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Results for “single-crystal x-ray diffraction”

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
NASA NTRS1988

High-pressure phase diagram and equation of state of solid helium from single-crystal X-ray diffraction to 23.3 GPa

Single-crystal X-ray diffraction measurements have been performed on solid He-4 from 15.6 to 23.3 GPa at 300 K with synchrotron radiation. The diffraction patterns demonstrate that the structure of the solid is hexagonal close packed over this pressure-temperature range, contrary to both the interpretation of high-pressure optical studies and to theoretical predictions. The solid is more compressible than is indicated by equations of state calculated with recently determined helium pair potentials. The results suggest that a significant revision of current views of the phase diagram and energetics of dense solid helium is in order.

Mao, H. K.↗
NASA NTRS1988

Crystal structure and density of helium to 232 kbar

The properties of helium and hydrogen at high pressure are topics of great interest to the understanding of planetary interiors. These materials constitute 95 percent of the entire solar system. A technique was presented for the measurement of X-ray diffraction from single-crystals of low-Z condenses gases in a diamond-anvil cell at high pressure. The first such single-crystal X-ray diffraction measurements on solid hydrogen to 26.5 GPa were presented. The application of this technique to the problem of the crystal structure, equation of state, and phase diagram of solid helium is reported. Crucial for X-ray diffraction studies of these materials is the use of a synchrotron radiation source which provides high brillance, narrow collimation of the incident and diffracted X-ray beams to reduce the background noise, and energy-dispersive diffraction techniques with polychromatic (white) radiation, which provides high detection efficiency.

Mao, H. K.↗
NASA NTRS1972

Petrology of basaltic and monomineralic soil fragments from the Sea of Fertility.

Basaltic and monomineralic fragments from the 150-425 micron size fractions of the Luna 16 core obtained from the Sea of Fertility were studied by optical petrographic, electron microprobe, and single-crystal X-ray diffraction techniques. Three textural varieties were identified in the basalts (intersertal, subophitic, and recrystallized). These textures, the assemblages, and individual mineral compositions (especially pyroxenes) indicate that these basalts crystallized under conditions very similar to those from Apollo 11. The pyroxenes have slightly lower Ti/Al (atomic) ratios than the Apollo 11 pyroxenes. We interpret the presence of octahedral Al as being due to the low TiO2/Al2O3 (weight %) ratio in the bulk rock. All observations made on the fine-grained basalt fragments are consistent with a rapid, near-surface, one-stage crystallization history.

Bence, A. E.↗
NASA NTRS1972

Apollo 14 inverted pigeonites - Possible samples of lunar plutonic rocks.

Analysis of 'inverted pigeonites' found in Apollo 14 samples 14082 and 14083 (a polymict breccia, the 'white rock') by a combination of optical, electron probe, and single-crystal X-ray diffraction techniques. These 'inverted pigeonites' are regarded as samples of plutonic rocks that have been blasted out of the Imbrium Basin. It is also concluded that lunar pigeonites will invert to orthopyroxenes, given sufficiently slow cooling histories even in very anhydrous environments.

Papike, J. J.↗
NASA NTRS1973

Petrology of fine-grained rock fragments and petrologic implications of single crystal from the Luna 20 soil.

Only fine-grained rocks are present in the Luna 20 samples, and coarser-grained rocks are represented by fragments of single crystals. A petrologic study has been made of 47 fine-grained crystalline rocks, microbreccias, and glassy aggregates. In addition, a total of 33 single crystals of pyroxene, plagioclase, olivine, and spinel, in the size range from 125 to 500 microns, have been examined using electron microprobe and single-crystal X-ray diffraction techniques. The most abundant fine-grained crystalline rocks in the samples examined are recrystallized anorthositic norite and anorthositic troctolite. Gabbroic rocks, anorthosite, and KREEP basalt are present but not common. Most of the single crystals of pyroxene and plagioclase could have been derived from coarser-grained noritic, troctolitic, and anorthositic rocks. However, three of the 14 pyroxene crystals, and two of the five olivine crystals have Fe/(Fe + Mg) contents greater than 0.45 and are believed to have been derived from mare basalts or related rocks.

