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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 1,405 records · Page 78
All sourcesNASA NTRSDOE OSTI
DOE OSTI2019

Acousto-optic modulators for a controlled frequency shift of light beams in optical and microwave cold-atom frequency standards

A series of specialised acousto-optic modulators/frequency shifters based on paratellurite (TeO{sub 2}) single crystals is developed for systems of laser cooling and frequency stabilisation of laser sources in optical and microwave frequency standards based on cold strontium, rubidium and caesium atoms. The methods of calculation and optimisation of the main parameters of acousto-optic modulators are considered; their basic technical characteristics are experimentally investigated in the spectral range of optical radiation 460 – 900 nm and in the frequency shift range of 5 – 400 MHz. The modulators have a high diffraction efficiency, low power consumption and the ability to work with linearly and randomly polarised optical radiation. (frequency standards)

71 CLASSICAL AND QUANTUM MECHANICS, GENERAL PHYSIC↗
DOE OSTI2019

Growth of Yb : Na{sub 2}SO{sub 4} crystals and study of their spectral – luminescent characteristics

Ytterbium-doped single crystals of the high-temperature hexagonal sodium sulphate modification are grown by the Czochralski method. It is found by energy dispersive analysis that the crystallisation occurs congruently. The Yb : Na{sub 2}SO{sub 4} crystals have additional (with respect to Yb{sup 3+} ions) absorption bands in the regions of 650, 850 and 1150 nm, which obviously belong to colour centres. The luminescence spectrum of the Yb : Na{sub 2}SO{sub 4} single crystal noticeably differs from the luminescence spectrum of Yb : YAG crystals by the presence of a broad band without a prominent peak. The luminescence decay curve for the powder is single-exponential with a time constant of 1175 μs, which is somewhat larger than that for the Yb : YAG crystal. The lifetime of the ytterbium excited state does not change during storage of the samples in air for a week. (active media)

71 CLASSICAL AND QUANTUM MECHANICS, GENERAL PHYSIC↗
DOE OSTI2020

Multifrequency stimulated Raman scattering of light in a calcite single crystal

Using pulses of multifrequency stimulated Raman scattering (SRS) in calcite, nonlinear photoluminescence in a stilbene molecular crystal is excited. When multifrequency SRS is excited by the radiation of a Nd{sup 3+} : YAG laser with a wavelength of 1064 nm, eleven anti-Stokes components are observed in the visible spectrum with an average frequency shift of 1086 cm{sup −1} between them. Using the second harmonic of the Nd {sup 3+} : YAG laser radiation allowed three anti-Stokes and four Stokes components to be recorded. The large spectral range of the frequency comb facilitated effective reduction in the duration and increase in the intensity of the radiation pulse of multifrequency SRS. (nonlinear optical phenomena)

71 CLASSICAL AND QUANTUM MECHANICS, GENERAL PHYSIC↗
DOE OSTI2020

Relaxation oscillations in a bipolarised Nd : YAG laser with a Fabry – Perot cavity

Based on the model of a bipolarised laser, which takes into account real orientations of absorbing and emitting dipoles of active centres in the unit cell of an Nd : YAG single crystal, we have shown that the appearance of low-frequency relaxation oscillations requires the participation of both competing pump channels through linearly and circularly polarised dipole transitions. (paper)

46 INSTRUMENTATION RELATED TO NUCLEAR SCIENCE AND ↗
DOE OSTI2020

Influence of growth temperature of KTiOAsO{sub 4} single crystals on their physicochemical parameters and formation of domain structures

