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At least 667 records · Page 37
All sourcesNASA NTRSDOE OSTI
DOE OSTI2013

Fergusonite-type CeNbO{sub 4+δ}: Single crystal growth, symmetry revision and conductivity

Large fergusonite-type (ABO{sub 4}, A=Ce, B=Nb) oxide crystals, a prototype electrolyte composition for solid oxide fuel cells (SOFC), were prepared for the first time in a floating zone mirror furnace under air or argon atmospheres. While CeNbO{sub 4} grown in air contained CeNbO{sub 4.08} as a minor impurity that compromised structural analysis, the argon atmosphere yielded a single phase crystal of monoclinic CeNbO{sub 4}, as confirmed by selected area electron diffraction, powder and single crystal X-ray diffraction. The structure was determined in the standard space group setting C12/c1 (No. 15), rather than the commonly adopted I12/a1. AC impedance spectroscopy conducted under argon found that stoichiometric CeNbO{sub 4} single crystals showed lower conductivity compared to CeNbO{sub 4+δ} confirming interstitial oxygen can penetrate through fergusonite and is responsible for the higher conductivity associated with these oxides. - Graphical abstract: Large fergusonite-type CeNbO{sub 4} crystals were prepared for the first time in a floating zone mirror furnace. Crystal growth in an argon atmosphere yielded a single phase monoclinic CeNbO4, as confirmed by selected area electron diffraction, powder and single crystal X-ray diffraction. The structure was determined in the standard space group setting C12/c1 (No. 15), rather than the commonly adopted I12/a1. AC impedance spectroscopy found CeNbO{sub 4} single crystals showed lower conductivity compared to CeNbO{sub 4+δ} confirming interstitial oxygen can penetrate through fergusonite and is responsible for the higher conductivity associated with these oxides. Highlights: • Preparation of single crystals of CeNbO{sub 4} using a floating zone mirror furnace. • Correction to the crystal symmetry of the monoclinic form of CeNbO{sub 4}. • Report the conductivity of a single crystal of CeNbO{sub 4}.

36 MATERIALS SCIENCE↗
NASA NTRS1972

A graphite crystal polarimeter for stellar X-ray astronomy.

The first crystal X-ray polarimeter to be used for X-ray astronomy is described. Polarization is measured by modulation of the X rays diffracted at an average 45 deg glancing angle from large, curved graphite crystal panels as these rotate about an axis parallel to the incident X-ray flux. Arrangement of the crystal panels, the design of the detector, and the signal-processing circuitry were optimized to minimize systematic effects produced by off-axis pointing of the rocket and cosmic ray induced events. The in-flight performance of the instrument in relation to the observed background signal is discussed.

Weisskopf, M. C.↗
NASA NTRS2004

Petrographic Evidence for Rapid Heating and Cooling During Chrondrule Formation

The chondrule cooling rates used in most chondrule-formation models appear to be too low. Recent petrographic evidence indicates that the amount of crystal (especially olivine) growth that occurred after the last melting event was about 30 smaller than the grain sizes simulated in order to estimate cooling rates. The smaller amount of growth leads to an upwards revision of cooling rates by about a factor of 1000. Most chondrules are porphyritic. They consist of large and small crystals of olivine and, less commonly, pyroxene immersed in a mesostasis having a plagioclase-rich composition. In the most primitive chondrites the mesostasis is often vitreous. Because the large majority of chondrules contain FeS, it is clear that the nebula had cooled below the FeS condensation temperature (ca. 650 K) before chondrule formation occurred. The high FeO/(FeO+MgO) ratios of some chondrules require still lower nebular temperatures (less than 500 K). The traditional view has been that porphyritic chondrules formed in a single heating/cooling event and many laboratory experiments have been carried out in various kinds of kinds of furnaces to try to simulate the formation of chondrules textures in a single heating/cooling cycle. These furnace experiments have been used to infer the cooling rates of chondrules during the temperature range at which olivine crystallized from the melt. Most of these inferred values are in the range 0.01-1 K per second. These low cooling rates are problematical because there is no long-term nebular environment that yields such values. In transparent regions chondrules would cool at rates orders of magnitude higher, whereas in an opaque nebular disk the cooling rates would be many orders of magnitude lower. And these latter conditions are not suitable locations for chondrule formation because such high temperatures would cause the complete evaporation of chondrules (which have melting temperatures about 600 K higher than their evaporation temperatures). During the last several years several kinds of petrographic evidence indicating rapid chondrule cooling have been recognized. These include thin overgrowths on relict grains, clusters of small crystals that grew following the most recent melting event, and fragments preserving shardlike shapes that would have been hidden had several tens of micrometers of new growth occurred following the last melting event. And there are other indications of rapid cooling including the preservation of volatiles such as FeS and one case where the modeling of O-isotopic and FeO/(FeO+MgO) gradients indicated a high cooling rate.

