanism in a narrow temperature range ΔT ~ 1 K in accordance with the theory of diffuse phase transitions.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗
DOE OSTI2019

Measurement of Residual Stresses by X-ray Diffraction Near Simulated Heat Affected Zones in Austenitic Stainless Steels

Simulated heat-affected zones (HAZs) were made in austenitic stainless steel specimens using a Gleeble. The samples were heated to temperatures as high as 1100°C by computer controlled resistance heating. By controlling the heating rate, maximum temperature, and cooling rate, a wide range of residual stresses were introduced in the specimens. Stress measurements were made using X-ray diffraction. It was found that significant stress gradients were produced in the simulated HAZs, and that all stresses were compressive in nature, both in the longitudinal and transverse directions. These results are not representative of the residual stresses determined in the HAZs of real welds, thus calling into question some aspects of the role of the Gleeble in such simulations.

36 MATERIALS SCIENCE↗
DOE OSTI2011

Spectroscopic and X-ray Diffraction Study of Structural Disorder in Cryomilled and Amorphous Griseofulvin

Structural disorder induced by cryogenic milling and by heating to the amorphous phase in the active pharmaceutical ingredient Griseofulvin has been studied using Raman spectroscopy, X-ray powder diffraction (XRPD), and fluorescence spectroscopy. A broad, exciting-frequency-independent scattering background in the Raman spectra and changes in intensities and splitting of some of the Raman lines due to lattice and molecular modes have been observed. In the cryomilled samples this strong background is deconvoluted into two components: one due to lattice disorder induced by cryomilling and the other due to Mie scattering from nanosized crystallites. A single-component background scattering attributed to lattice disorder is seen in the Raman spectrum of the amorphous sample. Fluorescence measurements showed an intrinsic fluorescence signal in as-received Griseofulvin that does not correspond to the inelastic background in the Raman spectra and, moreover, decreases in intensity upon cryomilling, thus excluding an assignment of the Raman background intensity to impurity- or molecular-defect-induced fluorescence. Wide-angle XRPD measurements on cryomilled Griseofulvin shows a broad two-component background consistent with the background-scattering component in the Raman data associated with lattice disorder, but at longer correlation lengths. Persistence of this disorder to even longer lengths is evident in small-angle synchrotron XRPD data on micronized Griseofulvin taken as a function of temperature from the crystalline to the amorphous phase.

74 ATOMIC AND MOLECULAR PHYSICS↗
DOE OSTI2023

Utah FORGE: Powder X-ray Diffraction Data from Well 16A(78)-32 Core

This dataset from Lawrence Livermore National Laboratory (LLNL) consists of four raw X-ray diffraction (XRD) scans and preliminary results of quantitative XRD analysis. The scanned samples were prepared from four subcores, which came from various depths of the FORGE well 16A(78)-32 core. Desired core lengths were selected from available core photos (on GDR), provided by FORGE personnel, and subcored at LLNL. The XRD scans were collected in May 2023 at LLNL as pre-experimental characterization data for these subcores, which will be used in core-flooding experiments at LLNL and in triaxial direct shear experiments at Los Alamos National Laboratory as part of DOE Project 5-2428. XRD scans are in RAW file format (e.g., FORGE-5477-full.raw) and are suitable for viewing and analysis using open-source quantitative XRD software (e.g., Profex; www.profex-xrd.org ) and/or other proprietary instrument software.

15 GEOTHERMAL ENERGY↗
DOE OSTI2021

Ultrafast X-ray Diffraction Study of a Shock-Compressed Iron Meteorite above 100 GPa

Natural kamacite samples (Fe92.5Ni7.5) from a fragment of the Gibeon meteorite were studied as a proxy material for terrestrial cores to examine phase transition kinetics under shock compression for a range of different pressures up to 140 GPa. In situ time-resolved X-ray diffraction (XRD) data were collected of a body-centered cubic (bcc) kamacite section that transforms to the high-pressure hexagonal close-packed (hcp) phase with sub-nanosecond temporal resolution. The coarse-grained crystal of kamacite rapidly transformed to highly oriented crystallites of the hcp phase at maximum compression. The hcp phase persisted for as long as 9.5 ns following shock release. Comparing the c/a ratio with previous static and dynamic work on Fe and Fe-rich Fe-Ni alloys, it was found that some shots exhibit a larger than ideal c/a ratio, up to nearly 1.65. This work represents the first time-resolved laser shock compression structural study of a natural iron meteorite, relevant for understanding the dynamic material properties of metallic planetary bodies during impact events and Earth’s core elasticity.