A potassium titanyl arsenate (KTiOAsO{sub 4}, KTA) crystal 50 × 80 × 60 mm in size has been grown by upgraded Czochralski method from flux (TGGS) with a decrease in temperature from 900 to 770 °C during pulling. It is shown that the spectroscopic properties of the parts of KTA crystals grown at 900 and 770 °C are close, whereas the electrical conductivity of the low-temperature (770 °C) KTA part turned out to be an order of magnitude lower than that of the high-temperature part. Visualisation of the domain structure by second-harmonic generation microscopy revealed a more efficient domain intergrowth (throughout the sample) in the low-temperature KTA, which is important for forming a regular domain structure (RDS) in a KTA-based nonlinear optical element. It is established that the quantum efficiency of parametric generation of light in the RDS formed in low-temperature KTA is several times higher than in the case of high-temperature KTA. The results obtained are important for optimising RDS parameters. (paper)

71 CLASSICAL AND QUANTUM MECHANICS, GENERAL PHYSIC↗
DOE OSTI2015

CIRCUMSTELLAR MAGNETITE FROM THE LAP 031117 CO3.0 CHONDRITE

We report the first microstructural confirmation of circumstellar magnetite, identified in a petrographic thin section of the LaPaz Icefield 031117 CO3.0 chondrite. The O-isotopic composition of the grain indicates an origin in a low-mass (∼2.2 M{sub ⊙}), approximately solar metallicity red/asymptotic giant branch (RGB/AGB) star undergoing first dredge-up. The magnetite is a single crystal measuring 750 × 670 nm, is free of defects, and is stoichiometric Fe{sub 3}O{sub 4}. We hypothesize that the magnetite formed via oxidation of previously condensed Fe dust within the circumstellar envelope of its progenitor star. Using an empirically derived rate constant for this reaction, we calculate that such oxidation could have occurred over timescales ranging from approximately ∼9000–500,000 years. This timescale is within the lifetime of estimates for dust condensation within RGB/AGB stars.

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

Quantum critical fluctuations in the heavy fermion compound Ce(Ni 0.935 Pd 0.065 ) 2 Ge 2

Electric resistivity, specific heat, magnetic susceptibility, and inelastic neutron scattering experi- ments were performed on a single crystal of the heavy fermion compound Ce(Ni 0.935 Pd 0.065 ) 2 Ge 2 in order to study the spin fluctuations near an antiferromagnetic (AF) quantum critical point (QCP). The resistivity and the specific heat coefficient for T ≤ 1 K exhibit the power law behavior expected for a 3D itinerant AF QCP (ρ(T) ~ T 3/2 and γ(T) ~ γ 0 - bT 1/2 ). However, for 2 ≤ T ≤ 10 K, the susceptibility and specific heat vary as log T and the resistivity varies linearly with temperature. Furthermore, despite the fact that the resistivity and specific heat exhibit the non-Fermi liquid behavior expected at a QCP, the correlation length, correlation time, and staggered susceptibility of the spin fluctuations remain finite at low temperature. We suggest that these deviations from the divergent behavior expected for a QCP may result from alloy disorder.

36 MATERIALS SCIENCE↗
DOE OSTI2014

Radiopurity of CaWO{sub 4} crystals for direct dark matter search with CRESST and EURECA

The direct dark matter search experiment CRESST uses scintillating CaWO{sub 4} single crystals as targets for possible WIMP scatterings. An intrinsic radioactive contamination of the crystals as low as possible is crucial for the sensitivity of the detectors. In the past CaWO{sub 4} crystals operated in CRESST were produced by institutes in Russia and the Ukraine. Since 2011 CaWO{sub 4} crystals have also been grown at the crystal laboratory of the Technische Universität München (TUM) to better meet the requirements of CRESST and of the future tonne-scale multi-material experiment EURECA. The radiopurity of the raw materials and of first TUM-grown crystals was measured by ultra-low background γ-spectrometry. Two TUM-grown crystals were also operated as low-temperature detectors at a test setup in the Gran Sasso underground laboratory. These measurements were used to determine the crystals' intrinsic α-activities which were compared to those of crystals produced at other institutes. The total α-activities of TUM-grown crystals as low as 1.23±0.06 mBq/kg were found to be significantly smaller than the activities of crystals grown at other institutes typically ranging between ∼ 15 mBq/kg and ∼ 35 mBq/kg.

