High-pressure studies with x-rays using diamond anvil cells

NASA Astrophysics Data System (ADS)

Shen, Guoyin; Mao, Ho Kwang

2017-01-01

Pressure profoundly alters all states of matter. The symbiotic development of ultrahigh-pressure diamond anvil cells, to compress samples to sustainable multi-megabar pressures; and synchrotron x-ray techniques, to probe materials’ properties in situ, has enabled the exploration of rich high-pressure (HP) science. In this article, we first introduce the essential concept of diamond anvil cell technology, together with recent developments and its integration with other extreme environments. We then provide an overview of the latest developments in HP synchrotron techniques, their applications, and current problems, followed by a discussion of HP scientific studies using x-rays in the key multidisciplinary fields. These HP studies include: HP x-ray emission spectroscopy, which provides information on the filled electronic states of HP samples; HP x-ray Raman spectroscopy, which probes the HP chemical bonding changes of light elements; HP electronic inelastic x-ray scattering spectroscopy, which accesses high energy electronic phenomena, including electronic band structure, Fermi surface, excitons, plasmons, and their dispersions; HP resonant inelastic x-ray scattering spectroscopy, which probes shallow core excitations, multiplet structures, and spin-resolved electronic structure; HP nuclear resonant x-ray spectroscopy, which provides phonon densities of state and time-resolved Mössbauer information; HP x-ray imaging, which provides information on hierarchical structures, dynamic processes, and internal strains; HP x-ray diffraction, which determines the fundamental structures and densities of single-crystal, polycrystalline, nanocrystalline, and non-crystalline materials; and HP radial x-ray diffraction, which yields deviatoric, elastic and rheological information. Integrating these tools with hydrostatic or uniaxial pressure media, laser and resistive heating, and cryogenic cooling, has enabled investigations of the structural, vibrational, electronic, and magnetic properties of materials over a wide range of pressure-temperature conditions.

Publications - GMC 338 | Alaska Division of Geological & Geophysical

Science.gov Websites

capillary pressure data, X-ray diffraction data, sample photographs, petrographic thin-section photographs '-13221.35'); which includes permeability and porosity data, mercury injection capillary pressure data, X-ray

Hydrothermal formation of tobermorite studied by in situ X-ray diffraction under autoclave condition.

PubMed

Kikuma, Jun; Tsunashima, Masamichi; Ishikawa, Tetsuji; Matsuno, Shin-ya; Ogawa, Akihiro; Matsui, Kunio; Sato, Masugu

2009-09-01

Hydrothermal formation of tobermorite from a pre-cured cake has been investigated by transmission X-ray diffraction (XRD) using high-energy X-rays from a synchrotron radiation source in combination with a newly designed autoclave cell. The autoclave cell has a large and thin beryllium window for wide-angle X-ray diffraction; nevertheless, it withstands a steam pressure of more than 1.2 MPa, which enables in situ XRD measurements in a temperature range of 373 to 463 K under a saturated steam pressure. Formation and/or decomposition of several components has been successfully observed during 7.5 h of reaction time. From the intensity changes of the intermediate materials, namely non-crystalline C-S-H and hydroxylellestadite, two pathways for tobermorite formation have been confirmed. Thus, the newly developed autoclave cell can be used for the analyses of reaction mechanisms under specific atmospheres and temperatures.

In-situ x-ray diffraction of a shock-induced phase transition in fluorite, CaF2

NASA Astrophysics Data System (ADS)

Glam, Benny; June Tracy, Sally; Turneaure, Stefan; Duffy, Thomas

2017-06-01

The difluorides are an important class of ionic compounds that show extensive polymorphism under both static and dynamic loading. In this study, the shock-induced phase transitions in CaF2 were investigated by in situ x-ray diffraction measurements in plate impact experiments carried out with the two-stage gas gun at the Dynamic Compression Sector of Argonne National Laboratory. Single-crystal samples in (100) and (111) orientations were shock loaded to pressures between 32 GPa to 70 GPa. The particle velocities at the interface between the sample and a LiF window were measured by VISAR and PDV. Synchrotron x-ray diffraction data were recorded at 153.4 ns intervals using a four-frame detector. The measured diffraction patterns show a high degree of sample texturing at all pressures. We observe evidence for a transition to a high-pressure phase followed by reverse transformation at late times during release. This study provides the first direct constraints on the high-pressure lattice structure of fluorite under shock compression.

Characterization of calcium crystals in Abelia using x-ray diffraction and electron microscopes

USDA-ARS?s Scientific Manuscript database

Localization, chemical composition, and morphology of calcium crystals in leaves and stems of Abelia mosanensis and A. ×grandiflora were analyzed with a variable pressure scanning electron microscope (VP-SEM) equipped with an X-ray diffraction system, low temperature SEM (LT-SEM) and a transmission ...

Multiple film plane diagnostic for shocked lattice measurements (invited)

NASA Astrophysics Data System (ADS)

Kalantar, Daniel H.; Bringa, E.; Caturla, M.; Colvin, J.; Lorenz, K. T.; Kumar, M.; Stölken, J.; Allen, A. M.; Rosolankova, K.; Wark, J. S.; Meyers, M. A.; Schneider, M.; Boehly, T. R.

2003-03-01

Laser-based shock experiments have been conducted in thin Si and Cu crystals at pressures above the Hugoniot elastic limit. In these experiments, static film and x-ray streak cameras recorded x rays diffracted from lattice planes both parallel and perpendicular to the shock direction. These data showed uniaxial compression of Si(100) along the shock direction and three-dimensional compression of Cu(100). In the case of the Si diffraction, there was a multiple wave structure observed, which may be due to a one-dimensional phase transition or a time variation in the shock pressure. A new film-based detector has been developed for these in situ dynamic diffraction experiments. This large-angle detector consists of three film cassettes that are positioned to record x rays diffracted from a shocked crystal anywhere within a full π steradian. It records x rays that are diffracted from multiple lattice planes both parallel and at oblique angles with respect to the shock direction. It is a time-integrating measurement, but time-resolved data may be recorded using a short duration laser pulse to create the diffraction source x rays. This new instrument has been fielded at the OMEGA and Janus lasers to study single-crystal materials shock compressed by direct laser irradiation. In these experiments, a multiple wave structure was observed on many different lattice planes in Si. These data provide information on the structure under compression.

In-situ high-pressure x-ray diffraction study of zinc ferrite nanoparticles

DOE PAGES

Ferrari, S.; Kumar, R. S.; Grinblat, F.; ...

2016-04-23

We have studied the high-pressure structural behavior of zinc ferrite (ZnFe 2O 4) nanoparticles by powder X-ray diffraction measurements up to 47 GPa. We found that the cubic spinel structure of ZnFe 2O 4 remains up to 33 GPa and a phase transition is induced beyond this pressure. The high-pressure phase is indexed to an orthorhombic CaMn 2O 4-type structure. Upon decompression the low- and high-pressure phases coexist. The compressibility of both structures was also investigated. We have observed that the lattice parameters of the high-pressure phase behave anisotropically upon compression. Further, we predict possible phase transition around 55 GPa.more » For comparison, we also studied the compression behavior of magnetite (Fe 3O 4) nanoparticles by X-ray diffraction up to 23 GPa. Spinel-type ZnFe 2O 4 and Fe 3O 4 nanoparticles have a bulk modulus of 172 (20) GPa and 152 (9) GPa, respectively. Lastly, this indicates that in both cases the nanoparticles do not undergo a Hall-Petch strengthening.« less

In-situ high-pressure x-ray diffraction study of zinc ferrite nanoparticles

DOE Office of Scientific and Technical Information (OSTI.GOV)

Ferrari, S.; Kumar, R. S.; Grinblat, F.

We have studied the high-pressure structural behavior of zinc ferrite (ZnFe 2O 4) nanoparticles by powder X-ray diffraction measurements up to 47 GPa. We found that the cubic spinel structure of ZnFe 2O 4 remains up to 33 GPa and a phase transition is induced beyond this pressure. The high-pressure phase is indexed to an orthorhombic CaMn 2O 4-type structure. Upon decompression the low- and high-pressure phases coexist. The compressibility of both structures was also investigated. We have observed that the lattice parameters of the high-pressure phase behave anisotropically upon compression. Further, we predict possible phase transition around 55 GPa.more » For comparison, we also studied the compression behavior of magnetite (Fe 3O 4) nanoparticles by X-ray diffraction up to 23 GPa. Spinel-type ZnFe 2O 4 and Fe 3O 4 nanoparticles have a bulk modulus of 172 (20) GPa and 152 (9) GPa, respectively. Lastly, this indicates that in both cases the nanoparticles do not undergo a Hall-Petch strengthening.« less

X-ray diffraction on radioactive materials

DOE Office of Scientific and Technical Information (OSTI.GOV)

Schiferl, D.; Roof, R.B.

1978-01-01

X-ray diffraction studies on radioactive materials are discussed with the aim of providing a guide to new researchers in the field. Considerable emphasis is placed on the safe handling and loading of not-too-exotic samples. Special considerations such as the problems of film blackening by the gamma rays and changes induced by the self-irradiation of the sample are covered. Some modifications of common diffraction techniques are presented. Finally, diffraction studies on radioactive samples under extreme conditions are discussed, with primary emphasis on high-pressure studies involving diamond-anvil cells.

X-ray investigations related to the shock history of the Shergotty achondrite

NASA Technical Reports Server (NTRS)

Horz, F.; Hanss, R.; Serna, C.

1986-01-01

The shock stress suffered by naturally shocked materials from the Shergotty achondrite was studied using X-ray diffraction techniques and experimentally shocked augite and enstatite as standards. The Shergotty pyroxenes revealed the formation of continuous diffraction rings, line broadening, preferred orientation of small scale diffraction domains, and other evidence of substantial lattice disorders. As disclosed by the application of Debye-Scherrer techniques, they are hybrids between single crystals and fine-grained random powders. The pyroxene lattice is very resistant to shock damage on smaller scales. While measurable lattice disaggregation and progressive fragmentation occur below 25 GPa, little additional damage is suffered from application of pressures between 30 to 60 GPa, making pressure calibration of naturally shocked pyroxenes via X-ray methods difficult. Powder diffractometer scans on pure maskelynite fractions of Shergotty revealed small amounts of still coherently diffracting plagioclase, which may contribute to the high refractive indices of the diaplectic feldspar glasses of Shergotty.

Valence fluctuating compound α-YbAlB4 studied by 174Yb Mössbauer spectroscopy and X-ray diffraction using synchrotron radiation

NASA Astrophysics Data System (ADS)

Oura, Momoko; Ikeda, Shugo; Masuda, Ryo; Kobayashi, Yasuhiro; Seto, Makoto; Yoda, Yoshitaka; Hirao, Naohisa; Kawaguchi, Saori I.; Ohishi, Yasuo; Suzuki, Shintaro; Kuga, Kentaro; Nakatsuji, Satoru; Kobayashi, Hisao

2018-05-01

The structural properties and the Yb 4 f electronic state of the valence fluctuating α-YbAlB4 have been investigated by powder X-ray diffraction under pressure and 174Yb Mössbauer spectroscopy with magnetic fields at low temperature, respectively, using synchrotron radiation. Powder X-ray diffraction patterns showed that the crystal structure does not change up to p ∼ 18 GPa at 8 K and the volume decreases smoothly. However, the pressure dependence of the difference in the structure factor between the (060) and (061) diffraction lines changes at ∼ 3.4 GPa, indicating the change of atomic coordination parameters. The 174Yb Mössbauer spectroscopy measurements at 2 K with 10 and 50 kOe suggest that the electrical quadrupole interaction changes by applied magnetic fields.

High pressure and high temperature in situ X-ray diffraction studies in the Paris-Edinburgh cell using a laboratory X-ray source†

NASA Astrophysics Data System (ADS)

Toulemonde, Pierre; Goujon, Céline; Laversenne, Laetitia; Bordet, Pierre; Bruyère, Rémy; Legendre, Murielle; Leynaud, Olivier; Prat, Alain; Mezouar, Mohamed

2014-04-01

We have developed a new laboratory experimental set-up to study in situ the pressure-temperature phase diagram of a given pure element or compound, its associated phase transitions, or the chemical reactions involved at high pressure and high temperature (HP-HT) between different solids and liquids. This new tool allows laboratory studies before conducting further detailed experiments using more brilliant synchrotron X-ray sources or before kinetic studies. This device uses the diffraction of X-rays produced by a quasi-monochromatic micro-beam source operating at the silver radiation (λ(Ag)Kα 1, 2≈0.56 Å). The experimental set-up is based on a VX Paris-Edinburgh cell equipped with tungsten carbide or sintered diamond anvils and uses standard B-epoxy 5 or 7 mm gaskets. The diffracted signal coming from the compressed (and heated) sample is collected on an image plate. The pressure and temperature calibrations were performed by diffraction, using conventional calibrants (BN, NaCl and MgO) for determination of the pressure, and by crossing isochores of BN, NaCl, Cu or Au for the determination of the temperature. The first examples of studies performed with this new laboratory set-up are presented in the article: determination of the melting point of germanium and magnesium under HP-HT, synthesis of MgB2 or C-diamond and partial study of the P, T phase diagram of MgH2.