Cameron, K. L.↗
NASA NTRS1975

Relative cooling rates of mare basalts at the Apollo 12 and 15 sites as estimated from pyroxene exsolution data

X-ray single-crystal diffraction studies, supplemented by electron microprobe analyses of core pigeonites and rim augites from rocks 12031, 15085, 15475, and 15495, have been used to suggest cooling rates for these and other Apollo 12 and 15 rocks studied by similar methods. The extent of subsolidus phase separation of pyroxenes is used as a measure of the cooling rate. The results were interpreted in terms of model cooling histories of a lava flow whose thickness was estimated from the absolute cooling rates obtained by cooling rate experiments and by temperature-time variation through an extrusive flow computed by employing simplified theory of Jaeger. All available data on the exsolution and cation distributions of pyroxenes from Apollo 12 and 15 samples at present are consistent with the hypothesis that these rocks were derived from the top and interior of lava flows with thicknesses of 4-10 m. A process for exsolution of augite from a host pigeonite on (100) has been related to its low-calcium content.

Takeda, H.↗
NASA NTRS2001

The Crystal and Molecular Structure of Acetatochlorobis(4-methylpyridine)oxovanadium (IV)

The crystal and molecular structure of the title compound, VOCl(O2CCH3)(4-CH3C5H4N)2, has been determined by single-crystal x-ray diffraction. The material crystallizes in the space group P 1(bar) (#2) with a = 7.822(2), b = 8.023(l), c = 14.841(2) Angstroms, alpha = 99.73(l), beta = 91.41(l), and gamma = 117.13(l). The coordination geometry around the vanadium is a highly distorted octahedron. The molecule is remarkable for being a monomeric oxovanadium (IV) carboxylate. A generalized synthetic strategy is proposed for the preparation of oxovanadium (IV) monomers.

Schupp, John D.↗
NASA NTRS2005

Lunar and Planetary Science XXXVI, Part 6

Contents include the following: A Model for Multiple Populations of Presolar Diamonds. Characterization of Martian North Polar Geologic Units Using Mars Odyssey THEMIS Data. Effect of Flow on the Internal Structure of the Martian North Polar Layered Deposits. Elemental Abundance Distributions in Basalt Clays and Meteorites: Is It a Biosignature? Early Results on the Saturn System from the Composite Infrared Spectrometer. NanoSIMS D/H Imaging of Isotopically Primitive Interplanetary Dust Particles. Presolar (Circumstellar and Interstellar) Phases in Renazzo: The Effects of Parent Body Processing. Catastrophic Disruption of Hydrated Targets: Implications for the Hydrated Asteroids and for the Production of Interplanetary Dust Particles. Chemical and Mineralogical Analyses of Particles from the Stratospheric Collections Coinciding with the 2002 Leonid Storm and the 2003 Comet Grigg-Skjellerup Trail Passage. An Analysis of the Solvus in the CaS-MnS System. ESA s SMART-1 Mission at the Moon: First Results, Status and Next Steps. Europa Analog Ice-splitting Measurements and Experiments with Ice-Hunveyor on the Frozen Balaton-Lake, Hungary. Chromium on Eros: Further Evidence of Ordinary Chondrite Composition. Dust Devil Tracks on Mars: Observation and Analysis from Orbit and the Surface. Spatial Variation of Methane and Other Trace Gases Detected on Mars: Interpretation with a General Circulation Model. Mars Water Ice and Carbon Dioxide Seasonal Polar Caps: GCM Modeling and Comparison with Mars Express Omega Observations. Component Separation of OMEGA Spectra with ICA. Clathrate Formation in the Near-Surface Environment of Titan. Space Weathering: A Proposed Laboratory Approach to Explaining the Sulfur Depletion on Eros. Sample Collection from Small Airless Bodies: Examination of Temperature Constraints for the TGIP. Sample Collector for the Hera Near-Earth Asteroid Sample Return Mission. A Rugged Miniature Mass-Spectrometer for Measuring Aqueous Geochemistry on Mars. Martian and Lunar Pyroxene Microstructures Studied by Single-Crystal X-Ray Diffraction.

Source record↗
NASA NTRS1988

Synchrotron X-ray diffraction measurements of single-crystal hydrogen to 26.5 gigapascals

The crystal structure and equation of state of solid hydrogen have been determined directly to 26.5 gigapascals at room temperature by new synchrotron X-ray diffraction techniques. Solid hydrogen remains in the hexagonal close packed structure under these pressure-temperature conditions and exhibits increasing structural anisotropy with pressure. The pressure-volume curve determined from the X-ray data represents the most accurate experimental measurement of the equation of state to date in this pressure range. The results remove the discrepancy between earlier indirect determinations and provide a new experimental constraint on the molecular-to-atomic transition predicted at higher pressures.