46 INSTRUMENTATION RELATED TO NUCLEAR SCIENCE AND ↗
DOE OSTI2014

Exploring the atomic structure and conformational flexibility of a 320 Å long engineered viral fiber using X-ray crystallography

This study presents the crystal structure of a ∼320 Å long protein fiber generated by in-frame extension of its repeated helical coiled-coil core. Protein fibers are widespread in nature, but only a limited number of high-resolution structures have been determined experimentally. Unlike globular proteins, fibers are usually recalcitrant to form three-dimensional crystals, preventing single-crystal X-ray diffraction analysis. In the absence of three-dimensional crystals, X-ray fiber diffraction is a powerful tool to determine the internal symmetry of a fiber, but it rarely yields atomic resolution structural information on complex protein fibers. An 85-residue-long minimal coiled-coil repeat unit (MiCRU) was previously identified in the trimeric helical core of tail needle gp26, a fibrous protein emanating from the tail apparatus of the bacteriophage P22 virion. Here, evidence is provided that an MiCRU can be inserted in frame inside the gp26 helical core to generate a rationally extended fiber (gp26-2M) which, like gp26, retains a trimeric quaternary structure in solution. The 2.7 Å resolution crystal structure of this engineered fiber, which measures ∼320 Å in length and is only 20–35 Å wide, was determined. This structure, the longest for a trimeric protein fiber to be determined to such a high resolution, reveals the architecture of 22 consecutive trimerization heptads and provides a framework to decipher the structural determinants for protein fiber assembly, stability and flexibility.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗
DOE OSTI2014

Towards accurate structural characterization of metal centres in protein crystals: the structures of Ni and Cu T{sub 6} bovine insulin derivatives

The level of structural detail around the metal sites in Ni{sup 2+} and Cu{sup 2+} T{sub 6} insulin derivatives was significantly improved by using a combination of single-crystal X-ray crystallography and X-ray absorption spectroscopy. Photoreduction and subsequent radiation damage of the Cu{sup 2+} sites in Cu insulin was followed by XANES spectroscopy. Using synchrotron radiation (SR), the crystal structures of T{sub 6} bovine insulin complexed with Ni{sup 2+} and Cu{sup 2+} were solved to 1.50 and 1.45 Å resolution, respectively. The level of detail around the metal centres in these structures was highly limited, and the coordination of water in Cu site II of the copper insulin derivative was deteriorated as a consequence of radiation damage. To provide more detail, X-ray absorption spectroscopy (XAS) was used to improve the information level about metal coordination in each derivative. The nickel derivative contains hexacoordinated Ni{sup 2+} with trigonal symmetry, whereas the copper derivative contains tetragonally distorted hexacoordinated Cu{sup 2+} as a result of the Jahn–Teller effect, with a significantly longer coordination distance for one of the three water molecules in the coordination sphere. That the copper centre is of type II was further confirmed by electron paramagnetic resonance (EPR). The coordination distances were refined from EXAFS with standard deviations within 0.01 Å. The insulin derivative containing Cu{sup 2+} is sensitive towards photoreduction when exposed to SR. During the reduction of Cu{sup 2+} to Cu{sup +}, the coordination geometry of copper changes towards lower coordination numbers. Primary damage, i.e. photoreduction, was followed directly by XANES as a function of radiation dose, while secondary damage in the form of structural changes around the Cu atoms after exposure to different radiation doses was studied by crystallography using a laboratory diffractometer. Protection against photoreduction and subsequent radiation damage was carried out by solid embedment of Cu insulin in a saccharose matrix. At 100 K the photoreduction was suppressed by ∼15%, and it was suppressed by a further ∼30% on cooling the samples to 20 K.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗
DOE OSTI2015

Capture and X-ray diffraction studies of protein microcrystals in a microfluidic trap array

