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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 19 records
All sourcesNASA NTRSDOE OSTI
DOE OSTI2011

Characterization of Large Grain Nb Ingot Microstructure Using OIM and Laue Methods

Large grain niobium is being examined for fabricating superconducting radiofrequency cavities as an alternative to using rolled sheet with fine grains. It is desirable to know the grain orientations of a niobium ingot slice before fabrication, as this allows heterogeneous strain and surface roughness effects arising from etching to be anticipated. Characterization of grain orientations has been done using orientation imaging microscopy (OIM), which requires destructive extraction of pieces from an ingot slice. Use of a Laue camera allows nondestructive characterization of grain orientations, a process useful for evaluating slices and deformation during the manufacturing process. Five ingot slices from CBMM, Ningxia, and Heraeus are compared. One set of slices was deformed into a half cell and the deformation processes that cause crystal rotations have been investigated and compared with analytical predictions. The five ingot slices are compared in terms of their grain orientations and grain boundary misorientations, indicating no obvious commonalities, which suggests that grain orientations develop randomly during solidification.

36 MATERIALS SCIENCE↗
DOE OSTI2011

Characterization of Large Grain Nb Ingot Microstructure Using EBSP Mapping and Laue Camera Methods

Large grain/single crystal Nb is currently being examined for fabricating superconducting radiofrequency (SRF) cavities as an alternative to using rolled sheet. Three ingot slices from different suppliers have been characterized and are compared. It is desirable to know the grain orientations of an ingot slice before fabrication. Characterization of an ingot slice has been done using electron backscattered pattern (EBSP) orientation imaging microscopy (OIM), which requires cutting out pieces from the slice, a destructive technique. Use of a Laue camera allows nondestructive characterization of grain orientations. The OIM method was used to examine ingot slices from CBMM and Ningxia, while the Laue method was used to examine a Heraeus ingot slice. The three ingot slices are compared in terms of their crystal orientations and grain boundary misorientations, indicating no obvious commonalities. The Laue method has practical advantages over OIM for evaluating ingot slices during the manufacturing process.

36 MATERIALS SCIENCE↗
DOE OSTI2010

LauePt, a graphical-user-interface program for simulating and analyzing white-beam x-ray diffraction Laue patterns.

LauePt is a robust and extremely easy-to-use Windows application for accurately simulating, indexing and analyzing white-beam X-ray diffraction Laue patterns of any crystals under arbitrary diffraction geometry. This program has a user-friendly graphic interface and can be conveniently used by nonspecialists with little X-ray diffraction or crystallography knowledge. Its wide range of applications include (1) determination of single-crystal orientation with the Laue method, (2) white-beam topography, (3) white-beam microdiffraction, (4) X-ray studies of twinning, domains and heterostructures, (5) verification or determination of crystal structures from white-beam diffraction, and (6) teaching of X-ray crystallography.

36 MATERIALS SCIENCE↗
DOE OSTI2018

Correct interpretation of diffraction properties of quartz crystals for X-ray optics applications

Quartz has hundreds of strong Bragg reflections that may offer a great number of choices for making fixed-angle X-ray analyzers and polarizers at virtually any hard X-ray energies with selectable resolution. However, quartz crystals, unlike silicon and germanium, are chiral and may thus appear in two different forms of handedness that are mirror images. Furthermore, because of the threefold rotational symmetry along the c axis, the { h 1 h 2 h 3 L } and { h 2 h 1 h 3 L } Bragg reflections may have quite different Darwin bandwidth, reflectivity and angular acceptance, although they have the same Bragg angle. The design of X-ray optics from quartz crystals therefore requires unambiguous determination of the orientation, handedness and polarity of the crystals. The Laue method and single-axis diffraction technique can provide such information, but the variety of conventions used in the literature to describe quartz structures has caused widespread confusion. The current studies give detailed guidelines for design and fabrication of quartz X-ray optics, with special emphasis on the correct interpretation of Laue patterns in terms of the crystallography and diffraction properties of quartz. Furthermore, the quartz crystals examined were confirmed by X-ray topography to have acceptably low densities of dislocations and other defects, which is the foundation for developing high-resolution quartz-based X-ray optics.