Mao, H. K.↗
NASA NTRS1994

Structure and stability of hydrous minerals at high pressure

The presence of even small amounts of hydrogen in the Earth's deep interior may have profound effects on mantle melting, rheology, and electrical conductivity. The recent discovery of a large class of high-pressure H-bearing silicates further underscores the potentially important role for hydrous minerals in the Earth's mantle. Hydrogen may also be a significant component of the Earth's core, as has been recently documented by studies of iron hydride at high pressure. In this study, we explore the role of H in crystal structures at high pressure through detailed Raman spectroscopic and x ray diffraction studies of hydrous minerals compressed in diamond anvil cells. Brucite, Mg(OH)2, has a simple structure and serves as an analogue for the more complex hydrous silicates. Over the past five years, this material has been studied at high pressure using shock-compression, powder x ray diffraction, infrared spectroscopy, Raman spectroscopy, and neutron diffraction. In addition, we have recently carried out single-crystal synchrotron x-ray diffraction on Mg(OH)2 and Raman spectroscopy on Mg(OD)2 at elevated pressure. From all these studies, an interesting picture of the crystal chemical behavior of this material at high pressure is beginning to emerge. Some of the primary conclusions are as follows: First, hydrogen bonding is enhanced by the application of pressure. Second, layered minerals which are elastically anisotropic at low pressure may not be so at high pressure. Furthermore, the brucite data place constraints on the effect of hydrogen on seismic velocities and density at very high pressure. Third, the stability of hydrous minerals may be enhanced at high P by subtle structural rearrangements that are difficult to detect using traditional probes and require detailed spectroscopic analyses. Finally, brucite appears to be unique in that it undergoes pressure-induced disordering that is confined solely to the H-containing layers of the structure.

Duffy, T. S.↗
NASA NTRS2004

Disordered Zinc in Zn4Sb3 with Phonon-Glass and Electron-Crystal Thermoelectric Properties

By converting waste heat into electricity, thermoelectric generators could be an important part of the solution to today's energy challenges. The compound Zn4Sb3 is one of the most efficient thermoelectric materials known. Its high efficiency results from an extraordinarily low thermal conductivity in conjunction with the electronic structure of a heavily doped semiconductor. Previous structural studies have been unable to explain this unusual combination of properties. Here, we show through a comprehensive structural analysis using single-crystal X-ray and powder-synchrotron-radiation diffraction methods, that both the electronic and thermal properties of Zn4Sb3 can be understood in terms of unique structural features that have been previously overlooked. The identification of Sb3- ions and Sb-2(4-) dimers reveals that Zn4Sb3 is a valence semiconductor with the ideal stoichiometry Zn13Sb10. In addition, the structure contains significant disorder, with zinc atoms distributed over multiple positions. The discovery of glass-like interstitial sites uncovers a highly effective mechanism for reducing thermal conductivity. Thus Zn4Sb3 is in many ways an ideal 'phonon glass, electron crystal' thermoelectric material.

phases↗
NASA NTRS1988

Experimental study of planetary gases with applications to planetary interior models

High-pressure experimental data on planetary materials are critical in developing planetary models and in addressing otherwise insoluble problems of the internal structure of the major planets. Progress in the last five years has been particularly marked. Maximum static pressure of 550 GPa was achieved. For the first time, X-ray diffraction of solidified gases (Ne, Xe) and ices (H2O) were obtained at pressures above one megabar, single-crystal diffraction of ultralight elements (H2, He) were detected up to 25 GPa, pressures over 200 GPa at 77 K were reached in solid hydrogen, including the discovery of a phase transformation in the molecular solid. Advances in instrumentation and new measurements performed during 1983 to 1988 are summarized.

Bell, Peter M.↗
NASA NTRS1985

Temperature dependence of gamma-gamma prime lattice mismatch in nickel-base superalloys

High temperature X-ray diffraction techniques were used to determine the gamma-gamma prime lattice mismatch of three different nickel-base superalloys at temperatures between 18 and 1000 C. The measurements were performed on oriented single-crystal disks which had been aged to produce a semicoherent gamma-gamma prime structure. The thermal expansion of the lattice parameters of the gamma and gamma-prime phases was described by a second-order polynomial expression. The expansion of the gamma-prime phase was consistently smaller than that of the gamma phase, which caused the lattice mismatch to become more negative at higher temperatures. It was also shown that high values of lattice mismatch resulted in increased rates of directional gamma-prime coarsening during elevated temperature creep exposure.