High-pressure x-ray diffraction study on lithium borohydride using a synchrotron radiation

NASA Astrophysics Data System (ADS)

Nakano, S.; Nakayama, A.; Kikegawa, T.

2008-07-01

Lithium borohydride (LiBH4) was compressed up to 10 GPa using a diamond-anvil-cell to investigate its high-pressure structure. In-situ x-ray diffraction profiles indicated a pressure-induced transformation at 1.1 GPa, which was consistent with the previous experimental observation such as Raman scattering spectroscopy. The high-pressure phase was indexed on a tetragonal symmetry of P42/mmc, which was not corresponding some structural models proposed by previous calculation studies. An unknown substance (presumably another Li-B-H compound), which was contained in the starting material, also transformed into its high-pressure phase at 0.6 GPa without any relation to the transformation of LiBH4.

Dolomite-II: A new high pressure polymorph of CaMg(CO3)2

NASA Astrophysics Data System (ADS)

Santillan, J.; Williams, Q.; Knittle, E.

2002-12-01

We have measured the infrared spectra and x-ray diffraction of CaMg(CO3)2-dolomite to pressures of 50 GPa at 300 K. We observe both splittings and disappearances of x-ray diffraction peaks between 15 and 20 GPa, as well as new bands in the infrared spectrum of dolomite. The onset of the changes in both the x-ray and infrared data appears to be gradual, and thus kinetically impeded: this is consistent with previous shock results. The infrared and x-ray data are consistent with dolomite adopting a calcite-III-like structure. The net volume change associated with the transition based on a calcite-III monoclinic unit cell is ~4 percent. We calculate that the high pressure phase of dolomite has a volume virtually indistinguishable from that of magnesite plus aragonite. Similarly, an assemblage of the high pressure phase of dolomite and magnesium silicate perovskite has an essentially volume to a magnesite plus calcium silicate perovskite assemblage. Our results thus indicate that high-pressure polymorphism in dolomite could stabilize CaMg(CO3)2 in the deep mantle, and thus that high-pressure polymorphs of dolomite could represent the main reservoir for carbon storage within Earth's lower mantle.

In situ Raman and synchrotron X-ray diffraction study on crystallization of Choline chloride/Urea deep eutectic solvent under high pressure

NASA Astrophysics Data System (ADS)

Yuan, Chaosheng; Chu, Kunkun; Li, Haining; Su, Lei; Yang, Kun; Wang, Yongqiang; Li, Xiaodong

2016-09-01

Pressure-induced crystallization of Choline chloride/Urea (ChCl/Urea) deep eutectic solvent (DES) has been investigated by in-situ Raman spectroscopy and synchrotron X-ray diffraction. The results indicated that high pressure crystals appeared at around 2.6 GPa, and the crystalline structure was different from that formed at ambient pressure. Upon increasing the pressure, the Nsbnd H stretching modes of Urea underwent dramatic change after liquid-solid transition. It appears that high pressures may enhance the hydrogen bonds formed between ChCl and Urea. P versus T phase diagram of ChCl/Urea DES was constructed, and the crystallization mechanism of ChCl/Urea DES was discussed in view of hydrogen bonds.

High pressure cosmochemistry of major planetary interiors: Laboratory studies of the water-rich region of the system ammonia-water

NASA Technical Reports Server (NTRS)

Nicol, Malcolm; Johnson, Mary; Boone, Steven; Cynn, Hyunchee

1987-01-01

Several studies relative to high pressure cosmochemistry of major planetary interiors are summarized. The behavior of gas-ice mixtures at very high pressures, studies of the phase diagram of (NH3) sub x (H2O) sub 1-x at pressures to 5GPa and temperatures from 240 to 370 K, single crystal growth of ammonia dihydrate at room temperature in order to determine their structures by x-ray diffraction, spectroscopy of chemical reactions during shock compression in order to evaluate how the reactions affect the interpretation of equation of state data obtained by shock methods, and temperature and x-ray diffraction measurements made on resistively heated wire in diamond anvil cells in order to obtain phase and structural data relevant to the interiors of terrestrial planets are among the studies discussed.

Infrastructure development for radioactive materials at the NSLS-II

DOE Office of Scientific and Technical Information (OSTI.GOV)

Sprouster, D. J.; Weidner, R.; Ghose, S. K.

2018-02-01

The X-ray Powder Diffraction (XPD) Beamline at the National Synchrotron Light Source-II is a multipurpose instrument designed for high-resolution, high-energy X-ray scattering techniques. In this article, the capabilities, opportunities and recent developments in the characterization of radioactive materials at XPD are described. The overarching goal of this work is to provide researchers access to advanced synchrotron techniques suited to the structural characterization of materials for advanced nuclear energy systems. XPD is a new beamline providing high photon flux for X-ray Diffraction, Pair Distribution Function analysis and Small Angle X-ray Scattering. The infrastructure and software described here extend the existing capabilitiesmore » at XPD to accommodate radioactive materials. Such techniques will contribute crucial information to the characterization and quantification of advanced materials for nuclear energy applications. We describe the automated radioactive sample collection capabilities and recent X-ray Diffraction and Small Angle X-ray Scattering results from neutron irradiated reactor pressure vessel steels and oxide dispersion strengthened steels.« less

Infrastructure development for radioactive materials at the NSLS-II

DOE PAGES

Sprouster, David J.; Weidner, R.; Ghose, S. K.; ...

2017-11-04

The X-ray Powder Diffraction (XPD) Beamline at the National Synchrotron Light Source-II is a multipurpose instrument designed for high-resolution, high-energy X-ray scattering techniques. In this paper, the capabilities, opportunities and recent developments in the characterization of radioactive materials at XPD are described. The overarching goal of this work is to provide researchers access to advanced synchrotron techniques suited to the structural characterization of materials for advanced nuclear energy systems. XPD is a new beamline providing high photon flux for X-ray Diffraction, Pair Distribution Function analysis and Small Angle X-ray Scattering. The infrastructure and software described here extend the existing capabilitiesmore » at XPD to accommodate radioactive materials. Such techniques will contribute crucial information to the characterization and quantification of advanced materials for nuclear energy applications. Finally, we describe the automated radioactive sample collection capabilities and recent X-ray Diffraction and Small Angle X-ray Scattering results from neutron irradiated reactor pressure vessel steels and oxide dispersion strengthened steels.« less

High Pressure X-Ray Diffraction Studies of Bi2-xSbxTe3 (x = 0,1,2)

NASA Astrophysics Data System (ADS)

Jacobsen, M. K.; Kumar, R. S.; Cornelius, A. L.; Sinogeiken, S. V.; Nico, M. F.

2007-12-01

Recently, pressure tuning of the thermoelectric figure of merit has been reported for several materials Bi2Te3 based thermoelectric materials [2],[10],[12]. In order to investigate the bulk properties of Bi2Te3, Sb2Te3, and their solid solution in detail, we have performed structural studies up to 20 GPa. Our diffraction results show that all three compounds transform from the ambient pressure structure to a high pressure phase between 7 and 10 GPa. In addition, these diffraction results have been converted to Vinet and Holzapfel equations of state to test the claim of electronic topological transitions in these structures [3].

High pressure single-crystal micro X-ray diffraction analysis with GSE_ADA/RSV software

NASA Astrophysics Data System (ADS)

Dera, Przemyslaw; Zhuravlev, Kirill; Prakapenka, Vitali; Rivers, Mark L.; Finkelstein, Gregory J.; Grubor-Urosevic, Ognjen; Tschauner, Oliver; Clark, Simon M.; Downs, Robert T.

2013-08-01

GSE_ADA/RSV is a free software package for custom analysis of single-crystal micro X-ray diffraction (SCμXRD) data, developed with particular emphasis on data from samples enclosed in diamond anvil cells and subject to high pressure conditions. The package has been in extensive use at the high pressure beamlines of Advanced Photon Source (APS), Argonne National Laboratory and Advanced Light Source (ALS), Lawrence Berkeley National Laboratory. The software is optimized for processing of wide-rotation images and includes a variety of peak intensity corrections and peak filtering features, which are custom-designed to make processing of high pressure SCμXRD easier and more reliable.

New results of the post-spinel transition pressure in Mg2SiO4 by means of in-situ X-ray diffraction in a multi-anvil press: complete agreement with the 660-km discontinuity depth

NASA Astrophysics Data System (ADS)

Ishii, T.; Huang, R.; Fei, H.; Koemets, I.; Liu, Z.; Maeda, F.; Yuan, L.; Wang, L.; Druzhbin, D.; Yamamoto, T.; Bhat, S.; Farla, R. J.; Kawazoe, T.; Tsujino, N.; Kulik, E.; Higo, Y.; Tange, Y.; Katsura, T.

2017-12-01

It has been accepted that the 660-km discontinuity (D660) is caused by the post-spinel (Psp) transition, which is decomposition of ringwoodite (Rw) to bridgmanite (Brg) + ferropericlase. Nevertheless, all of in-situ X-ray diffraction studies with multi-anvil presses (MAP) gave distinctively lower transition pressures than that of the D660 (23.4 GPa). Although Fei et al. (2004) claimed that their Psp transition pressure explains the D660, it is still 0.5 GPa lower by considering the geotherm. If these results were accepted, the Psp would not account for the D660. In this study, we re-investigated the Psp transition pressure in Mg2SiO4 by in-situ X-ray diffraction using a MAP. A fine-grained mixture of forsterite, enstatite and periclase (Pc) and an MgO pressure marker were placed at the center of a furnace. The sample was compressed to 6-7 MN and heated to 1100 K to synthesize a mixture of Rw, akimotoite and Pc. After that, more press load was applied to obtain sample pressures of ca. 23 GPa, and the sample was then heated to 1700 K, keeping this temperature for 1-2 hours. During keeping the temperature, the press load was first rapidly, and then gradually increased to prevent pressure drop. Phase identification and pressure determination were conducted with alternatively accumulated diffraction patterns of the sample and pressure maker. We bracketed the transition pressures by 23.7 and 24.0 GPa at 1700 K based on the third-order Birch-Murnaghan and Vinet EOSs of MgO given by Tange et al. (2009), respectively. The transition pressure at 2000 K is estimated to be 23.2-23.5 GPa by applying the Psp transition slope based on Fei et al. (2004). Thus, the present transition pressure completely agrees with the D660 depth. The reason for the lower transition pressures by the previous studies is pressure drop during heating. Although the transition completes at the beginning of target temperature, pressure significantly drops during or even before accumulating a diffraction pattern for 3-5 minutes. We obtained the correct transition pressure by preventing the pressure drop by pumping. This problem should be omnipresent in high P-T in-situ X-ray diffraction experiments to determine a phase boundary.

Use of a miniature diamond-anvil cell in high-pressure single-crystal neutron Laue diffraction

PubMed Central

Binns, Jack; Kamenev, Konstantin V.; McIntyre, Garry J.; Moggach, Stephen A.; Parsons, Simon

2016-01-01

The first high-pressure neutron diffraction study in a miniature diamond-anvil cell of a single crystal of size typical for X-ray diffraction is reported. This is made possible by modern Laue diffraction using a large solid-angle image-plate detector. An unexpected finding is that even reflections whose diffracted beams pass through the cell body are reliably observed, albeit with some attenuation. The cell body does limit the range of usable incident angles, but the crystallographic completeness for a high-symmetry unit cell is only slightly less than for a data collection without the cell. Data collections for two sizes of hexamine single crystals, with and without the pressure cell, and at 300 and 150 K, show that sample size and temperature are the most important factors that influence data quality. Despite the smaller crystal size and dominant parasitic scattering from the diamond-anvil cell, the data collected allow a full anisotropic refinement of hexamine with bond lengths and angles that agree with literature data within experimental error. This technique is shown to be suitable for low-symmetry crystals, and in these cases the transmission of diffracted beams through the cell body results in much higher completeness values than are possible with X-rays. The way is now open for joint X-ray and neutron studies on the same sample under identical conditions. PMID:27158503

Structural properties of barium stannate

NASA Astrophysics Data System (ADS)

Phelan, D.; Han, F.; Lopez-Bezanilla, A.; Krogstad, M. J.; Gim, Y.; Rong, Y.; Zhang, Junjie; Parshall, D.; Zheng, H.; Cooper, S. L.; Feygenson, M.; Yang, Wenge; Chen, Yu-Sheng

2018-06-01

BaSnO3 has attracted attention as a transparent conducting oxide with high room temperature carrier mobility. We report a series of measurements that were carried out to assess the structure of BaSnO3 over a variety of length scales. Measurements included single crystal neutron and x-ray diffraction, Rietveld and pair distribution analysis of neutron powder diffraction, Raman scattering, and high-pressure x-ray diffraction. Results from the various diffraction probes indicate that both the long-range and local structures are consistent with the cubic symmetry. The diffraction data under pressure was consistent with a robustly cubic phase up to 48.9 GPa, which is supported by density functional calculations. Additionally, transverse phonon velocities were determined from measured dispersion of the transverse acoustic phonon branches, the results of which are in good agreement with previous theoretical estimates and ultrasound measurements.