Wasson, J. T.↗
DOE OSTI2024

Stressful crystal histories recorded around melt inclusions in volcanic quartz

Abstract Magma ascent and eruption are driven by a set of internally and externally generated stresses that act upon the magma. We present microstructural maps around melt inclusions in quartz crystals from six large rhyolitic eruptions using synchrotron Laue X-ray microdiffraction to quantify elastic residual strain and stress. We measure plastic strain using average diffraction peak width and lattice misorientation, highlighting dislocations and subgrain boundaries. Quartz crystals across studied magma systems preserve similar and relatively small magnitudes of elastic residual stress (mean 53–135 MPa, median 46–116 MPa) in comparison to the strength of quartz (~ 10 GPa). However, the distribution of strain in the lattice around inclusions varies between samples. We hypothesize that dislocation and twin systems may be established during compaction of crystal-rich magma, which affects the magnitude and distribution of preserved elastic strains. Given the lack of stress-free haloes around faceted inclusions, we conclude that most residual strain and stress was imparted after inclusion faceting. Fragmentation may be one of the final strain events that superimposes stresses of ~ 100 MPa across all studied crystals. Overall, volcanic quartz crystals preserve complex, overprinted deformation textures indicating that quartz crystals have prolonged deformation histories throughout storage, fragmentation, and eruption.

58 GEOSCIENCES↗
DOE OSTI2015

Characterization of submillisecond response optical addressing phase modulator based on low light scattering polymer network liquid crystal

Optically addressed conventional nematic liquid crystal spatial light modulator has attracted wide research interests. But the slow response speed limited its further application. In this paper, polymer network liquid crystal (PNLC) was proposed to replace the conventional nematic liquid crystal to enhance the response time to the order of submillisecond. The maximum light scattering of the employed PNLC was suppressed to be less than 2% at 1.064 μm by optimizing polymerization conditions and selecting large viscosity liquid crystal as solvent. The occurrence of phase ripple phenomenon due to electron diffusion and drift in photoconductor was found to deteriorate the phase modulation effect of the optical addressed PNLC phase modulator. The wavelength effect and AC voltage frequency effect on the on state dynamic response of phase change was investigated by experimental methods. These effects were interpreted by electron diffusion and drift theory based on the assumption that free electron was inhomogeneously distributed in accordance with the writing beam intensity distribution along the incident direction. The experimental results indicated that the phase ripple could be suppressed by optimizing the wavelength of the writing beam and the driving AC voltage frequency when varying the writing beam intensity to generate phase change in 2π range. The modulation transfer function was also measured.

71 CLASSICAL AND QUANTUM MECHANICS, GENERAL PHYSIC↗
NASA NTRS1981

Orientation dependence of the stress rupture properties of Nickel-base superalloy single crystals

The influence of orientation of the stress rupture behavior of Mar-M247 single crystals was studied. Stress rupture tests were performed at 724 MPa and 774 C where the effect of anisotropy is prominent. The mechanical behavior of the single crystals was rationalized on the basis of the Schmid factors for the operative slip systems and the lattice rotations which the crystals underwent during deformation. The stress rupture lives were found to be greatly influenced by the lattice rotations required to produce intersecting slip, because steady-state creep does not begin until after the onset of intersecting slip. Crystals which required large rotations to become oriented for intersecting slip exhibited a large primary creep strain, a large effective stress level at the onset of steady-state creep, and consequently a short stress rupture life. A unified analysis was attained for the stress rupture behavior of the Mar-M247 single crystals tested in this study at 774 C and that of the Mar-M200 single crystals tested in a prior study at 760 C. In this analysis, the standard 001-011-111 stereographic triangle was divided into several regions of crystallographic orientation which were rank ordered according to stress rupture life for this temperature regime. This plot indicates that those crystals having orientations within about 25 deg of the 001 exhibited significantly longer lives when their orientations were closer to the 001-011 boundary of the stereographic triangle than to the 001-111 boundary.