36 MATERIALS SCIENCE↗
DOE OSTI2015

Restricted Photochemistry in the Molecular Solid State: Structural Changes on Photoexcitation of Cu(I) Phenanthroline Metal-to-Ligand Charge Transfer (MLCT) Complexes by Time-Resolved Diffraction

The excited-state structure of Cu{sup I}[(1,10-phenanthroline-N,N') bis(triphenylphosphine)] cations in their crystalline [BF{sub 4}] salt has been determined at both 180 and 90 K by single-pulse time-resolved synchrotron experiments with the modified polychromatic Laue method. The two independent molecules in the crystal show distortions on MLCT excitation that differ in magnitude and direction, a difference attributed to a pronounced difference in the molecular environment of the two complexes. As the excited states differ, the decay of the emission is biexponential with two strongly different lifetimes, the longer lifetime, assigned to the more restricted molecule, becoming more prevalent as the temperature increases. Standard deviations in the current Laue study are very much lower than those achieved in a previous monochromatic study of a Cu(I) 2,9-dimethylphenanthroline substituted complex (J. Am. Chem. Soc. 2009, 131, 6566), but the magnitudes of the shifts on excitation are similar, indicating that lattice restrictions dominate over the steric effect of the methyl substitution. Above all, the study illustrates emphatically that molecules in solids have physical properties different from those of isolated molecules and that their properties depend on the specific molecular environment. This conclusion is relevant for the understanding of the properties of molecular solid-state devices, which are increasingly used in current technology.

Makal, Anna↗
NASA NTRS2008

Synchrotron X-Ray Diffraction Studies of Olivine from Comet Wild 2

We have analyzed a collection of the Comet Wild 2 coma grains returned by the NASA Stardust Mission, using micro-area Laue diffraction equipment. The purpose of the diffraction experiment is to permit the structure refinement of olivine including site occupancies. In addition to the intrinsic importance of the olivine structures for revealing the thermal history of Wild 2 materials, we wish to test reports that olivine recovered after hypervelocity capture in silica aerogel has undergone a basic structural change due to capture heating [1]. The diffraction equipment placed at beam line BL- 4B1 of PF, KEK was developed with a micropinhole and an imaging plate (Fuji Co. Ltd.) using the Laue method combined with polychromatic X-ray of synchrotron radiation operated at energy of 2.5 GeV. The incident beam is limited to 1.6 m in diameter by a micropinhole set just upstream of the sample [2, 3]. It is essential to apply a microbeam to obtain diffracted intensities with high signal to noise ratios. This equipment has been successfully applied to various extraterrestrial materials, including meteorites and interplanetary dust particles [4]. The Laue pattern of the sample C2067,1,111,4 (Fig. 1) was successfully taken on an imaging plate after a 120 minute exposure (Fig. 2).

Source record↗
DOE OSTI2020

An automated platform for in situ serial crystallography at room temperature

Direct observation of functional motions in protein structures is highly desirable for understanding how these nanomachineries of life operate at the molecular level. Because cryogenic temperatures are non-physiological and may prohibit or even alter protein structural dynamics, it is necessary to develop robust X-ray diffraction methods that enable routine data collection at room temperature. We recently reported a crystal-on-crystal device to facilitate in situ diffraction of protein crystals at room temperature devoid of any sample manipulation. Here an automated serial crystallography platform based on this crystal-on-crystal technology is presented. A hardware and software prototype has been implemented, and protocols have been established that allow users to image, recognize and rank hundreds to thousands of protein crystals grown on a chip in optical scanning mode prior to serial introduction of these crystals to an X-ray beam in a programmable and high-throughput manner. This platform has been tested extensively using fragile protein crystals. We demonstrate that with affordable sample consumption, this in situ serial crystallography technology could give rise to room-temperature protein structures of higher resolution and superior map quality for those protein crystals that encounter difficulties during freezing. This serial data collection platform is compatible with both monochromatic oscillation and Laue methods for X-ray diffraction and presents a widely applicable approach for static and dynamic crystallographic studies at room temperature.

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

Zone compensated multilayer laue lens and apparatus and method of fabricating the same

A multilayer Laue Lens includes a compensation layer formed in between a first multilayer section and a second multilayer section. Each of the first and second multilayer sections includes a plurality of alternating layers made of a pair of different materials. Also, the thickness of layers of the first multilayer section is monotonically increased so that a layer adjacent the substrate has a minimum thickness, and the thickness of layers of the second multilayer section is monotonically decreased so that a layer adjacent the compensation layer has a maximum thickness. In particular, the compensation layer of the multilayer Laue lens has an in-plane thickness gradient laterally offset by 90.degree. as compared to other layers in the first and second multilayer sections, thereby eliminating the strict requirement of the placement error.