The behavior of single-crystal silicon to dynamic loading using in-situ X-ray diffraction and phase contrast imaging

NASA Astrophysics Data System (ADS)

Lee, Hae Ja; Xing, Zhou; Galtier, Eric; Arnold, Brice; Granados, Eduardo; Brown, Shaughnessy B.; Tavella, Franz; McBride, Emma; Fry, Alan; Nagler, Bob; Schropp, Andreas; Seiboth, Frank; Samberg, Dirk; Schroer, Christian; Gleason, Arianna E.; Higginbotham, Andrew

Hydrostatic and uniaxial compression studies have revealed that crystalline silicon undergoes phase transitions from a cubic diamond structure to a variety of phases including orthorhombic Imma phase, body-centered tetragonal phase, and a hexagonal primitive phase. The dynamic response of silicon at high pressure, however, is not well understood. Phase contrast imaging has proven to be a powerful tool for probing density changes caused by the shock propagation into a material. In order to characterize the elastic and phase transitions, we image shock waves in Si with high spatial resolution using the LCLS X-ray free electron laser and Matter in Extreme Conditions instrument. In this study, the long pulse optical laser with pseudo-flat top shape creates high pressures up to 60 GPa. We measure the crystal structure by observing X-ray diffraction orthogonal to the shock propagation direction over a range of pressures. We describe the capability of simultaneously performing phase contrast imaging and in situ X-ray diffraction during shock loading and discuss the dynamic response of Si in high-pressure phases Use of the Linac Coherent Light Source (LCLS), SLAC National Accelerator Laboratory, is supported by the U.S. Department of Energy, Office of Science, Office of Basic Energy Sciences under Contract No. DE-AC02-76SF00515. The MEC instrument is supported by.

Elastic Wave Velocity Measurements on Mantle Peridotite at High Pressure and Temperature

NASA Astrophysics Data System (ADS)

Mistler, G. W.; Ishikawa, M.; Li, B.

2002-12-01

With the success of conducting ultrasonic measurements at high pressure and high temperature in large volume high pressure apparatus with in-situ measurement of the sample length by X-ray imaging, it is now possible to measure elastic wave velocities on aggregate samples with candidate compositions of the mantle to the conditions of the Earth's transition zone in the laboratory. These data can be directly compared with seismic data to distinguish the compositional models in debate. In this work, we carried out velocity measurements on natural peridotite KLB-1 at the conditions of the Earth's upper mantle. Fine powered sample of natural KLB-1 was used as starting material. Specimens for ultrasonic measurements were hot-pressed and equilibrated at various pressure and temperature conditions along geotherm up to the transition zone. The recovered samples were characterized with density measurement, X-ray diffraction and microprobe analysis. Bench top P and S wave velocities of KLB-1 sample sintered at 3-4 GPa and 1400 degree centigrade showed a very good agreement with the VRH average of pyrolite. High pressure and high temperature measurements was conducted up to 7 GPa and 800 degree centigrade using ultrasonic interferometric method in a DIA-type high pressure apparatus in conjunction with X-ray diffraction and X-ray imaging. The utilization of X-ray imaging technique provides direct measurements of sample lengths at high pressure and high temperature, ensuring a precise determination of velocities. The results of P and S wave velocities at high pressure and high temperature as well as their comparison with calculated pyrolite model will be presented.

DOE Office of Scientific and Technical Information (OSTI.GOV)

Rittman, Dylan R.; Turner, Katlyn M.; Park, Sulgiye

Strain engineering is a promising method for next-generation materials processing techniques. Here, we use mechanical milling and annealing followed by compression in diamond anvil cell to tailor the intrinsic and extrinsic strain in pyrochlore, Dy 2Ti 2O 7 and Dy 2Zr 2O 7. Raman spectroscopy, X-ray pair distribution function analysis, and X-ray diffraction were used to characterize atomic order over short-, medium-, and long-range spatial scales, respectively, under ambient conditions. Raman spectroscopy and X-ray diffraction were further employed to interrogate the material in situ at high pressure. High-pressure behavior is found to depend on the species and concentration of defectsmore » in the sample at ambient conditions. Overall, we show that defects can be engineered to lower the phase transformation onset pressure by ~50% in the ordered pyrochlore Dy 2Ti 2O 7, and lower the phase transformation completion pressure by ~20% in the disordered pyrochlore Dy 2Zr 2O 7. Lastly, these improvements are achieved without significantly sacrificing mechanical integrity, as characterized by bulk modulus.« less

DOE Office of Scientific and Technical Information (OSTI.GOV)

Rittman, Dylan R.; Turner, Katlyn M.; Park, Sulgiye

Strain engineering is a promising method for next-generation materials processing techniques. Here, we use mechanical milling and annealing followed by compression in diamond anvil cell to tailor the intrinsic and extrinsic strain in pyrochlore, Dy 2Ti 2O 7 and Dy 2Zr 2O 7. Raman spectroscopy, X-ray pair distribution function analysis, and X-ray diffraction were used to characterize atomic order over short-, medium-, and long-range spatial scales, respectively, under ambient conditions. Raman spectroscopy and X-ray diffraction were further employed to interrogate the material in situ at high pressure. High-pressure behavior is found to depend on the species and concentration of defectsmore » in the sample at ambient conditions. Overall, we show that defects can be engineered to lower the phase transformation onset pressure by ~50% in the ordered pyrochlore Dy 2Zr 2O 7, and lower the phase transformation completion pressure by ~20% in the disordered pyrochlore Dy 2Zr 2O 7. These improvements are achieved without significantly sacrificing mechanical integrity, as characterized by bulk modulus.« less

Rotator Phases of n-Heptane under High Pressure: Raman Scattering and X-ray Diffraction Studies

DOE Office of Scientific and Technical Information (OSTI.GOV)

C Ma; Q Zhou; F Li

2011-12-31

We performed high-pressure Raman scattering and angle-dispersive synchrotron X-ray diffraction measurements on n-heptane at room temperature. It has been found that n-heptane undergoes a liquid to rotator phase III (R{sub III}) transition at 1.2 GPa and then transforms into another rotator phase R{sub IV} at about 3 GPa. As the pressure reaches 7.5 GPa, a transition from an orientationally disordered R{sub IV} phase to an ordered crystalline state starts and is completed around 14.5 GPa. Our results clearly present the high-pressure phase transition sequence (liquid-R{sub III}-R{sub IV}-crystal) of n-heptane, similar to that of normal alkanes.

The high pressure structure and equation of state of 2,6-diamino-3,5-dinitropyrazine-1-oxide (LLM-105) up to 20 GPa: X-ray diffraction measurements and first principles molecular dynamics simulations

DOE PAGES

Stavou, Elissaios; Manaa, M. Riad; Zaug, Joseph M.; ...

2015-10-14

Recent theoretical studies of 2,6-diamino-3,5-dinitropyrazine-1-oxide (C 4H 4N 6O 5 Lawrence Livermore Molecule No. 105, LLM-105) report unreacted high pressure equations of state that include several structural phase transitions, between 8 and 50 GPa, while one published experimental study reports equation of state (EOS) data up to a pressure of 6 GPa with no observed transition. Here we report the results of a synchrotron-based X-ray diffraction study and also ambient temperature isobaric-isothermal atomistic molecular dynamics simulations of LLM-105 up to 20 GPa. We find that the ambient pressure phase remains stable up to 20 GPa; there is no indication ofmore » a pressure induced phase transition. We do find a prominent decrease in b-axis compressibility starting at approximately 13 GPa and attribute the stiffening to a critical length where inter-sheet distance becomes similar to the intermolecular distance within individual sheets. The ambient temperature isothermal equation of state was determined through refinements of measured X-ray diffraction patterns. The pressure-volume data were fit using various EOS models to yield bulk moduli with corresponding pressure derivatives. As a result, we find very good agreement between the experimental and theoretically derived EOS.« less

Pressure dependence of the monoclinic phase in (1–x)Pb(Mg 1/3Nb 2/3)O 3-xPbTiO₃ solid solutions

DOE PAGES

Ahart, Muhtar; Sinogeikin, Stanislav; Shebanova, Olga; ...

2012-12-26

We combine high-pressure x-ray diffraction, high-pressure Raman scattering, and optical microscopy to investigate a series of (1–x)Pb(Mg 1/3Nb 2/3)O 3-xPbTiO₃ (PMN-xPT) solid solutions (x=0.2, 0.3, 0.33, 0.35, 0.37, 0.4) in diamond anvil cells up to 20 GPa at 300 K. The Raman spectra show a peak centered at 380 cm⁻¹ starting above 6 GPa for all samples, in agreement with previous observations. X-ray diffraction measurements are consistent with this spectral change indicating a structural phase transition; we find that the triplet at the pseudocubic (220) Bragg peak merges into a doublet above 6 GPa. Our results indicate that the morphotropicmore » phase boundary region (x=0.33–0.37) with the presence of monoclinic symmetry persists up to 7 GPa. The pressure dependence of ferroelectric domains in PMN-0.32PT single crystals was observed using a polarizing optical microscope. The domain wall density decreases with pressure and the domains disappear at a modest pressure of 3 GPa. We propose a pressure-composition phase diagram for PMN-xPT solid solutions.« less

Structural Properties of Barium Stannate.

DOE Office of Scientific and Technical Information (OSTI.GOV)

Phelan, D.; Han, F.; Lopez-Bezanilla, A.

2018-06-01

BaSnO3 has attracted attention as a transparent conducting oxide with high room temperature carrier mobility. We report a series of measurements that were carried out to assess the structure of BaSnO3 over a variety of length scales. Measurements included single crystal neutron and x-ray diffraction, Rietveld and pair distribution analysis of neutron powder diffraction, Raman scattering, and high-pressure x-ray diffraction. Results from the various diffraction probes indicate that both the long-range and local structures are consistent with the cubic symmetry. The diffraction data under pressure was consistent with a robustly cubic phase up to 48.9 GPa, which is supported bymore » density functional calculations. Additionally, transverse phonon velocities were determined from measured dispersion of the transverse acoustic phonon branches, the results of which are in good agreement with previous theoretical estimates and ultrasound measurements.« less

X-ray diffraction diagnostic design for the National Ignition Facility

NASA Astrophysics Data System (ADS)

Ahmed, Maryum F.; House, Allen; Smith, R. F.; Ayers, Jay; Lamb, Zachary S.; Swift, David W.

2013-09-01

This paper describes the design considerations for Target Diffraction In-Situ (TARDIS), an x-ray diffraction diagnostic at the National Ignition Facility. A crystal sample is ramp-compressed to peak pressures between 10 and 30 Mbar and, during a pressure hold period, is probed with quasi-monochromatic x-rays emanating from a backlighter source foil. The crystal spectrography diffraction lines are recorded onto image plates. The crystal sample, filter, and image plates are packaged into one assembly, allowing for accurate and repeatable target to image plate registration. Unconverted laser light impinges upon the device, generating debris, the effects of which have been mitigated. Dimpled blast shields, high strength steel alloy, and high-z tungsten are used to shield and protect the image plates. A tapered opening was designed to provide adequate thickness of shielding materials without blocking the drive beams or x-ray source from reaching the crystal target. The high strength steel unit serves as a mount for the crystal target and x-ray source foil. A tungsten body contains the imaging components. Inside this sub-assembly, there are three image plates: a 160 degree field of view curved plate directly opposite the target opening and two flat plates for the top and bottom. A polycarbonate frame, coated with the appropriate filter material and embedded with registration features for image plate location, is inserted into the diagnostic body. The target assembly is metrologized and then the diagnostic assembly is attached.

BX90: A new diamond anvil cell design for X-ray diffraction and optical measurements

NASA Astrophysics Data System (ADS)

Kantor, I.; Prakapenka, V.; Kantor, A.; Dera, P.; Kurnosov, A.; Sinogeikin, S.; Dubrovinskaia, N.; Dubrovinsky, L.

2012-12-01

We present a new design of a universal diamond anvil cell, suitable for different kinds of experimental studies under high pressures. Main features of the cell are an ultimate 90-degrees symmetrical axial opening and high stability, making the presented cell design suitable for a whole range of techniques from optical absorption to single-crystal X-ray diffraction studies, also in combination with external resistive or double-side laser heating. Three examples of the cell applications are provided: a Brillouin scattering of neon, single-crystal X-ray diffraction of α-Cr2O3, and resistivity measurements on the (Mg0.60Fe0.40)(Si0.63Al0.37)O3 silicate perovskite.