Mackay, R. A.↗
DOE OSTI2022

Large-Area Periodic Arrays of Atomically Flat Single-Crystal Gold Nanotriangles Formed Directly on Substrate Surfaces

The advancement of nanoenabled wafer-based devices requires the establishment of core competencies related to the deterministic positioning of nanometric building blocks over large areas. Within this realm, plasmonic single-crystal gold nanotriangles represent one of the most attractive nanoscale components but where the formation of addressable arrays at scale has heretofore proven impracticable. In this work, a benchtop process is presented for the formation of large-area periodic arrays of gold nanotriangles. The devised growth pathway sees the formation of an array of defect-laden seeds using lithographic and vapor-phase assembly processes followed by their placement in a growth solution promoting planar growth and threefold symmetric side-faceting. The nanotriangles formed in this high-yield synthesis distinguish themselves in that they are epitaxially aligned with the underlying substrate, grown to thicknesses that are not readily obtainable in colloidal syntheses, and present atomically flat pristine surfaces exhibiting gold atoms with a close-packed structure. As such, they express crisp and unambiguous plasmonic modes and form photoactive surfaces with highly tunable and readily modeled plasmon resonances. The devised methods, hence, advance the integration of single-crystal gold nanotriangles into device platforms and provide an overall fabrication strategy that is adaptable to other nanomaterials.

42 ENGINEERING↗
DOE OSTI2022

The Effects of Mixing Multi-Component HLW Glasses on Spinel Crystal Size

The Hanford Waste Treatment and Immobilization Plant will vitrify radioactive waste into borosilicate glass. The high-level waste (HLW) glass formulations are constrained by processing and property requirements, including restrictions aimed at avoiding detrimental impacts of spinel crystallization in the melter. To understand the impact of glass chemistry on crystallization, two HLW glasses precipitating small (?5 µm) spinel crystals were individually mixed with a glass that precipitated large (?45 µm) spinel crystals in ratios of 25, 50, and 75 wt%. The size of spinel crystals in the mixed glasses varied from 5 to 20 µm. Small crystal size was attributed to: (1) high concentrations of nuclei due to the presence of ruthenium oxide and (2) chromium oxide aiding high rates of nucleation. Results indicate that the spinel crystal size can be controlled using chromium oxide and/or noble metal concentrations in the melt, even in complex mixtures like HLW glasses. Small crystals tend to settle slowly, so they are acceptable in the melter without a risk of failure. Allowing higher concentrations of spinel-forming waste components in the waste glass enables glass compositions with higher waste loading, thus increasing plant operational flexibility. An additional benefit to the presence of chromium oxide in the glass composition is the potential for the oxide to protect melter walls against corrosion.