A microfluidic platform has been developed for the capture and X-ray analysis of protein microcrystals, affording a means to improve the efficiency of XFEL and synchrotron experiments. X-ray free-electron lasers (XFELs) promise to enable the collection of interpretable diffraction data from samples that are refractory to data collection at synchrotron sources. At present, however, more efficient sample-delivery methods that minimize the consumption of microcrystalline material are needed to allow the application of XFEL sources to a wide range of challenging structural targets of biological importance. Here, a microfluidic chip is presented in which microcrystals can be captured at fixed, addressable points in a trap array from a small volume (<10 µl) of a pre-existing slurry grown off-chip. The device can be mounted on a standard goniostat for conducting diffraction experiments at room temperature without the need for flash-cooling. Proof-of-principle tests with a model system (hen egg-white lysozyme) demonstrated the high efficiency of the microfluidic approach for crystal harvesting, permitting the collection of sufficient data from only 265 single-crystal still images to permit determination and refinement of the structure of the protein. This work shows that microfluidic capture devices can be readily used to facilitate data collection from protein microcrystals grown in traditional laboratory formats, enabling analysis when cryopreservation is problematic or when only small numbers of crystals are available. Such microfluidic capture devices may also be useful for data collection at synchrotron sources.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗
DOE OSTI2015

Practical macromolecular cryocrystallography

Current methods, reagents and experimental hardware for successfully and reproducibly flash-cooling macromolecular crystals to cryogenic temperatures for X-ray diffraction data collection are reviewed. Cryocrystallography is an indispensable technique that is routinely used for single-crystal X-ray diffraction data collection at temperatures near 100 K, where radiation damage is mitigated. Modern procedures and tools to cryoprotect and rapidly cool macromolecular crystals with a significant solvent fraction to below the glass-transition phase of water are reviewed. Reagents and methods to help prevent the stresses that damage crystals when flash-cooling are described. A method of using isopentane to assess whether cryogenic temperatures have been preserved when dismounting screened crystals is also presented.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗
DOE OSTI2016

LCP crystallization and X-ray diffraction analysis of VcmN, a MATE transporter from Vibrio cholerae

A V. cholerae MATE transporter was crystallized using the lipidic cubic phase (LCP) method. X-ray diffraction data sets were collected from single crystals obtained in a sandwich plate and a sitting-drop plate to resolutions of 2.5 and 2.2 Å, respectively. Multidrug and toxic compound extrusion (MATE) transporters, one of the multidrug exporter families, efflux xenobiotics towards the extracellular side of the membrane. Since MATE transporters expressed in bacterial pathogens contribute to multidrug resistance, they are important therapeutic targets. Here, a MATE-transporter homologue from Vibrio cholerae, VcmN, was overexpressed in Escherichia coli, purified and crystallized in lipidic cubic phase (LCP). X-ray diffraction data were collected to 2.5 Å resolution from a single crystal obtained in a sandwich plate. The crystal belonged to space group P2{sub 1}2{sub 1}2{sub 1}, with unit-cell parameters a = 52.3, b = 93.7, c = 100.2 Å. As a result of further LCP crystallization trials, crystals of larger size were obtained using sitting-drop plates. X-ray diffraction data were collected to 2.2 Å resolution from a single crystal obtained in a sitting-drop plate. The crystal belonged to space group P2{sub 1}2{sub 1}2{sub 1}, with unit-cell parameters a = 61.9, b = 91.8, c = 100.9 Å. The present work provides valuable insights into the atomic resolution structure determination of membrane transporters.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗
DOE OSTI2014