An in situ X ray diffraction study of the kinetics of the Ni2SiO4 olivine-spinel transformation

NASA Technical Reports Server (NTRS)

Rubie, D. C.; Tsuchida, Y.; Yagi, T.; Utsumi, W.; Kikegawa, T.

1990-01-01

The kinetics of the olivine-spinel transformation in Ni2SiO4 were investigated in an in situ X-ray diffraction experiments in which synchrotron radiation was used as an X-ray source. The starting material was Ni2SO4 olivine which was hot-pressed in situ at 980 C and 2.5 GPa; during the transformation, X-ray diffraction patterns were collected at intervals of 30 or 120 sec. The kinetic data were analyzed using Cahn's (1956) model. The activation energy for growth at 3.6-3.7 GPa was estimated as 438 + or - 199 kJ/mol. It is shown that, in order to make significant extrapolations of the kinetic data to a geological scale, the dependence of the rates of both nucleation and growth on temperature and pressure must be evaluated separately.

A perforated diamond anvil cell for high-energy x-ray diffraction of liquids and amorphous solids at high pressure.

PubMed

Soignard, Emmanuel; Benmore, Chris J; Yarger, Jeffery L

2010-03-01

Diamond anvil cells (DACs) are widely used for the study of materials at high pressure. The typical diamonds used are between 1 and 3 mm thick, while the sample contained within the opposing diamonds is often just a few microns in thickness. Hence, any absorbance or scattering from diamond can cause a significant background or interference when probing a sample in a DAC. By perforating the diamond to within 50-100 microm of the sample, the amount of diamond and the resulting background or interference can be dramatically reduced. The DAC presented in this article is designed to study amorphous materials at high pressure using high-energy x-ray scattering (>60 keV) using laser-perforated diamonds. A small diameter perforation maintains structural integrity and has allowed us to reach pressures >50 GPa, while dramatically decreasing the intensity of the x-ray diffraction background (primarily Compton scattering) when compared to studies using solid diamonds. This cell design allows us for the first time measurement of x-ray scattering from light (low Z) amorphous materials. Here, we present data for two examples using the described DAC with one and two perforated diamond geometries for the high-pressure structural studies of SiO(2) glass and B(2)O(3) glass.

Equation of state of rhenium and application for ultra high pressure calibration

DOE Office of Scientific and Technical Information (OSTI.GOV)

Anzellini, Simone; Dewaele, Agnès; Occelli, Florent

2014-01-28

The isothermal equation of state of rhenium has been measured by powder X-ray diffraction experiments up to 144 GPa at room temperature in a diamond anvil cell. A helium pressure transmitting medium was used to minimize the non-hydrostatic stress on the sample. The fit of pressure-volume data yields a bulk modulus K{sub 0} = 352.6 GPa and a pressure derivative of the bulk modulus K′{sub 0}=4.56. This equation of state differs significantly from a recent determination [Dubrovinsky et al., Nat. Commun. 3, 1163 (2012)], giving here a lower pressure at a given volume. The possibility of using rhenium gasket X-ray diffraction signal, with themore » present equation of state, to evaluate multi-Mbar pressures in the chamber of diamond anvil cells is discussed.« less

Pressure-induced phase transition in GaN nanocrystals

NASA Astrophysics Data System (ADS)

Cui, Q.; Pan, Y.; Zhang, W.; Wang, X.; Zhang, J.; Cui, T.; Xie, Y.; Liu, J.; Zou, G.

2002-11-01

High-pressure in situ energy-dispersive x-ray diffraction experiments on GaN nanocrystals with 50 nm diameter have been carried out using a synchrotron x-ray source and a diamond-anvil cell up to about 79 GPa at room temperature. A pressure-induced first-order structural phase transition from the wurtzite-type structure to the rock-salt-type structure starts at about 48.8 GPa. The rock-salt-type phase persists to the highest pressure in our experimental range.

Investigation and Characterization of Water-Recrystallized Croconic Acid

DTIC Science & Technology

2016-12-01

high- pressure synthesis. Thermal analysis, bomb calorimetry, X-ray diffraction, and Raman spectroscopy were performed on water- recrystallized...3.2.3 Raman Spectroscopy and X-ray Diffraction 12 3.2.4 Bomb Calorimetry 13 4. Conclusions 15 5. References 16 List of Symbols, Abbreviations, and...and is called the β-phase (the as-received [AR] material is also known as the α-phase). Bomb calorimeter testing of the β-CA indicated a heat of

Structure, Elastic Constants and XRD Spectra of Extended Solids under High Pressure

DOE Office of Scientific and Technical Information (OSTI.GOV)

Batyrev, I. G.; Coleman, S. P.; Ciezak-Jenkins, J. A.

We present results of evolutionary simulations based on density functional calculations of a potentially new type of energetic materials called extended solids: P-N and N-H. High-density structures with covalent bonds generated using variable and fixed concentration methods were analysed in terms of thermo-dynamical stability and agreement with experimental X-ray diffraction (XRD) spectra. X-ray diffraction spectra were calculated using a virtual diffraction algorithm that computes kinematic diffraction intensity in three-dimensional reciprocal space before being reduced to a two-theta line profile. Calculated XRD patterns were used to search for the structure of extended solids present at experimental pressures by optimizing data accordingmore » to experimental XRD peak position, peak intensity and theoretically calculated enthalpy. Elastic constants has been calculated for thermodynamically stable structures of P-N system.« less

Strain engineered pyrochlore at high pressure

DOE PAGES

Rittman, Dylan R.; Turner, Katlyn M.; Park, Sulgiye; ...

2017-05-22

Strain engineering is a promising method for next-generation materials processing techniques. Here, we use mechanical milling and annealing followed by compression in diamond anvil cell to tailor the intrinsic and extrinsic strain in pyrochlore, Dy 2Ti 2O 7 and Dy 2Zr 2O 7. Raman spectroscopy, X-ray pair distribution function analysis, and X-ray diffraction were used to characterize atomic order over short-, medium-, and long-range spatial scales, respectively, under ambient conditions. Raman spectroscopy and X-ray diffraction were further employed to interrogate the material in situ at high pressure. High-pressure behavior is found to depend on the species and concentration of defectsmore » in the sample at ambient conditions. Overall, we show that defects can be engineered to lower the phase transformation onset pressure by ~50% in the ordered pyrochlore Dy 2Ti 2O 7, and lower the phase transformation completion pressure by ~20% in the disordered pyrochlore Dy 2Zr 2O 7. Lastly, these improvements are achieved without significantly sacrificing mechanical integrity, as characterized by bulk modulus.« less

In situ x-ray diffraction observation of multiple texture turnovers in sputtered Cr films

NASA Astrophysics Data System (ADS)

Zhao, Z. B.; Rek, Z. U.; Yalisove, S. M.; Bilello, J. C.

2004-11-01

A series of Cr films were deposited onto native oxides of (100) Si substrates via a confocal deposition geometry in a magnetron sputter chamber. The film growth chamber was incorporated with an in situ x-ray diffraction system, which allowed the collection of x-ray diffraction data on the growing film in a quasi real time fashion without interruption of film deposition. The in situ x-ray diffraction, coupled with other ex situ characterization techniques, was used to study structural evolutions of the Cr films deposited at various Ar pressures. It was observed that the evolution of the crystallographic structures of Cr films was very sensitive to both deposition conditions and film thickness. With the confocal deposition geometry, the Cr films developed various types of out-of-plane textures. In addition to the (110) and (100) types of textures commonly reported for vapor deposited Cr films, the (111) and (112) types of textures were also observed. The film deposited at low Ar pressure (2 mTorr) developed strong (111) type texture. With the increase in either Ar pressure or film thickness, the Cr films tended to develop (112) and (100) types of texture. At high Ar pressures (>10 mTorr), several changes in texture type with increasing film thickness were observed. The sequence can be described as (110)-->(112)-->(100). The strong tendency for these films to ultimately assume the (100) type of texture could be related to significant rises in substrate temperatures during the late stages of film growth with high Ar pressures. The observation of the multiple texture type changes suggests that the evolution of Cr films is controlled by complex growth kinetics. The competitive growth of grains with different orientations can be altered not only by controllable deposition parameters such as Ar pressure, but also by the variations of in situ film attributes (e.g., residual stress and substrate temperature) occurring concurrently with film growth.

Pressure induced structural transitions in CuSbS 2 and CuSbSe 2 thermoelectric compounds

DOE Office of Scientific and Technical Information (OSTI.GOV)

Baker, Jason; Kumar, Ravhi S.; Sneed, Daniel

Here, we investigate the structural behavior of CuSbS 2 and CuSbSe 2 thermoelectric materials under high pressure conditions up to 80 GPa using angle dispersive X-ray diffraction in a diamond anvil cell (DAC). We also perform high pressure Raman spectroscopy measurements up to 16 GPa. We observed a pressure-induced structural transformation from the ambient orthorhombic structure with space group Pnma to a triclinic type structure with space group P1 beginning around 8 GPa in both samples and completing at 13 GPa and 10 GPa in CuSbS 2 and CuSbSe 2, respectively. High pressure Raman experiments complement the transitions observed bymore » high pressure X-ray diffraction (HPXRD). Finally, the transitions were found to be reversible on releasing the pressure to ambient in the DAC. The bulk modulus and compressibility of these materials are further discussed.« less

Pressure induced structural transitions in CuSbS 2 and CuSbSe 2 thermoelectric compounds

DOE PAGES

Baker, Jason; Kumar, Ravhi S.; Sneed, Daniel; ...

2015-04-27

Here, we investigate the structural behavior of CuSbS 2 and CuSbSe 2 thermoelectric materials under high pressure conditions up to 80 GPa using angle dispersive X-ray diffraction in a diamond anvil cell (DAC). We also perform high pressure Raman spectroscopy measurements up to 16 GPa. We observed a pressure-induced structural transformation from the ambient orthorhombic structure with space group Pnma to a triclinic type structure with space group P1 beginning around 8 GPa in both samples and completing at 13 GPa and 10 GPa in CuSbS 2 and CuSbSe 2, respectively. High pressure Raman experiments complement the transitions observed bymore » high pressure X-ray diffraction (HPXRD). Finally, the transitions were found to be reversible on releasing the pressure to ambient in the DAC. The bulk modulus and compressibility of these materials are further discussed.« less

Reactor for nano-focused x-ray diffraction and imaging under catalytic in situ conditions

NASA Astrophysics Data System (ADS)

Richard, M.-I.; Fernández, S.; Hofmann, J. P.; Gao, L.; Chahine, G. A.; Leake, S. J.; Djazouli, H.; De Bortoli, Y.; Petit, L.; Boesecke, P.; Labat, S.; Hensen, E. J. M.; Thomas, O.; Schülli, T.

2017-09-01

A reactor cell for in situ studies of individual catalyst nanoparticles or surfaces by nano-focused (coherent) x-ray diffraction has been developed. Catalytic reactions can be studied in flow mode in a pressure range of 10-2-103 mbar and temperatures up to 900 °C. This instrument bridges the pressure and materials gap at the same time within one experimental setup. It allows us to probe in situ the structure (e.g., shape, size, strain, faceting, composition, and defects) of individual nanoparticles using a nano-focused x-ray beam. Here, the setup was used to observe strain and facet evolution of individual model Pt catalysts during in situ experiments. It can be used for heating other (non-catalytically active) nanoparticles (e.g., nanowires) in inert or reactive gas atmospheres or vacuum as well.

Reactor for nano-focused x-ray diffraction and imaging under catalytic in situ conditions.

PubMed

Richard, M-I; Fernández, S; Hofmann, J P; Gao, L; Chahine, G A; Leake, S J; Djazouli, H; De Bortoli, Y; Petit, L; Boesecke, P; Labat, S; Hensen, E J M; Thomas, O; Schülli, T

2017-09-01

A reactor cell for in situ studies of individual catalyst nanoparticles or surfaces by nano-focused (coherent) x-ray diffraction has been developed. Catalytic reactions can be studied in flow mode in a pressure range of 10 -2 -10 3 mbar and temperatures up to 900 °C. This instrument bridges the pressure and materials gap at the same time within one experimental setup. It allows us to probe in situ the structure (e.g., shape, size, strain, faceting, composition, and defects) of individual nanoparticles using a nano-focused x-ray beam. Here, the setup was used to observe strain and facet evolution of individual model Pt catalysts during in situ experiments. It can be used for heating other (non-catalytically active) nanoparticles (e.g., nanowires) in inert or reactive gas atmospheres or vacuum as well.

Equation of state and pressure induced amorphization of beta-boron from X-ray measurements up to 100 GPa.