Lonergan, Charmayne E.↗
DOE OSTI2022

Polytypism in semi-disordered lizardite and amesite by low-dose HAADF-STEM

Serpentine minerals exert important controls on the physical properties of ultramafic rocks and have the potential to influence deformation phenomena in fault zones and to control the release of water in subducted slabs. Sheet serpentine generally, and lizardite and amesite specifically, can adopt alternative crystallographic stacking arrangements called polytypes. Polytypism has been extensively studied in fully ordered crystals, but it remains largely enigmatic in the more common semi-disordered crystals that in long-range analyses such as X-ray diffraction only exhibit random combinations of 0b and ±1/3b interlayer shifts. To date, atomic-resolution imaging to identify locally ordered polytypes has been precluded by the beam-sensitive nature of this hydrous magnesium silicate mineral. Here, in this study, we employed low-dose high-angle annular dark-field scanning transmission electron microscopy (HAADF-STEM) to study the polytypic structure of semi-disordered lizardite and amesite. Because the electron dose was as low as ~6000 e–/Å 2 , it was possible to directly resolve oxygen atomic columns and all the cations with a resolution of ~1 Å and reveal the short-range order. For lizardite, we identified long-period non-standard polytypes, including examples with 3, 4, 8, and 9 layers stemming from the ordering of the octahedral tilt along the a-axis. For amesite, we found short-range ordered polytypes with periodicities of up to 42 Å stemming from the ordering of interlayer shifts along the b-axis. The resolution was sufficient to determine the relative abundance of 6R 2 , 6R 1 , 2H 1 , and 2H 2 polytypes in amesite to be 46.1, 29.6, 7.7, and 1.9%, respectively. This is contrary to the expectation that the most common form of amesite is the 2H 2 polytype, which may be more likely to form macroscopic crystals suitable for conventional X-ray diffraction-based studies. We conclude that HAADF-STEM methods open the way for the characterization of beam-sensitive minerals and to resolve the structural details of less well-ordered (but possibly more abundant) minerals at a unit-cell scale.

58 GEOSCIENCES↗
DOE OSTI2015

Thermal neutron filter design for the neutron radiography facility at the LVR-15 reactor

In 2011 a decision was made to build a neutron radiography facility at one of the unused horizontal channels of the LVR-15 research reactor in Rez, Czech Republic. One of the key conditions for operating an effective radiography facility is the delivery of a high intensity, homogeneous and collimated thermal neutron beam at the sample location. Additionally the intensity of fast neutrons has to be kept as low as possible as the fast neutrons may damage the detectors used for neutron imaging. As the spectrum in the empty horizontal channel roughly copies the spectrum in the reactor core, which has a high ratio of fast neutrons, neutron filter components have to be installed inside the channel in order to achieve desired beam parameters. As the channel design does not allow the instalment of complex filters and collimators, an optimal solution represent neutron filters made of large single-crystal ingots of proper material composition. Single-crystal silicon was chosen as a favorable filter material for its wide availability in sufficient dimensions. Besides its ability to reasonably lower the ratio of fast neutrons while still keeping high intensities of thermal neutrons, due to its large dimensions, it suits as a shielding against gamma radiation from the reactor core. For designing the necessary filter dimensions the Monte-Carlo MCNP transport code was used. As the code does not provide neutron cross-section libraries for thermal neutron transport through single-crystalline silicon, these had to be created by approximating the theory of thermal neutron scattering and modifying the original cross-section data which are provided with the code. Carrying out a series of calculations the filter thickness of 1 m proved good for gaining a beam with desired parameters and a low gamma background. After mounting the filter inside the channel several measurements of the neutron field were realized at the beam exit. The results have justified the expected calculated values. After the successful filter installing and a series of measurements, first test neutron radiography attempts with test samples could been carried out. (authors)

21 SPECIFIC NUCLEAR REACTORS AND ASSOCIATED PLANTS↗
DOE OSTI2017

Alloy-assisted deposition of three-dimensional arrays of atomic gold catalyst for crystal growth studies

Large-scale assembly of individual atoms over smooth surfaces is difficult to achieve. A configuration of an atom reservoir, in which individual atoms can be readily extracted, may successfully address this challenge. In this work, we demonstrate that a liquid gold-silicon alloy established in classical vapor-liquid-solid growth can deposit ordered and three-dimensional rings of isolated gold atoms over silicon nanowire sidewalls. Here, we perform ab initio molecular dynamics simulation and unveil a surprising single atomic gold-catalyzed chemical etching of silicon. Experimental verification of this catalytic process in silicon nanowires yields dopant-dependent, massive and ordered 3D grooves with spacing down to similar to 5 nm. Finally, we use these grooves as self-labeled and ex situ markers to resolve several complex silicon growths, including the formation of nodes, kinks, scale-like interfaces, and curved backbones.

36 MATERIALS SCIENCE↗
NASA NTRS1991

Growth of large, defect-free pure C60 single crystals

Millimeter-sized single crystals of C60 were grown by sublimation of C60 powder in a vacuum for 6-24 h. The crystals had excellent facets, were free of C70 or solvent, and showed face-centered cubic symmetry with a very small mosaic spread down to 0.01 deg.