A new theory for X-ray diffraction

By considering the scattering distributed throughout space, there is an intensity enhancement at the Bragg angle even when the Bragg condition is not satisfied. This leads to an alternative explanation for the diffraction from powders and small crystals. This article proposes a new theory of X-ray scattering that has particular relevance to powder diffraction. The underlying concept of this theory is that the scattering from a crystal or crystallite is distributed throughout space: this leads to the effect that enhanced scatter can be observed at the ‘Bragg position’ even if the ‘Bragg condition’ is not satisfied. The scatter from a single crystal or crystallite, in any fixed orientation, has the fascinating property of contributing simultaneously to many ‘Bragg positions’. It also explains why diffraction peaks are obtained from samples with very few crystallites, which cannot be explained with the conventional theory. The intensity ratios for an Si powder sample are predicted with greater accuracy and the temperature factors are more realistic. Another consequence is that this new theory predicts a reliability in the intensity measurements which agrees much more closely with experimental observations compared to conventional theory that is based on ‘Bragg-type’ scatter. The role of dynamical effects (extinction etc.) is discussed and how they are suppressed with diffuse scattering. An alternative explanation for the Lorentz factor is presented that is more general and based on the capture volume in diffraction space. This theory, when applied to the scattering from powders, will evaluate the full scattering profile, including peak widths and the ‘background’. The theory should provide an increased understanding of the reliability of powder diffraction measurements, and may also have wider implications for the analysis of powder diffraction data, by increasing the accuracy of intensities predicted from structural models.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗
DOE OSTI2015

Analysis of rapidly synthesized guest-filled porous complexes with synchrotron radiation: practical guidelines for the crystalline sponge method

This report describes complete practical guidelines and insights for the crystalline sponge method, which have been derived through the first use of synchrotron radiation on these systems, and includes a procedure for faster synthesis of the sponges. These guidelines will be applicable to crystal sponge data collected at synchrotrons or in-house facilities, and will allow researchers to obtain reliable high-quality data and construct chemically and physically sensible models for guest structural determination. A detailed set of synthetic and crystallographic guidelines for the crystalline sponge method based upon the analysis of expediently synthesized crystal sponges using third-generation synchrotron radiation are reported. The procedure for the synthesis of the zinc-based metal–organic framework used in initial crystal sponge reports has been modified to yield competent crystals in 3 days instead of 2 weeks. These crystal sponges were tested on some small molecules, with two being unexpectedly difficult cases for analysis with in-house diffractometers in regard to data quality and proper space-group determination. These issues were easily resolved by the use of synchrotron radiation using data-collection times of less than an hour. One of these guests induced a single-crystal-to-single-crystal transformation to create a larger unit cell with over 500 non-H atoms in the asymmetric unit. This led to a non-trivial refinement scenario that afforded the best Flack x absolute stereochemical determination parameter to date for these systems. The structures did not require the use of PLATON/SQUEEZE or other solvent-masking programs, and are the highest-quality crystalline sponge systems reported to date where the results are strongly supported by the data. A set of guidelines for the entire crystallographic process were developed through these studies. In particular, the refinement guidelines include strategies to refine the host framework, locate guests and determine occupancies, discussion of the proper use of geometric and anisotropic displacement parameter restraints and constraints, and whether to perform solvent squeezing/masking. The single-crystal-to-single-crystal transformation process for the crystal sponges is also discussed. The presented general guidelines will be invaluable for researchers interested in using the crystalline sponge method at in-house diffraction or synchrotron facilities, will facilitate the collection and analysis of reliable high-quality data, and will allow construction of chemically and physically sensible models for guest structural determination.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗
DOE OSTI2015

SHELXT – Integrated space-group and crystal-structure determination

SHELXT automates routine small-molecule structure determination starting from single-crystal reflection data, the Laue group and a reasonable guess as to which elements might be present. The new computer program SHELXT employs a novel dual-space algorithm to solve the phase problem for single-crystal reflection data expanded to the space group P1. Missing data are taken into account and the resolution extended if necessary. All space groups in the specified Laue group are tested to find which are consistent with the P1 phases. After applying the resulting origin shifts and space-group symmetry, the solutions are subject to further dual-space recycling followed by a peak search and summation of the electron density around each peak. Elements are assigned to give the best fit to the integrated peak densities and if necessary additional elements are considered. An isotropic refinement is followed for non-centrosymmetric space groups by the calculation of a Flack parameter and, if appropriate, inversion of the structure. The structure is assembled to maximize its connectivity and centred optimally in the unit cell. SHELXT has already solved many thousand structures with a high success rate, and is optimized for multiprocessor computers. It is, however, unsuitable for severely disordered and twinned structures because it is based on the assumption that the structure consists of atoms.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗
DOE OSTI2014