PubMed

Sanz, Delia Nieto; Loubeyre, Paul; Mezouar, Mohamed

2002-12-09

The equation of state of boron has been measured up to 100 GPa by single-crystal x-ray diffraction with helium as the pressure transmitting medium. Rhombohedral beta-boron is the stable structure up to 100 GPa under hydrostatic conditions. Nonhydrostatic stress stabilizes a different rhombohedral structure. At about 100 GPa a pressure-induced amorphization is observed. The amorphous phase can be quenched to ambient pressure. An explanation is proposed based on the different stability under pressure between intraicosahedra and intericosahedra bonds.

Phase transformations and equation of state of praseodymium metal to 103 GPa

DOE Office of Scientific and Technical Information (OSTI.GOV)

Chesnut, Gary N.; Vohra, Yogesh K.

2000-08-01

Pressure-induced structural phase transformations in a trivalent rare-earth metal praseodymium (Pr) were studied at room temperature in a diamond anvil cell to 103 GPa by energy dispersive x-ray diffraction using a synchrotron source. Our x-ray diffraction studies document the following crystal structure sequence: dhcp{yields}fcc{yields}distorted fcc(hR24 type){yields}monoclinic(C2/m){yields}{alpha}-uranium with increasing pressure. We measure a 16.7% volume collapse at the transition to the {alpha}-uranium phase at 20 GPa. The high-pressure {alpha}-uranium phase in Pr was found to be stable to the highest pressure of 103 GPa, which corresponds to a volume compression V/V{sub 0}=0.407. (c) 2000 The American Physical Society.

New developments in laser-heated diamond anvil cell with in situ synchrotron x-ray diffraction at High Pressure Collaborative Access Team

DOE Office of Scientific and Technical Information (OSTI.GOV)

Meng, Yue; Hrubiak, Rostislav; Rod, Eric

An overview of the in situ laser heating system at the High Pressure Collaborative Access Team, with emphasis on newly developed capabilities, is presented. Since its establishment at the beamline 16-ID-B a decade ago, laser-heated diamond anvil cell coupled with in situ synchrotron x-ray diffraction has been widely used for studying the structural properties of materials under simultaneous high pressure and high temperature conditions. Recent developments in both continuous-wave and modulated heating techniques have been focusing on resolving technical issues of the most challenging research areas. Furthermore, the new capabilities have demonstrated clear benefits and provide new opportunities in researchmore » areas including high-pressure melting, pressure-temperature-volume equations of state, chemical reaction, and time resolved studies.« less

New developments in laser-heated diamond anvil cell with in situ synchrotron x-ray diffraction at High Pressure Collaborative Access Team

DOE PAGES

Meng, Yue; Hrubiak, Rostislav; Rod, Eric; ...

2015-07-17

An overview of the in situ laser heating system at the High Pressure Collaborative Access Team, with emphasis on newly developed capabilities, is presented. Since its establishment at the beamline 16-ID-B a decade ago, laser-heated diamond anvil cell coupled with in situ synchrotron x-ray diffraction has been widely used for studying the structural properties of materials under simultaneous high pressure and high temperature conditions. Recent developments in both continuous-wave and modulated heating techniques have been focusing on resolving technical issues of the most challenging research areas. Furthermore, the new capabilities have demonstrated clear benefits and provide new opportunities in researchmore » areas including high-pressure melting, pressure-temperature-volume equations of state, chemical reaction, and time resolved studies.« less

New developments in laser-heated diamond anvil cell with in situ synchrotron x-ray diffraction at High Pressure Collaborative Access Team

DOE Office of Scientific and Technical Information (OSTI.GOV)

Meng, Yue; Hrubiak, Rostislav; Rod, Eric

An overview of the in situ laser heating system at the High Pressure Collaborative Access Team, with emphasis on newly developed capabilities, is presented. Since its establishment at the beamline 16-ID-B a decade ago, laser-heated diamond anvil cell coupled with in situ synchrotron x-ray diffraction has been widely used for studying the structural properties of materials under simultaneous high pressure and high temperature conditions. Recent developments in both continuous-wave and modulated heating techniques have been focusing on resolving technical issues of the most challenging research areas. The new capabilities have demonstrated clear benefits and provide new opportunities in research areasmore » including high-pressure melting, pressure-temperature-volume equations of state, chemical reaction, and time resolved studies.« less

In situ Raman and X-ray diffraction studies on the high pressure and temperature stability of methane hydrate up to 55 GPa.

PubMed

Kadobayashi, Hirokazu; Hirai, Hisako; Ohfuji, Hiroaki; Ohtake, Michika; Yamamoto, Yoshitaka

2018-04-28

High-temperature and high-pressure experiments were performed under 2-55 GPa and 298-653 K using in situ Raman spectroscopy and X-ray diffraction combined with externally heated diamond anvil cells to investigate the stability of methane hydrate. Prior to in situ experiments, the typical C-H vibration modes of methane hydrate and their pressure dependence were measured at room temperature using Raman spectroscopy to make a clear discrimination between methane hydrate and solid methane which forms through the decomposition of methane hydrate at high temperature. The sequential in situ Raman spectroscopy and X-ray diffraction revealed that methane hydrate survives up to 633 K and 40.3 GPa and then decomposes into solid methane and ice VII above the conditions. The decomposition curve of methane hydrate estimated by the present experiments is >200 K lower than the melting curves of solid methane and ice VII, and moderately increases with increasing pressure. Our result suggests that although methane hydrate may be an important candidate for major constituents of cool exoplanets and other icy bodies, it is unlikely to be present in the ice mantle of Neptune and Uranus, where the temperature is expected to be far beyond the decomposition temperatures.

In situ Raman and X-ray diffraction studies on the high pressure and temperature stability of methane hydrate up to 55 GPa

NASA Astrophysics Data System (ADS)

Kadobayashi, Hirokazu; Hirai, Hisako; Ohfuji, Hiroaki; Ohtake, Michika; Yamamoto, Yoshitaka

2018-04-01

High-temperature and high-pressure experiments were performed under 2-55 GPa and 298-653 K using in situ Raman spectroscopy and X-ray diffraction combined with externally heated diamond anvil cells to investigate the stability of methane hydrate. Prior to in situ experiments, the typical C-H vibration modes of methane hydrate and their pressure dependence were measured at room temperature using Raman spectroscopy to make a clear discrimination between methane hydrate and solid methane which forms through the decomposition of methane hydrate at high temperature. The sequential in situ Raman spectroscopy and X-ray diffraction revealed that methane hydrate survives up to 633 K and 40.3 GPa and then decomposes into solid methane and ice VII above the conditions. The decomposition curve of methane hydrate estimated by the present experiments is >200 K lower than the melting curves of solid methane and ice VII, and moderately increases with increasing pressure. Our result suggests that although methane hydrate may be an important candidate for major constituents of cool exoplanets and other icy bodies, it is unlikely to be present in the ice mantle of Neptune and Uranus, where the temperature is expected to be far beyond the decomposition temperatures.

High-pressure studies of cycloheptane up to 30 GPa

NASA Astrophysics Data System (ADS)

Ma, Chunli; Cui, Qiliang; Liu, Zhenxian

2013-06-01

High-pressure synchrotron angle dispersive x-ray diffraction, Raman scattering and infrared absorption studies have been performed on cycloheptane (C7H14) up to 30 GPa at room temperature by using diamond anvil cell techniques. The synchrotron x-ray diffraction results indicate that the liquid cyclopentane undergoes two phase transitions at around 0.5 and 1.0 GPa, respectively. Then, it gradually turns into glass state starting from 3.0 GPa. The features of the Raman scattering and infrared absorption show no significant changes with increasing pressure below 3 GPa. This implies that the two phases observed by the x-ray diffraction can be attributed to plastic phases in which the cycloheptane molecules are held in an ordered structure while the molecular orientation is disordered. Up on further compression, all Raman and infrared bands begin broadening around 3.0 GPa that provide further evidence on the transition to glass state. Our results also suggest different paths on phase transitions under isothermal compression at room temperature compare to that previously reported under isobaric cooling at ambient pressure. This work was supported by the NSF of China (91014004, 11004074,11074089), the specialized Research Fund for the Doctoral Program of Higher Education (20110061110011, 20100061120093), and the National Basic Research Program of China (2011CB808200).

Quantitative analysis of crystalline pharmaceuticals in tablets by pattern-fitting procedure using X-ray diffraction pattern.

PubMed

Takehira, Rieko; Momose, Yasunori; Yamamura, Shigeo

2010-10-15

A pattern-fitting procedure using an X-ray diffraction pattern was applied to the quantitative analysis of binary system of crystalline pharmaceuticals in tablets. Orthorhombic crystals of isoniazid (INH) and mannitol (MAN) were used for the analysis. Tablets were prepared under various compression pressures using a direct compression method with various compositions of INH and MAN. Assuming that X-ray diffraction pattern of INH-MAN system consists of diffraction intensities from respective crystals, observed diffraction intensities were fitted to analytic expression based on X-ray diffraction theory and separated into two intensities from INH and MAN crystals by a nonlinear least-squares procedure. After separation, the contents of INH were determined by using the optimized normalization constants for INH and MAN. The correction parameter including all the factors that are beyond experimental control was required for quantitative analysis without calibration curve. The pattern-fitting procedure made it possible to determine crystalline phases in the range of 10-90% (w/w) of the INH contents. Further, certain characteristics of the crystals in the tablets, such as the preferred orientation, size of crystallite, and lattice disorder were determined simultaneously. This method can be adopted to analyze compounds whose crystal structures are known. It is a potentially powerful tool for the quantitative phase analysis and characterization of crystals in tablets and powders using X-ray diffraction patterns. Copyright 2010 Elsevier B.V. All rights reserved.

Experiments with phase transitions at very high pressure

NASA Technical Reports Server (NTRS)

Spain, I. L.

1984-01-01

A diamond anvil cell is described which was developed for studying hydrogen and other materials to pressure above 100 PGa, including measurements at low temperature. The benefits of X-ray diffraction using synchrotron radiation and using a fixed anode source are examined as well as the optimization of X-ray diffraction at low temperature. A Ge diode detector was incorporated into apparatus for measuring optical absorption, reflectance, and fluorescence in order to enable luminescence studies and Raman spectra were obtained. Results of experiments on Si, Ge, GaP, InAs, hydrogen, benzene, nitrogen, graphite, and the superconductor CeCu2Si2 are given.

Strongly coupled electronic, magnetic, and lattice degrees of freedom in LaCo 5 under pressure

DOE PAGES

Stillwell, Ryan L.; Jeffries, Jason R.; McCall, Scott K.; ...

2015-11-25

In this study, we have performed high-pressure magnetotransport and x-ray diffraction measurements on ferromagnetic LaCo 5, confirming the theoretically predicted electronic topological transition driving the magnetoelastic collapse seen in the related compound YCo 5. Our x-ray diffraction results show an anisotropic lattice collapse of the c axis near 10 GPa that is also commensurate with a change in the majority charge carriers evident from high-pressure Hall effect measurements. The coupling of the electronic, magnetic, and lattice degrees of freedom is further substantiated by the evolution of the anomalous Hall effect, which couples to the magnetization of the ordered state ofmore » LaCo 5.« less

Phase transition studies of germanium to 1. 25 Mbar

DOE Office of Scientific and Technical Information (OSTI.GOV)

Vohra, Y.K.; Brister, K.E.; Desgreniers, S.

1986-05-05

New phase transitions in Ge were observed by energy-dispersive x-ray diffraction techniques for pressures up to 125 GPa (1.25 Mbar) as follows: the ..beta..-Sn structure to the simple hexagonal (sh) phase at 75 +- 3 GPa and to the double hexagonal close-packed structure (dhcp) at 102 +- 5 GPa. These are the highest pressures for which a crystalline structure change has been directly observed in any material by x-ray diffraction. Total-energy pseudopotential calculations predict 84 +- 10 GPa for the ..beta..-Sn to sh phase transition and 105 +- 21 GPa for sh to hcp (not dhcp) transition. The role ofmore » 3d core electrons in increasing the transformation pressures in Ge, as compared to Si, is emphasized.« less

Neutron and X-ray investigations of the Jahn–Teller switch in partially deuterated ammonium copper Tutton salt, (NH 4 ) 2 [Cu(H 2 O) 6 ](SO 4 ) 2

DOE Office of Scientific and Technical Information (OSTI.GOV)

Jørgensen, Mads R. V.; Piccoli, Paula M. B.; Hathwar, Venkatesha R.

2017-01-31

The structural phase transition accompanied by a Jahn–Teller switch has been studied over a range of H/D ratios in (NH 4) 2[Cu(H 2O) 6](SO 4) 2(ACTS). In particular, single-crystal neutron diffraction investigations of crystals with deuteration in the range 50 to 82% are shown to be consistent with previous electron paramagnetic resonance (EPR) experiments exhibiting a phase boundary at 50% deuteration under ambient pressure. Polycrystalline samples show that the two phases can co-exist. In addition, single-crystal neutron and polycrystalline X-ray diffraction pressure experiments show a shift to lower pressure at 60% deuterationversusprevious measurements at 100% deuteration.