Nathal, M. V.↗
NASA NTRS2002

Failure Morphologies of Cyclically Oxidized ZrO2-Based Thermal Barrier Coatings

Advanced and baseline thermal barrier coatings (TBCs) were thermal cycle tested in air at 1163 C until delamination or spallation of the ceramic top coat. The top coat of the advanced TBC s consisted of ZrO2 with various amounts of Y2O3, Yb2O3, Gd2O3, or Nd2O3 dopants. The composition of the top coat of the baseline TBC was ZrO2-8wt.%Y2O3. All top coats were deposited by air plasma spraying. A NiCrAlY or NiCoCrAlY bond coat was deposited by low pressure plasma spraying onto a single-crystal, Ni-base superalloy. The TBC lifetime for the baseline coatings was approximately 190 cycles (45 minutes at 1163 C per cycle) while the lifetime for the advanced coatings was as high as 425 cycles. The fracture surfaces and sample cross sections were examined after TBC failure by SEM and optical microscopy, and the top coats were further examined by X-ray diffraction. These post-test studies revealed that the fracture path largely followed splat boundaries with some trans-splat fracture. However, there were no obvious distinguishing features which explained the difference in TBC lifetimes between some of the advanced and baseline coatings.

Nesbitt, James A.↗
NASA NTRS1981

Silicide surface phases on gold

The crystalline silicide layers formed on (111) and (100) surfaces of Au films on various Si single-crystal substrates are studied by LEED and AES in conjunction with sputter-depth profiling as a function of annealing temperature. On the (111) surface, three basic silicide structures are obtained corresponding to layers of various thicknesses as obtained by different preparation conditions. The (100) surface shows only two different structures. None of the structures is compatible with the various bulk silicide structures deduced from X-ray diffraction. Using LEED as a criterion for the presence or absence of silicide on the surface, smaller layer thicknesses are obtained than reported previously on the basis of AES studies.

Green, A. K.↗
NASA NTRS1975

Evaluation of silicon ribbon material for solar cell fabrication

Optical microscopy, electron microscopy, and X-ray diffraction were utilized to characterize silicon ribbon structure. Complex twin formation was observed in nearly all ribbons examined. Twins formed in the 110-plane 112-line ribbon orientation appear stable, and this orientation may be preferable when the ribbon is utilized for solar cells. In addition to twinning, grain boundaries and other structural defects were observed in the ribbon material. Hall effect, resistivity, spreading resistance, surface photovoltage, and solar cell electrical/optical measurements were performed on ribbon samples and correlated with structural and ribbon growth characteristics. Only those ribbon samples with either single-crystal structure or with 'parallel' twin formations were capable of solar-cell performance approaching that of Czochralski material.

Leipold, M.↗
NASA NTRS1976

Interaction of metal layers with polycrystalline Si

Solid-phase reactions of metal films deposited on 0.5-micron-thick polycrystalline layers of Si grown by chemical vapor deposition at 640 C were investigated by MeV He-4 backscattering spectrometry, glancing angle X-ray diffraction, and SEM observations. For the metals Al, Ag, and Au, which form simple eutectics, heat treatment at temperatures below the eutectic results in erosion of the poly-Si layer and growth of Si crystallites in the metal film. Crystallite formation is observed at temperatures exceeding 550 C for Ag, at those exceeding 400 C for Al, and at those exceeding 200 C for Au films. For Pd, Ni, and Cr, heat treatment results in silicide formation. The same initial silicides (Pd2Si, Ni2Si, and CrSi2), are formed at similar temperatures on single-crystal substrates.

Nakamura, K.↗
NASA NTRS2001

A Compact X-Ray System for Support of High Throughput Crystallography

Standard x-ray systems for crystallography rely on massive generators coupled with optics that guide X-ray beams onto the crystal sample. Optics for single-crystal diffractometry include total reflection mirrors, polycapillary optics or graded multilayer monochromators. The benefit of using polycapillary optic is that it can collect x-rays over tile greatest solid angle, and thus most efficiently, utilize the greatest portion of X-rays emitted from the Source, The x-ray generator has to have a small anode spot, and thus its size and power requirements can be substantially reduced We present the design and results from the first high flux x-ray system for crystallography that combine's a microfocus X-ray generator (40microns FWHM Spot size at a power of 45 W) and a collimating, polycapillary optic. Diffraction data collected from small test crystals with cell dimensions up to 160A (lysozyme and thaumatin) are of high quality. For example, diffraction data collected from a lysozyme crystal at RT yielded R=5.0% for data extending to 1.70A. We compare these results with measurements taken from standard crystallographic systems. Our current microfocus X-ray diffraction system is attractive for supporting crystal growth research in the standard crystallography laboratory as well as in remote, automated crystal growth laboratory. Its small volume, light-weight, and low power requirements are sufficient to have it installed in unique environments, i.e.. on-board International Space Station.

Ciszak, Ewa↗