36 MATERIALS SCIENCE↗
DOE OSTI2010

Beamline electrostatic levitator for in situ high energy x-ray diffraction studies of levitated solids and liquids

Determinations of the phase formation sequence, crystal structures and the thermo-physical properties of materials at high temperatures are hampered by contamination from the sample container and environment. Containerless processing techniques, such as electrostatic (ESL), electromagnetic, aerodynamic, and acoustic levitation, are most suitable for these studies. An adaptation of ESL for in situ structural studies of a wide range of materials using high energy (30-130 keV) x rays at a synchrotron source is described here. This beamline ESL (BESL) allows the in situ determination of the atomic structures of equilibrium solid and liquid phases, undercooled liquids and time-resolved studies of solid-solid and liquid-solid phase transformations. The use of area detectors enables the rapid acquisition of complete diffraction patterns over a wide range (0.5-14 {angstrom}{sup -1}) of reciprocal space. The wide temperature range (300-2500 K), containerless processing environment under high vacuum (10{sup -7}-10{sup -8} Torr), and fast data acquisition capability, make BESL particularly well suited for phase stability studies of high temperature solids and liquids. An additional, but important, feature of BESL is the capability for simultaneous measurements of a host of thermo-physical properties including the specific heat, enthalpy of transformation, solidus and liquidus temperatures, density, viscosity, and surface tension, all on the same sample during the structural measurements.

36 MATERIALS SCIENCE↗
DOE OSTI2010

Single-crystal synchrotron X-ray diffraction study of wustite and magnesiowustite at lower-mantle pressures

This study demonstrates the use of monochromatic synchrotron X-ray radiation of 40 keV for high-precision equation-of-state studies on sets of single crystals analysed individually in the same diamond-anvil pressure cell. Angle-dispersive zone-axis diffraction patterns were obtained from crystals of wuestite-Fe{sub 0.93}O and magnesiowuestite-(Mg{sub 0.73}Fe{sub 0.27})O to 51 GPa in a hydrostatic helium pressure medium. The rhombohedral phase of Fe{sub 0.93}O was observed above 23 GPa, and its isothermal bulk modulus (K{sub 0}) was determined to be 134 ({+-}4) GPa, assuming K' = 4. The rhombohedral phase of Fe{sub 0.93}O is more compressible than B1-structured Fe{sub 0.93}O, with K{sub 0} = 146 ({+-}2) GPa. Magnesiowuestite-(Mg{sub 0.73}Fe{sub 0.27})O remains cubic over the experimental pressure range, and has a bulk modulus of 154 ({+-}3) GPa with K' = 4.0 ({+-}0.1).

43 PARTICLE ACCELERATORS↗
DOE OSTI2010

Strategies for reducing preferred orientation and strain in powder samples for high-pressure synchrotron X-ray diffraction in diamond-anvil cells

Among the many problems associated with high-pressure X-ray diffraction from polycrystalline samples in the diamond-anvil cell are strain and preferred orientation. A method is presented for efficiently reducing preferred orientation of powder samples compressed in diamond-anvil cells to pressures in excess of 20 GPa. This method may be successfully applied to samples of yield strength higher than alkalihalides. In addition, the problem of strain is discussed using ice-VII as an example and as an illustration of the importance of laser heating as a method of minimizing strain.

36 MATERIALS SCIENCE↗
DOE OSTI2011

Real-Time Studies of Pulsed Laser Deposition Using Surface X-ray Diffraction

We review recent results in the study of the growth kinetics in pulsed laser deposition by real-time surface x-ray diffraction. Interlayer transport as the primary driving force behind formation of atomically sharp interfaces is analyzed quantitatively from the measurements of time constants and from shot-to-shot changes in the single laser shot time dependent coverages in the model perovskite SrTiO3. The results show that direct deposition into the open layers and very fast interlayer transport driven by energetic species during the arrival of the laser plume are the main components of layer growth per a laser shot. Diffuse scattering was used to study the role of the island size distribution and island size evolution in moderating interlayer transport. We conclude that interference with fast interlayer transport is the main factor in departure from layer-by-layer growth in both homo- and heteroepitaxy of complex oxides.

36 MATERIALS SCIENCE↗
DOE OSTI2011

The Crystal Structures of two Anhydrous Magnesium Hydroxychloride Phases from in situ Synchrotron Powder Diffraction Data

The crystal structures of two members of the solid solution series Mg(OH){sub x}Cl{sub y}x+y = 2, Mg(OH){sub 1.7}Cl{sub 0.3} (P{sup {bar 3}}m1, a = 3.169(2) {angstrom}, c = 5.530(12), V = 48.1(1) {angstrom}{sup 3} at T = 365 C) and MgOHCl (R{sup {bar 3}}m, a = 3.3877(4) {angstrom}, c = 17.534(4) {angstrom}, V = 174.27(6) {angstrom}{sup 3} at T = 625 C) were determined from in situ synchrotron powder diffraction data at high temperature upon dehydration of 3Mg(OH){sub 2} {center_dot} MgCl{sub 2} {center_dot} 8H{sub 2}O (F3) and 5Mg(OH){sub 2} {center_dot} MgCl{sub 2} {center_dot} 8H{sub 2}O (F5) phases. The crystal structures of Mg(OH){sub 1.7}Cl{sub 0.3} (example of ss-type-OH) and MgOHCl (example of ss-type-Cl) can be related to the C19 (CdCl{sub 2}) and C6 (CdI{sub 2}) structure type, respectively, with the disordered chloride and hydroxide anions occupying the same crystallographic site in layers.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