Meng, R. L.↗
DOE OSTI2024

Controlling the Crystal Packing and Morphology of Metal–Organic Macrocycles through Side-Chain Modification

Supramolecular nanotubes constructed from the self-assembly of conjugated metal–organic macrocycles provide a unique collection of materials properties, including solution processability, porosity, and electrical conductivity. Here we show how small modifications to the macrocycle periphery subtly alter the noncovalent interactions governing self-assembly, leading to large changes in crystal packing, crystal morphology, and materials properties. Specifically, we synthesized five distinct copper-based macrocycles that differ in either the steric bulk, polarity, or hydrogen-bonding ability of the peripheral side chains. We show that the electrical conductivity of these macrocycles is highly sensitive to steric bulk, decreasing by 3 orders of magnitude upon introduction of peripheral neopentyl substituents. Here, we further show that the introduction of hydrogen-bonding groups leads to more ordered packing and a dramatic increase in crystallite size. Together, these results establish side-chain engineering as a rich toolkit for controlling the packing structure, particle morphology, and bulk properties of conjugated metal–organic macrocycles.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2018

Polyelectrolyte Complex Films Influence the Formation of Polycrystalline Micro-Structures

Silica-carbonate biomorphs are inorganic materials composed of thousands of crystalline nanorods that assemble complex morphologies such as helices, vessels, and sheets. We investigate the effect on biomorph crystallization of polyelectrolyte complex films that are prepared using the layer-by-layer deposition technique and post-processed to obtain three stable, chemically distinct films. Biomorph growth on poly(diallyldimethylammonium)-dominated substrates (cationic) shows polycrystalline helical and sheet structures bounded by large witherite prisms. Crystallization on poly(styrenesulfonate)-dominated (anionic) and stoichiometric substrates follows a qualitatively different pathway. We observe islands of radial mineral films that over several days extend at a remarkably constant velocity of 0.48 µm/h and eventually mineralize the whole substrate. Our work opens exciting avenues for the use of polyelectrolyte films as tunable substrates for biomimetic crystallization.

Nakouzi, Elias↗
DOE OSTI2026

Towards time-resolved MicroED grid preparation using mix-and-inject gas dynamic virtual nozzles

Recent progress in gas dynamic virtual nozzle (GDVN) technologies in combination with high-brilliance synchrotron and X-ray free-electron lasers (XFELs) has allowed the visualization of protein dynamics in crystallo by mixing macromolecular protein crystals with a substrate using tunable mixing times on the order of milliseconds to seconds prior to serial X-ray diffraction data collection. This has become the method of choice for high-resolution structure determination of intermediate states. However, such experiments require large counts of crystals of proper sizes for high-resolution data collection, and premium beam times for screening efforts. Cryogenic microcrystal electron diffraction (MicroED) represents a complementary technique that may be a more accessible avenue for time-resolved nanocrystallography compared with serial X-ray diffraction experiments. MicroED can produce full diffraction datasets from just a few submicrometre-thick crystals, and the approach is more readily accessible, requiring standard cryogenic transmission electron microscopy (TEM) equipment available at many universities and institutes. Cryogenic MicroED, like other forms of cryo-EM, begins with rapidly freezing biological material on electron microscopy grids. In the case of MicroED, micro- to nano-crystals (<500 nm thick) are deposited onto electron microscopy grids and plunge-frozen for subsequent electron diffraction data collection. Here, we have incorporated GDVN technology developed originally for XFEL experiments into the freezing process as a first step towards time-resolved studies. We describe the limited deposition efficiency of the model MicroED protein proteinase K on TEM grids using GDVNs, preceding sample vitrification and successful MicroED data collection. We discuss both the initial results from such experiments and the methodological challenges in developing this approach into a reliable workflow for millisecond-to-second time-resolved structural studies of macromolecules. Our results promise a strategy to deposit crystals on grids using GDVNs and determine high-resolution structures by MicroED, constituting a first step towards development of time-resolved MicroED experiments.

MicroED↗