Influence of seed layers on the vertical growth of ZnO nanowires by low-temperature wet chemical bath deposition on ITO-coated glass substrate

Aligned ZnO nanowires (NWs) were synthesized by low-temperature wet chemical bath deposition (CBD) technique on indium tin oxide (ITO)-coated glass substrates using c-axis orientated ZnO and AZO (Al-doped ZnO) seed layers through the RF sputtering deposition process under different conditions. The growth direction of ZnO NW was controlled by using the two different seed layers. Results showed single-crystalline structure of the ZnO NWs with the highest peak intensity in (002) crystalline direction. In addition, NWs seeding form AZO layer, grown on ITO coated glass, were vertically aligned and uniformly distributed on the substrate. The effects of precursor concentration, growth temperature, and seed layer on NW morphology were investigated in two different seed layers systematically. The intensity of broad emissions at 500–600 nm emission was observed in room temperature photoluminescence (PL) spectra for samples prepared under optimized parameters. In addition, the green emission intensity of ZnO NWs growth on the ZnO seed layer was much weaker than that of AZO seed layer. The experimental results indicate that the selection of seed layers, precursor concentration, and the growth temperature are key parameters to vertical growth of NWs for the application of nanoscale devices.

77 NANOSCIENCE AND NANOTECHNOLOGY↗
DOE OSTI2013

Physical properties of epitaxial ZrN/MgO(001) layers grown by reactive magnetron sputtering

Single-crystal ZrN films, 830 nm thick, are grown on MgO(001) at 450 °C by magnetically unbalanced reactive magnetron sputtering. The combination of high-resolution x-ray diffraction reciprocal lattice maps, high-resolution cross-sectional transmission electron microscopy, and selected-area electron diffraction shows that ZrN grows epitaxially on MgO(001) with a cube-on-cube orientational relationship, (001){sub ZrN}‖(001){sub MgO} and [100]{sub ZrN}‖[100]{sub MgO}. The layers are essentially fully relaxed with a lattice parameter of 0.4575 nm, in good agreement with reported results for bulk ZrN crystals. X-ray reflectivity results reveal that the films are completely dense with smooth surfaces (roughness = 1.3 nm, consistent with atomic-force microscopy analyses). Based on temperature-dependent electronic transport measurements, epitaxial ZrN/MgO(001) layers have a room-temperature resistivity ρ{sub 300K} of 12.0 μΩ-cm, a temperature coefficient of resistivity between 100 and 300 K of 5.6 × 10{sup −8}Ω-cm K{sup −1}, a residual resistivity ρ{sub o} below 30 K of 0.78 μΩ-cm (corresponding to a residual resistivity ratio ρ{sub 300Κ}/ρ{sub 15K} = 15), and the layers exhibit a superconducting transition temperature of 10.4 K. The relatively high residual resistivity ratio, combined with long in-plane and out-of-plane x-ray coherence lengths, ξ{sub ‖} = 18 nm and ξ{sub ⊥} = 161 nm, indicates high crystalline quality with low mosaicity. The reflectance of ZrN(001), as determined by variable-angle spectroscopic ellipsometry, decreases slowly from 95% at 1 eV to 90% at 2 eV with a reflectance edge at 3.04 eV. Interband transitions dominate the dielectric response above 2 eV. The ZrN(001) nanoindentation hardness and modulus are 22.7 ± 1.7 and 450 ± 25 GPa.

36 MATERIALS SCIENCE↗