[Effects of dynamic high-pressure microfluidization on the structure of waxy rice starch].

PubMed

Tu, Zong-Cai; Zhu, Xiu-Mei; Chen, Gang; Wang, Hui; Zhang, Bo; Huang, Xiao-Qin; Li, Zhi

2010-03-01

The effects of dynamic ultra high-pressure microfluidization on the structure of waxy rice starch solutions (6%) were analyzed using SEM, UV-Vis spectra, polarized light microscopy, and X-ray diffraction spectra. The results showed that: SEM graphs demonstrated that the crystal structure of waxy rice starch under different pressure treatment was destroyed with different degrees and impacted into flake up to 160 MPa; from the ultraviolet-visible spectrum we know the reduction in the blue iodine value and the decrease in the amylopectin content, which illustrated that the structure of waxy rice starch was fractured; polarized microscopic images showed that the polarization crosses of starch molecules became misty with the pressure increasing, and most of starch molecules lost polarization cross when the pressure reached 160 MPa; X-ray diffraction spectra indicated that relative crystallinity began to decline at 120 MPa with pressure treatment, and the decreased amplitude was slightly lower.

Combined experimental and computational study of high-pressure behavior of triphenylene

PubMed Central

Zhao, Xiao-Miao; Zhong, Guo-Hua; Zhang, Jiang; Huang, Qiao-Wei; Goncharov, Alexander F.; Lin, Hai-Qing; Chen, Xiao-Jia

2016-01-01

We have performed measurements of Raman scattering, synchrotron x-ray diffraction, and visible transmission spectroscopy combined with density functional theory calculations to study the pressure effect on solid triphenylene. The spectroscopic results demonstrate substantial change of the molecular configuration at 1.4 GPa from the abrupt change of splitting, disappearance, and appearance of some modes. The structure of triphenylene is found be to stable at high pressures without any evidence of structural transition from the x-ray diffraction patterns. The obtained lattice parameters show a good agreement between experiments and calculations. The obtained band gap systematically decreases with increasing pressure. With the application of pressure, the molecular planes become more and more parallel relative to each other. The theoretical calculations indicate that this organic compound becomes metallic at 180 GPa, fueling the hope for the possible realization of superconductivity at high pressure. PMID:27161429

White-beam X-ray diffraction and radiography studies on high-boron-containing borosilicate glass at high pressures

DOE Office of Scientific and Technical Information (OSTI.GOV)

Ham, Kathryn J.; Vohra, Yogesh K.; Kono, Yoshio

Multi-angle energy-dispersive X-ray diffraction studies and white-beam X-ray radiography were conducted with a cylindrically shaped (1 mm diameter and 0.7 mm high) high-boron-content borosilicate glass sample (17.6% B 2O 3) to a pressure of 13.7 GPa using a Paris-Edinburgh (PE) press at Beamline 16-BM-B, HPCAT of the Advanced Photon Source. The measured structure factor S(q) to large q = 19 Å –1 is used to determine information about the internuclear bond distances between various species of atoms within the glass sample. Sample pressure was determined with gold as a pressure standard. The sample height as measured by radiography showed anmore » overall uniaxial compression of 22.5% at 13.7 GPa with 10.6% permanent compaction after decompression to ambient conditions. The reduced pair distribution function G(r) was extracted and Si–O, O–O and Si–Si bond distances were measured as a function of pressure. Lastly, Raman spectroscopy of the pressure recovered sample as compared to starting material showed blue-shift and changes in intensity and widths of Raman bands associated with silicate and four-coordinated boron.« less

White-beam X-ray diffraction and radiography studies on high-boron-containing borosilicate glass at high pressures

DOE PAGES

Ham, Kathryn J.; Vohra, Yogesh K.; Kono, Yoshio; ...

2017-02-06

Multi-angle energy-dispersive X-ray diffraction studies and white-beam X-ray radiography were conducted with a cylindrically shaped (1 mm diameter and 0.7 mm high) high-boron-content borosilicate glass sample (17.6% B 2O 3) to a pressure of 13.7 GPa using a Paris-Edinburgh (PE) press at Beamline 16-BM-B, HPCAT of the Advanced Photon Source. The measured structure factor S(q) to large q = 19 Å –1 is used to determine information about the internuclear bond distances between various species of atoms within the glass sample. Sample pressure was determined with gold as a pressure standard. The sample height as measured by radiography showed anmore » overall uniaxial compression of 22.5% at 13.7 GPa with 10.6% permanent compaction after decompression to ambient conditions. The reduced pair distribution function G(r) was extracted and Si–O, O–O and Si–Si bond distances were measured as a function of pressure. Lastly, Raman spectroscopy of the pressure recovered sample as compared to starting material showed blue-shift and changes in intensity and widths of Raman bands associated with silicate and four-coordinated boron.« less

Shear induced weakening of the hydrogen bonding lattice of the energetic material 5,5'-Hydrazinebistetrazole at high-pressure

DOE Office of Scientific and Technical Information (OSTI.GOV)

Ciezak-Jenkins, Jennifer A.; Jenkins, Timothy A.

5,5'-Hydrazinebistetrazole (HBTA) has been studied by in-situ x-ray diffraction and vibrational spectroscopy to pressures near 25 GPa at room temperature. Analysis of the x-ray diffraction pattern of HBTA collected at ambient pressure and temperature revealed a monoclinic structure consistent with that previously reported. Under compression, the x-ray diffraction reveals little evidence of a phase transition over the pressure range studied. Slight anisotropy in response to compression was noted and the β angle decreased moderately, suggesting geometry modifications occur in the hydrogen bonding lattice and between neighboring HBTA molecules as a result of compression along the c axis. Blue shifts inmore » the Infrared active N-H stretching modes were observed, implying a weakening of the hydrogen bond with compression. The weakening of the hydrogen bonding lattice with pressure may lead to an increase in the bending angle of the C-N=N-C bridge between the tetrazole rings and an increased overlap between the π-bonding orbitals. The Raman spectra showed a number of modes associated with H-N=N-H motions of the bridge become more prominent in the spectra under compression. Additionally, the possibility that the increased bend in the angle of the C-N=N-C bridge results from a shearing deformation is discussed.« less

Effect of exit beam phase aberrations on coherent x-ray reconstructions of Au nanocrystals

NASA Astrophysics Data System (ADS)

Hruszkewycz, Stephan; Harder, Ross; Fuoss, Paul

2010-03-01

Current studies in coherent x-ray diffractive imaging (CXDI) are focusing on in-situ imaging under a variety of environmental conditions. Such studies often involve environmental sample chambers through which the x-ray beam must pass before and after interacting with the sample: i.e. cryostats or high pressure cells. Such sample chambers usually contain polycrystalline x-ray windows with structural imperfections that can in turn interact with the diffracted beam. A phase object in the near field that interacts with the beam exiting the sample can introduce distortions at the detector plane that may affect coherent reconstructions. We investigate the effects of a thin beryllium membrane on the coherent exit beam of a gold nanoparticle. We compare three dimensional reconstructions from experimental diffraction patterns measured with and without a 380 micron thick Be dome and find that the reconstructions are reproducible within experimental errors. Simulated near-field distortions of the exit beam consistent with micron sized voids in Be establish a ``worst case scenario'' where distorted diffraction patterns inhibit accurate inversions.

Structure and stability of hydrous minerals at high pressure

NASA Technical Reports Server (NTRS)

Duffy, T. S.; Fei, Y.; Meade, C.; Hemley, R. J.; Mao, H. K.

1994-01-01

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.

Structural Mineral Physics at Extreme Conditions

NASA Astrophysics Data System (ADS)

Chariton, S.; Dubrovinsky, L. S.; Dubrovinskaia, N.

2017-12-01

Laser heating techniques in diamond anvil cells (DACs) cover a wide pressure-temperature range - above 300 GPa and up to 5000 K. Recent advantages in on-line laser heating techniques resulted in a significant improvement of reliability of in situ X-ray powder diffraction studies in laser-heated DACs, which have become routine at a number of synchrotron facilities including specialized beam-lines at the 3rd generation synchrotrons. However, until recently, existing DAC laser-heating systems could not be used for structural X-ray diffraction studies aimed at structural refinements, i.e. measuring of the diffraction intensities, and not only at determining of lattice parameters. The reason is that in existing DAC laser-heating facilities the laser beam enters the cell at a fixed angle, and a partial rotation of the DAC, as required in monochromatic structural X-ray diffraction experiments, results in a loss of the target crystal and may be even dangerous if the powerful laser light starts to scatter in arbitrary directions by the diamond anvils. In order to overcome this problem we have develop a portable laser heating system and implement it at different diffraction beam lines. We demonstrate the application of this system for simultaneous high-pressure and high-temperature powder and single crystal diffraction studies using examples of studies of chemical and phase relations in the Fe-O system, transition metals carbonates, and silicate perovskites.

X-ray-induced dissociation of H.sub.2O and formation of an O.sub.2-H.sub.2 alloy at high pressure

DOEpatents

Mao, Ho-kwang [Washington, DC; Mao, Wendy L [Washington, DC

2011-11-29

A novel molecular alloy of O.sub.2 and H.sub.2 and a method of producing such a molecular alloy are provided. When subjected to high pressure and extensive x-radiation, H.sub.2O molecules cleaved, forming O--O and H--H bonds. In the method of the present invention, the O and H framework in ice VII was converted into a molecular alloy of O.sub.2 and H.sub.2. X-ray diffraction, x-ray Raman scattering, and optical Raman spectroscopy demonstrate that this crystalline solid differs from previously known phases.

Pressure-induced densification in GeO{sub 2} glass: A transmission x-ray microscopy study

DOE Office of Scientific and Technical Information (OSTI.GOV)

Lin, Yu, E-mail: lyforest@stanford.edu; Zeng, Qiaoshi; Yang, Wenge

2013-12-23

Nanoscale transmission x-ray microscopy measurements have been performed to determine the effect of pressure (P) on the volume (V) change in GeO{sub 2} glass up to 38.5 GPa. The P-V data show a continuous increase upon compression, indicating that the density-driven structural transformation is a gradual process. Over the pressure range studied, a transition is observed at approximately 10–13 GPa, where the material displays distinct compression behaviors. The pressure-induced densification that involves the coordination number change has been discussed. Using this newly developed high-pressure imaging technique with tens of nanometer resolution, we have provided a direct and unequivocal way for measuring densitymore » of amorphous materials to much higher pressures with accuracy rivaling x-ray diffraction of crystalline solids.« less

In Situ Observation of High-Pressure Phase Transitions in SiO2 Under Shock Loading Using Time Resolved X-Ray Diffraction

NASA Astrophysics Data System (ADS)

Tracy, S. J.; Turneaure, S.; Duffy, T. S.

2016-12-01

Quartz is one of the most abundant minerals in Earth's crust and serves as an archetype for silicate minerals generally. The shock metamorphism of silica is important for understanding and interpreting meteorite impact events. Shock compression of quartz is characterized by a phase transition occurring over a broad mixed-phase region ( 10-40 GPa). Despite decades of study, the nature of this transformation and the structure of the high-pressure phase remain poorly understood. In situ x-ray diffraction data on shock-compressed SiO2 was collected at the Dynamic Compression Sector at the Advanced Photon Source. The behavior both single crystal alpha-quartz and fused silica was investigated under dynamic loading through a series real-time synchrotron x-ray diffraction measurements during peak stresses up to 65 GPa. A two-stage light gas gun was used to accelerate LiF flyer plates that impacted the SiO2 samples resulting in a propagating step-like increase in pressure and temperature behind the shock front. Four consecutive x-ray frames, separated by 153 ns, were collected during the transient loading and unloading. These measurements allow for the determination of time-dependent atomic arrangements, demonstrating that both amorphous silica as well as crystalline alpha-quartz transform to stishovite above 36 GPa. These measurements reveal important information about the role of kinetics as well texture development and potential defect structures in the transformed material.

Pressure mapping for sphere and half-sphere enhanced diamond anvil cells using synchrotron x-ray diffraction and fluorescence techniques

NASA Astrophysics Data System (ADS)

Liu, H.; Liu, L. L.; Cai, Z.; Shu, J.