42 ENGINEERING↗
DOE OSTI2012

Laue crystal structure of Shewanella oneidensis cytochrome c nitrite reductase from a high-yield expression system

The high-yield expression and purification of Shewanella oneidensis cytochrome c nitrite reductase (ccNiR) and its characterization by a variety of methods, notably Laue crystallography, are reported. A key component of the expression system is an artificial ccNiR gene in which the N-terminal signal peptide from the highly expressed S. oneidensis protein 'small tetraheme c' replaces the wild-type signal peptide. This gene, inserted into the plasmid pHSG298 and expressed in S. oneidensis TSP-1 strain, generated approximately 20 mg crude ccNiR per liter of culture, compared with 0.5-1 mg/L for untransformed cells. Purified ccNiR has nitrite and hydroxylamine reductase activities comparable to those previously reported for Escherichia coli ccNiR, and is stable for over 2 weeks in pH 7 solution at 4 C. UV/vis spectropotentiometric titrations and protein film voltammetry identified five independent one-electron reduction processes. Global analysis of the spectropotentiometric data also allowed determination of the extinction coefficient spectra for the five reduced ccNiR species. The characteristics of the individual extinction coefficient spectra suggest that, within each reduced species, the electrons are distributed among the various hemes, rather than being localized on specific heme centers. The purified ccNiR yielded good-quality crystals, with which the 2.59-{angstrom}-resolution structure was solved at room temperature using the Laue diffraction method. The structure is similar to that of E. coli ccNiR, except in the region where the enzyme interacts with its physiological electron donor (CymA in the case of S. oneidensis ccNiR, NrfB in the case of the E. coli protein).

59 BASIC BIOLOGICAL SCIENCES↗
DOE OSTI2018

Abnormal grain growth induced by grain boundary segregation of yttrium in grain-oriented Fe-3%Si steel

Highlights: • The abnormal grain growth in Fe-3%Si was induced without precipitates by alloying of yttrium. • Grains grew abnormally to sizes exceeding 10 mm after secondary recrystallization. • Observations by the Laue diffraction method confirmed that the abnormally grown grains had the Goss orientation. The possibility of abnormal grain growth in grain-oriented Fe-3%Si steel by grain boundary segregation was investigated. Yttrium was selected to inhibit normal grain growth because its segregation at grain boundaries would efficiently reduce the grain boundary energy of iron, decreasing the driving force for grain growth. After secondary recrystallization, abnormal grain growth was successfully achieved without any precipitates. Observations by the Laue diffraction method confirmed that the abnormally grown grains had the Goss orientation.

36 MATERIALS SCIENCE↗
DOE OSTI2015

The LaueUtil toolkit for Laue photocrystallography. I. Rapid orientation matrix determination for intermediate-size-unit-cell Laue data

A new method for determination of the orientation matrix of Laue X-ray data is presented. The method is based on matching of the experimental patterns of central reciprocal lattice rows projected on a unit sphere centered on the origin of the reciprocal lattice with the corresponding pattern of a monochromatic data set on the same material. This technique is applied to the complete data set and thus eliminates problems often encountered when single frames with a limited number of peaks are to be used for orientation matrix determination. Application of the method to a series of Laue data sets on organometallic crystals is described. The corresponding program is available under a Mozilla Public License-like open-source license.

Kalinowski, Jaroslaw A.↗
DOE OSTI2024

High Magnetic Anisotropy and Magnetocaloric Effects in Single-Crystal Cr 2 Te 3

Here, we report a systematic investigation of anisotropic magnetocaloric effects in single-crystal Cr 2 Te 3 . Single-crystal samples are synthesized by chemical vapor transport and characterized by X-ray and Laue diffraction methods. The maximum magnetic entropy change –ΔS M max is 4.50 J kg –1 K –1 for the easy c-axis (3.36 J kg –1 K –1 for the hard axis along ab-plane), and the relative cooling power (RCP) is 296.7 J kg –1 for the easy c-axis (183.84 J kg –1 for the hard axis along ab-plane) for a magnetic field change of 9 T near the Curie temperature. The magneto-crystalline anisotropy constant K u is estimated to be 580.12 kJ m –3 at 140 K, decreasing to 148.60 kJ m –3 at 168 K. Meanwhile, the maximum of the rotational magnetic entropy change –ΔS M R (T, H) between the c-axis and the ab-plane is about 1.14 J kg –1 K –1 for magnetic-field change of 9 T. The critical exponents are estimated by analyzing magnetocaloric effects, which indicate a 2D-Ising type magnetic system. The accuracy of estimated critical exponents is verified by scaling analysis. The maximum magnetic entropy change –ΔS M max ≈ 5.25 J kg –1 K –1 (along the c-axis) and the corresponding adiabatic temperature change ΔT ad ≈ 3.31 K (along the c-axis) are estimated by analyzing heat capacity measurements with a magnetic field up to 9 T.