2015-12-01

The measurement for equation of state (EoS) of materials under pressure conditions above 200 GPa is a long-standing challenging subject. Recently, second stage anvil, which was loaded inside the diamond anvil cell (DAC), had been reported by various groups. This method could generate pressure over 300 GPa, or above 600 GPa from the EoS measurement of Re metal between the tiny anvil or 2 half-spheres. Several alternative approaches, using ruby balls, or glassy carbon, or diamond, with single sphere, 2 half-spheres, or multi spheres geometry inside DAC, were tested. The NIST X-ray powder standard, ZnO was selected as pressure marker. Focused ion beam (FIB) was used to cut the half-sphere from diamond anvil top directly to avoid the difficulty of alignment. The synchrotron x-ray diffraction with fine beam size down to 100 nm using zone plate set-up was used to map the pressure gradient at the sphere or half-sphere zone inside DAC. The pressure could be boosted at center of sphere by up to 10 - 70 GPa at about 200 GPa conditions. From broken anvils, trace element analysis using fine focusing synchrotron x-ray fluorescence method revealed the potential anvil damage from FIB cutting the diamond anvil tip, which might decrease the strength of anvils. Fine touch from FIB cutting at final stage using low ion beam current is suggested.

Ultrapressure materials science

NASA Technical Reports Server (NTRS)

Ruoff, A. L.

1984-01-01

Three active areas of research at ultra pressure are pursued, i.e., diffraction studies with the Cornell High Energy Synchrotron Source (CHESS), band gap and absorption edge effects, indentor-anvil experiments and theory and research to attain higher pressures. The range over which X-ray diffraction data and absorption edge data are obtained is extended to 700 kbars. Using the indentor technique pressures of 2.1 Mbars are obtained. Research results and methods are discussed.

Ultrafast X-Ray Diffraction Studies of the Phase Transitions and Equation of State of Scandium Shock Compressed to 82 GPa

DOE PAGES

Briggs, R.; Gorman, M. G.; Coleman, A. L.; ...

2017-01-09

Using x-ray diffraction at the Linac Coherent Light Source x-ray free-electron laser, we have determined simultaneously and self-consistently the phase transitions and equation of state (EOS) of the lightest transition metal, scandium, under shock compression. On compression scandium undergoes a structural phase transition between 32 and 35 GPa to the same bcc structure seen at high temperatures at ambient pressures, and then a further transition at 46 GPa to the incommensurate host-guest polymorph found above 21 GPa in static compression at room temperature. Furthermore, shock melting of the host-guest phase is observed between 53 and 72 GPa with the disappearancemore » of Bragg scattering and the growth of a broad asymmetric diffraction peak from the high-density liquid.« less

Ultrafast X-Ray Diffraction Studies of the Phase Transitions and Equation of State of Scandium Shock Compressed to 82 GPa.

PubMed

Briggs, R; Gorman, M G; Coleman, A L; McWilliams, R S; McBride, E E; McGonegle, D; Wark, J S; Peacock, L; Rothman, S; Macleod, S G; Bolme, C A; Gleason, A E; Collins, G W; Eggert, J H; Fratanduono, D E; Smith, R F; Galtier, E; Granados, E; Lee, H J; Nagler, B; Nam, I; Xing, Z; McMahon, M I

2017-01-13

Using x-ray diffraction at the Linac Coherent Light Source x-ray free-electron laser, we have determined simultaneously and self-consistently the phase transitions and equation of state (EOS) of the lightest transition metal, scandium, under shock compression. On compression scandium undergoes a structural phase transition between 32 and 35 GPa to the same bcc structure seen at high temperatures at ambient pressures, and then a further transition at 46 GPa to the incommensurate host-guest polymorph found above 21 GPa in static compression at room temperature. Shock melting of the host-guest phase is observed between 53 and 72 GPa with the disappearance of Bragg scattering and the growth of a broad asymmetric diffraction peak from the high-density liquid.

Pressure-induced structural transition in chalcopyrite ZnSiP2

NASA Astrophysics Data System (ADS)

Bhadram, Venkata S.; Krishna, Lakshmi; Toberer, Eric S.; Hrubiak, Rostislav; Greenberg, Eran; Prakapenka, Vitali B.; Strobel, Timothy A.

2017-05-01

The pressure-dependent phase behavior of semiconducting chalcopyrite ZnSiP2 was studied up to 30 GPa using in situ X-ray diffraction and Raman spectroscopy in a diamond-anvil cell. A structural phase transition to the rock salt type structure was observed between 27 and 30 GPa, which is accompanied by soft phonon mode behavior and simultaneous loss of Raman signal and optical transmission through the sample. The high-pressure rock salt type phase possesses cationic disorder as evident from broad features in the X-ray diffraction patterns. The behavior of the low-frequency Raman modes during compression establishes a two-stage, order-disorder phase transition mechanism. The phase transition is partially reversible, and the parent chalcopyrite structure coexists with an amorphous phase upon slow decompression to ambient conditions.

Static strength of molybdenum to 92 GPa under radial X-ray diffraction

NASA Astrophysics Data System (ADS)

Xiong, L.; Tu, P.; Li, B.; Wu, S. Y.; Hao, J. B.; Bai, L. G.; Li, X. D.; Liu, J.

2018-06-01

The high-pressure strength of molybdenum (Mo) to 92 GPa has been studied by radial X-ray diffraction (RXRD) technique. The ratio of t/G is found to decrease above ˜24 GPa, showing the yield of Mo which is caused by plastic deformation at this pressure. Combined with high-pressure shear modulus, it was found that the differential stress corresponding to the yield of Mo at 24 GPa due to plastic deformation is 1.73 GPa. The second increase of t values occurs after ˜66 GPa, suggesting the strength of Mo with a differential stress of ˜1.93 GPa. In addition, the maximum difference stress of molybdenum at 87 GPa is 3.01 GPa.

Elasticity and Anelasticity of Materials from Time-Resolved X-ray Diffraction

NASA Astrophysics Data System (ADS)

Sinogeikin, S. V.; Smith, J.; Lin, C.; Bai, L.; Rod, E.; Shen, G.

2014-12-01

Recent advances in synchrotron sources, x-ray optics, area detectors, and sample environment control have enabled many time-resolved experimental techniques for studying materials at extreme pressure and temperature conditions. The High Pressure Collaborative Access Team (HPCAT) at the Advanced Photon Source has made a sustained effort to develop and assemble a powerful collection of high-pressure apparatus for time-resolved research, and considerable time has been invested in developing techniques for collecting high-quality time-resolved x-ray scattering data. In this talk we will outline recently developed capabilities at HPCAT for studying elasticity and anelasticity of minerals using fast compression and cyclic compression-decompression. A few recent studies will be highlighted. For example, with fast x-ray area detectors having millisecond time resolution, accurate thermal equations of state of materials at temperatures up to 1000K and megabar pressures can be collected in a matter of seconds using membrane-driven diamond anvil cells (DAC), yielding unprecedented time and pressure resolution of true isotherms. Short duration of the experiments eliminates temperature variation during the experiments and in general allows volume measurements at higher pressures and temperatures. Alternatively, high-frequency (kilohertz range) radial diffraction measurements in a panoramic DAC combined with fast, precise cyclic loading/unloading by piezo drive could provide the short time scale necessary for studying rheology of minerals from the elastic response and lattice relaxation as a function of pressure, temperature and strain rate. Finally, we consider some possible future applications for time-resolved high-pressure, high-temperature research of mantle minerals.

Integrated in-situ probes for structural and dynamic properties of geological materials at ultrahigh pressures and temperatures

NASA Astrophysics Data System (ADS)

Mao, H.; Mao, W. L.

2005-12-01

Multiple x-ray and allied probes have been recently developed and integrated with diamond-anvil cells at synchrotron facilities. They have effectively opened up the vast field area of the Earth's interior to direct, in-situ study. For instance, x-ray emission spectroscopy identifies the high-spin-low-spin transition that governs Fe-Mg partitioning, the most important factor in element differentiation in the mantle. Inelastic x-ray near-edge spectroscopy reveals the bonding nature of light elements that control the phase transitions, structure and partitioning of these elements (e.g., carbon bonding changes as an element, and in oxides, carbonates, and silicates). X-ray diffraction combined with laser-heated diamond anvil cell determines crystal structures and P-V-T equations of state. Shear moduli, single-crystal elasticity, and phonon dynamics can be measured to the core pressures with newly-enabled, complementary techniques, including radial x-ray diffraction, nuclear resonant inelastic x-ray scattering, non-resonant inelastic x-ray scattering, high-temperature Raman spectroscopy, and Brillouin scattering spectroscopy. The nonhydrostatic stress in solid samples which was previously regarded as a nuisance that degraded the experiments, can now be used for extracting important rheological information, including deformation mechanisms, preferred orientation, slip systems, plasticity, failure, and shear strength of major mantle and core minerals at high pressures. With the new arsenal of experimental techniques over the extended P-T-x regimes at we can now address questions that were not conceivable only a decade ago. Knowledge of the high P-T properties is leading to fundamental improvements in interpreting seismological observations and understanding the structure, dynamics, and evolution of the Earth's deep interior.

Synchrotron Radial X-ray Diffraction Studies of Deformation of Polycrystalline MgO

NASA Astrophysics Data System (ADS)

Girard, J.; Tsujino, N.; Mohiuddin, A.; Karato, S. I.

2016-12-01

X-ray diffraction analyses have been used for decades to study mechanical properties of polycrystalline samples during in-situ high-pressure deformation. When polycrystalline materials are deformed, stresses develop in grains and lead to lattice distortion. Using X-ray diffraction we can estimate the lattice strain for each (hkl) diffraction plans and calculate the applied stress for each (hkl), using [Singh, 1993] relation. However, this method doesn't take into account plastic anisotropy. As a results of plastic anisotropy present in the material, stress estimated from this method can be largely differ depending on (hkl) diffraction planes [Karato, 2009]. Studying the stress estimate for each (hkl) plane, might help us distinguish dominant deformation mechanisms activated during deformation such as diffusion (we will observe small stress variation as a function of (hkl) diffraction planes) or dislocation creep (we will observe a stress variation as a function of (hkl) diffraction planes that could also give us clues on potential slip system activity). In this study we observed stress evolution in MgO polycrystalline samples deformed under mantle pressure and temperature for (200) and (220) diffraction planes. Using a range MgO grain sizes we were able to control the active deformation mechanism (for e.g. diffusion creep or dislocation creep). For coarse-grained specimens, we observed strong (hkl) dependence of radial strain indicating the operation of dislocation creep. The observed (hkl) dependence changes with pressure suggesting a change in the slip system: at pressures higher than 27 GPa, (200) shows larger stress estimate than (220). In contrast, at lower pressures, (220) shows larger stress estimate than (200). This might indicate a slip system transition in MgO occurring under lower mantle conditions. From {110} plane to {100} plane. This is in good agreement with theoretical predictions and numerical calculation [Amodeo et al., 2012] and has an important implication for the interpretation of seismic anisotropy in the D" layer [Karato, 1998]. Amodeo, J., Carrey P., and P. Cordier (2012), Philosophical Magazine, 92(12). Karato, S-I. (1998), Earth and planets Space, 50, 1019-1028 Karato, S.-I. (2009), Physical Review. B, 79(21). Singh, A. K., (1993), Journal of Applied Physic, 73, 4278.

Time-resolved x-ray diffraction and electrical resistance measurements of structural phase transitions in zirconium

DOE PAGES

Velisavljevic, N.; Sinogeikin, S.; Saavedra, R.; ...

2014-05-07

Here, we have designed a portable pressure controller module to tune compression rates and maximum pressures attainable in a standard gas-membrane diamond anvil cell (DAC). During preliminary experiments, performed on zirconium (Zr) metal sample, pressure jumps of up to 80 GPa were systematically obtained in less than 0.2s (resulting in compression rate of few GPa/s up to more than 400 GPa/s). In-situ x-ray diffraction and electrical resistance measurements were performed simultaneously during this rapid pressure increase to provide the first time resolved data on α → ω → β structural evolution in Zr at high pressures. Direct control of compressionmore » rates and peak pressures, which can be held for prolonged time, allows for investigation of structural evolution and kinetics of structural phase transitions of materials under previously unexplored compression rate-pressure conditions that bridge traditional static and shock/dynamic experimental platforms.« less

New diamond cell for single-crystal x-ray diffraction

NASA Astrophysics Data System (ADS)

Boehler, Reinhard

2006-11-01

A new design for a high-precision diamond cell is described. Two kinematically mounted steel disks are elastically deflected to generate pressure. This principle provides higher precision in the diamond anvil alignment than most sliding piston-cylinder or guide-pin devices at significantly lower cost. With this new diamond cell conical diamond anvils with an x-ray aperture of 85° were successfully tested to over 50GPa using helium as a pressure medium. Anvil thickness of less than 1.4mm provides high x-ray transmission and low background, a significant improvement compared to beryllium or diamond-disk backing plates. Because the diamond anvils are supported by tungsten carbide seats, samples and pressure media can be annealed by external or laser heating to provide hydrostatic pressure conditions.