36 MATERIALS SCIENCE↗
DOE OSTI2012

Quantitative measurement of hard x-ray spectra for high intensity laser produced plasma

X-ray line spectra ranging from 17 to 77 keV were quantitatively measured with a Laue spectrometer, composed of a cylindrically curved crystal and a detector. Either a visible CCD detector coupled with a CsI phosphor screen or an imaging plate can be chosen, depending on the signal intensities and exposure times. The absolute sensitivity of the spectrometer system was calibrated using pre-characterized laser-produced x-ray sources and radioisotopes. The integrated reflectivity for the crystal is in good agreement with predictions by an open code for x-ray diffraction. The energy transfer efficiency from incident laser beams to hot electrons, as the energy transfer agency for specific x-ray line emissions, is derived as a consequence of this work.

46 INSTRUMENTATION RELATED TO NUCLEAR SCIENCE AND ↗
DOE OSTI2016

One dimensional focusing with high numerical aperture multilayer Laue lens

Multilayer Laue lenses (MLLs) capitalize on the developments in multilayer deposition technologies for fabricating reflective coatings, specifically undertaken for EUV lithography, where layer thicknesses of several nanometers can be achieved. MLLs are deposited layer by layer, with their thicknesses following the zone plate law, and then pieces are sliced and extracted for use in focusing. Rays are reflected in the Laue geometry. The efficiency of a MLL can be very high, and is maximized by making the slice equal to about a half Pendellosung period so that most energy is transferred from the undiffracted to the diffracted beam, and by ensuring that the Bragg condition is met at each point in the zone plate. This latter condition requires that the layers are tilted to the beam by an amount that varies with layer position; e.g. for focusing a collimated beam, the layers should be normal to a cylinder of radius of twice the focal length. We have fabricated such tilted-zone MLLs and find that they exhibit improved efficiency across their entire pupil as compared with parallel-zone MLLs. This leads to a higher effective NA of the optic and hence higher resolution.

71 CLASSICAL AND QUANTUM MECHANICS, GENERAL PHYSIC↗
DOE OSTI2016

In-vacuum multi-modal monochromator for synchrotron-based hard x-ray micro-imaging

The original monochromator design we present consists in a high-vacuum vessel comprising three monochromators mounted side-by-side: a Lauë/Lauë, a Bragg/Bragg, and a double-multilayer monochromator. The selection of one monochromator type is done remotely by sliding laterally the crystal support in the monochromator vessel. In this way, exotic combinations such as Lauë/Bragg are also possible. Installation and commissioning of the new monochromator at ESRF beamline ID19 was carried out 2013-2014 (the multilayers not being installed yet). Beamline ID19 offers not only superb beam characteristics for phase-contrast imaging with a high level of sensitivity but also compared to other synchrotron X-ray imaging facilities a large beam of currently up to 7 cm × 1.3 cm. A wide energy range can be accessed in a fixed-exit mode (depending on the optics chosen the accessible energy range is between 10 keV and 200 keV). A beryllium exit window (10 cm × 10 cm active opening) completes the monochromator assembly.

46 INSTRUMENTATION RELATED TO NUCLEAR SCIENCE AND ↗
DOE OSTI2013

Curved focusing crystals for hard X-ray astronomy

A lens made by a properly arranged array of crystals can be used to focus x-rays of energy ranging from 30 to 500 keV for x-ray astronomy. Mosaic or curved crystals can be employed as x-ray optical elements. In this work self standing curved focusing Si and GaAs crystals in which the lattice bending is induced by a controlled damaging process on one side of planar crystals are characterized. Diffraction profiles in Laue geometry have been measured in crystals at x-ray energies E = 17, 59 and 120 keV. An enhancement of diffraction efficiency is found in asymmetric geometries.

36 MATERIALS SCIENCE↗
DOE OSTI2012

Coherent X-ray radiation generated by a relativistic electron in an artificial periodic structure

A theory of coherent X-ray radiation from a relativistic electron crossing an artificial periodic layered structure in the Laue scattering geometry is constructed. The expressions describing the spectral-angular radiation parameters are obtained. It is shown that the radiation yield in such a medium may substantially exceed the radiation yield in a crystal under analogous conditions.

73 NUCLEAR PHYSICS AND RADIATION PHYSICS↗