High Pressure Single Crystal Diffraction at PX 2

DOE Office of Scientific and Technical Information (OSTI.GOV)

Zhang, Dongzhou; Dera, Przemyslaw K.; Eng, Peter J.

2017-01-01

In this report, we describe detailed procedures for carrying out single crystal X-ray diffraction experiments with a diamond anvil cell at the GSECARS 13-BM-C beamline at the Advanced Photon Source. ATREX and RSV programs are used to analyze the data.

Diffraction studies of the high pressure phases of GaAs and GaP

NASA Technical Reports Server (NTRS)

Baublitz, M., Jr.; Ruoff, A. L.

1982-01-01

High pressure structural phase transitions of GaAs and GaP have been studied by energy dispersive X-ray diffraction with the radiation from the Cornell High Energy Synchrotron Source. GaAs began to transform at 172 + or - 7 kbar to an orthorhombic structure possibly belonging to space group Fmmm. GaP transformed to a tetragonal beta-Sn type phase at 215 + or - 8 kbar. Although pressure transmitting media were used to minimize shear stresses in the specimens, the high pressure diffraction results were interpreted as showing evidence for planar defects in the specimens.

White-Beam X-ray Diffraction and Radiography Studies on High-Boron Containing Borosilicate Glass at High Pressures

NASA Astrophysics Data System (ADS)

Ham, Kathryn; Vohra, Yogesh; Kono, Yoshio; Wereszczak, Andrew; Patel, Parimal

Multi-angle energy-dispersive x-ray diffraction studies and white-beam x-ray radiography were conducted with a cylindrically shaped (1 mm diameter and 0.7 mm high) high-boron content borosilicate glass sample (17.6% B2O3) to a pressure of 13.7 GPa using a Paris-Edinburgh (PE) press at Beamline 16-BM-B, HPCAT of the Advanced Photon Source. The measured structure factor S(q) to large q = 19 Å-1, is used to determine information about the internuclear bond distances between various species of atoms within the glass sample. Sample pressure was determined with gold as a pressure standard. The sample height as measured by radiography showed an overall uniaxial compression of 22.5 % at 13.7 GPa with 10.6% permanent compaction after decompression to ambient conditions. The reduced pair distribution function G(r) was extracted and Si-O, O-O, and Si-Si bond distances were measured as a function of pressure. Raman spectroscopy of pressure recovered sample as compared to starting material showed blue-shift and changes in intensity and widths of Raman bands associated with silicate and B3O6 boroxol rings. US Army Research Office under Grant No. W911NF-15-1-0614.

Boron monosulfide: Equation of state and pressure-induced phase transition

NASA Astrophysics Data System (ADS)

Cherednichenko, K. A.; Kruglov, I. A.; Oganov, A. R.; Le Godec, Y.; Mezouar, M.; Solozhenko, V. L.

2018-04-01

Quasi-hydrostatic compression of rhombohedral boron monosulfide (r-BS) has been studied up to 50 GPa at room temperature using diamond-anvil cells and angle-dispersive synchrotron X-ray diffraction. A fit of the experimental P-V data to the Vinet equation of state yields the bulk modulus B0 of 42.2(1.4) GPa and its first pressure derivative B0' of 7.6(2) that are in excellent agreement with our ab initio calculations. Formation of a new high-pressure phase of boron monosulfide (hp-BS) has been observed above 35 GPa. According to ab initio evolutionary crystal structure predictions combined with Rietveld refinement of high-pressure X-ray diffraction data, the structure of hp-BS has trigonal symmetry and belongs to the space group P-3m1. As it follows from the electron density of state calculations, the phase transformation is accompanied by an insulator-metal transition.

Equation of state for technetium from X-ray diffraction and first-principle calculations

DOE PAGES

Mast, Daniel S.; Kim, Eunja; Siska, Emily M.; ...

2016-03-20

Here, the ambient temperature equation of state (EoS) of technetium metal has been measured by X-ray diffraction. The metal was compressed using a diamond anvil cell and using a 4:1 methanol-ethanol pressure transmitting medium. The maximum pressure achieved, as determined from the gold pressure scale, was 67 GPa. The compression data shows that the HCP phase of technetium is stable up to 67 GPa. The compression curve of technetium was also calculated using first-principles total-energy calculations. Utilizing a number of fitting strategies to compare the experimental and theoretical data it is determined that the Vinet equation of state with anmore » ambient isothermal bulk modulus of B 0T = 288 GPa and a first pressure derivative of B' = 5.9(2) best represent the compression behavior of technetium metal.« less

Arsenolite: a quasi-hydrostatic solid pressure-transmitting medium.

PubMed

Sans, J A; Manjón, F J; Popescu, C; Muñoz, A; Rodríguez-Hernández, P; Jordá, J L; Rey, F

2016-11-30

This study reports the experimental characterization of the hydrostatic properties of arsenolite (As4O6), a molecular solid which is one of the softest minerals in the absence of hydrogen bonding. The high compressibility of arsenolite and its stability up to 15 GPa have been proved by x-ray diffraction measurements, and the progressive loss of hydrostaticity with increasing pressure up to 20 GPa has been monitored by ruby photoluminescence. Arsenolite has been found to exhibit hydrostatic behavior up to 2.5 GPa and a quasi-hydrostatic behavior up to 10 GPa at room temperature. This result opens the way to explore other molecular solids as possible quasi-hydrostatic pressure-transmitting media. The validity of arsenolite as an insulating, stable, non-penetrating and quasi-hydrostatic medium is explored by the study of the x-ray diffraction of zeolite ITQ-29 at high pressure.

High pressure transport and structural studies on Nb 3Ga superconductor

DOE PAGES

Mkrtcheyan, Vahe; Kumar, Ravhi; Baker, Jason; ...

2014-11-24

We investigated the crystal structure of A-15 superconductor Nb 3Ga with a critical temperature T c = 16.5 K by high pressure x-ray diffraction (HPXRD) using synchrotron x-rays and a diamond anvil cell under Ne pressure medium. Furthermore, the high pressure structural results indicate that Nb 3Ga is stable up to 41 GPa. The P-V plot shows an anomaly around 15 GPa even though there are no pressure induced structural transitions are observed. High pressure resistance measurements were performed up to 0.5 GPa to understand the variation of T c under pressure. Finally, our results show a positive pressure effectmore » on T c.« less

Diamond-anvil cell for radial x-ray diffraction.

PubMed

Chesnut, G N; Schiferl, D; Streetman, B D; Anderson, W W

2006-06-28

We have designed a new diamond-anvil cell capable of radial x-ray diffraction to pressures of a few hundred GPa. The diffraction geometry allows access to multiple angles of Ψ, which is the angle between each reciprocal lattice vector g(hkl) and the compression axis of the cell. At the 'magic angle', Ψ≈54.7°, the effects of deviatoric stresses on the interplanar spacings, d(hkl), are significantly reduced. Because the systematic errors, which are different for each d(hkl), are significantly reduced, the crystal structures and the derived equations of state can be determined reliably. At other values of Ψ, the effects of deviatoric stresses on the diffraction pattern could eventually be used to determine elastic constants.

Impurity incorporation, deposition kinetics, and microstructural evolution in sputtered Ta films

NASA Astrophysics Data System (ADS)

Whitacre, Jay Fredric

There is an increasing need to control the microstructure in thin sputtered Ta films for application as high-temperature coatings or diffusion barriers in microelectronic interconnect structures. To this end, the relationship between impurity incorporation, deposition kinetics, and microstructural evolution was examined for room-temperature low growth rate DC magnetron sputtered Ta films. Impurity levels present during deposition were controlled by pumping the chamber to various base pressures before growth. Ar pressures ranging from 2 to 20 mTorr were used to create contrasting kinetic environments in the sputter gas. This affected both the distribution of adatom kinetic energies at the substrate as well as the rate of impurity desorption from the chamber walls: at higher Ar pressures adatoms has lower kinetic energies, and there was an increase in impurity concentration. X-ray diffraction, high-resolution transmission electron microscopy (HREM), transmission electron diffraction (TED), scanning electron microscopy (SEM), secondary ion mass spectrometry (SIMS), and x-ray photoelectron. spectroscopy (XPS) were used to examine film crystallography, microstructure, and composition. A novel laboratory-based in-situ x-ray diffractometer was constructed. This new set-up allowed for the direct observation of microstructural evolution during growth. Films deposited at increasingly higher Ar pressures displayed a systematic decrease in grain size and degree of texturing, while surface morphology was found to vary from a nearly flat surface to a rough surface with several length scales of organization. In-situ x-ray results showed that the rate of texture evolution was found to be much higher in films grown using lower Ar pressures. These effects were studied in films less than 200 A thick using high resolution x-ray diffraction in conjunction with a synchrotron light source (SSRL B.L. 7-2). Films grown using higher Ar pressures (above 10 mTorr) with a pre-growth base pressure of 1 x 10--6 Torr had grains less than 10 nm in diameter and significant amorphous content Calculated radial distribution functions show a significant increase in average inter-atomic spacing in films grown using higher base pressures and Ar pressures. The amorphous content in the films was determined via comparison between ideal crystalline diffraction patterns and actual data. Thinner films grown at higher Ar pressures had relatively greater amorphous content. Real-time process control using the in-situ diffractometer was also demonstrated. The effects observed are discussed in the context of previous theories and experiments that document room-temperature sputter film growth. The changes in film microstructure observed were impurity mediated. Specifically, oxygen desorbed from the chamber walls during growth were incorporated into the film and subsequently limited grain development and texturing. A second phase consisting of amorphous Ta2O5 formed between the grain nuclei. Adatom kinetics played a role in determining surface morphology: at low Ar pressures (2 mTorr) significant adatom kinetic energies served to flattened the film surface, though impurity levels dominated grain development even in these conditions.

Pressure-induced structural transition in chalcopyrite ZnSiP 2

DOE Office of Scientific and Technical Information (OSTI.GOV)

Bhadram, Venkata S.; Krishna, Lakshmi; Toberer, Eric S.

The pressure-dependent phase behavior of semiconducting chalcopyrite ZnSiP 2 was studied up to 30 GPa using in situ X-ray diffraction and Raman spectroscopy in a diamond-anvil cell. A structural phase transition to the rock salt type structure was observed between 27 and 30 GPa, which is accompanied by soft phonon mode behavior and simultaneous loss of Raman signal and optical transmission through the sample. The high-pressure rock salt type phase possesses cationic disorder as evident from broad features in the X-ray diffraction patterns. The behavior of the low-frequency Raman modes during compression establishes a two-stage, order-disorder phase transition mechanism. Themore » phase transition is partially reversible, and the parent chalcopyrite structure coexists with an amorphous phase upon slow decompression to ambient conditions.« less

Toward Sodium X-Ray Diffraction in the High-Pressure Regime

NASA Astrophysics Data System (ADS)

Gong, X.; Polsin, D. N.; Rygg, J. R.; Boehly, T. R.; Crandall, L.; Henderson, B. J.; Hu, S. X.; Huff, M.; Saha, R.; Collins, G. W.; Smith, R.; Eggert, J.; Lazicki, A. E.; McMahon, M.

2017-10-01

We are working to quasi-isentropically compress sodium into the terapascal regime to test theoretical predictions that sodium transforms to an electride. A series of hydrodynamic simulations have been performed to design experiments to investigate the structure and optical properties of sodium at pressures up to 500 GPa. We show preliminary results where sodium samples, sandwiched between diamond plates and lithium-fluoride windows, are ramp compressed by a gradual increase in the drive-laser intensity. The low sound speed in sodium makes it particularly susceptible to forming a shock; therefore, it is difficult to compress without melting the sample. Powder x-ray diffraction is used to provide information on the structure of sodium at these high pressures. This material is based upon work supported by the Department of Energy National Nuclear Security Administration under Award Number DE-NA0001944.

Structural and conformational properties of 1-decyl-3-methylimidazolium tetrafluoroborate under high pressure

NASA Astrophysics Data System (ADS)

Chen, Liucheng; Li, Haining; Zhu, Xiang; Su, Lei; Yang, Kun; Yuan, Chaosheng; Yang, Guoqiang; Li, Xiaodong

2017-06-01

In situ crystalization of 1-decyl-3-methylimidazolium tetrafluoroborate ([C10MIM][BF4]) from melt has been investigated under high pressure up to 3.4 GPa at room temperature by using Raman spectroscopy and synchrotron X-ray diffraction measurement. Raman spectral analysis indicated that [C10MIM][BF4] experienced two successive phase transitions at about 0.3 GPa and 1.6 GPa. And the polymorphism was also discussed in view of the conformational isomerism of [C10MIM]+ cation between gauche and trans conformers. Notably, liquid-crystal and crystal-crystal phase transitions were further confirmed by synchrotron X-ray diffraction measurement. Moreover, it also indicated that high structural flexibility of the cations with long alkyl chain might have effect on the degree of disorder of pressure-induced crystallization for ionic liquids.

Diffraction leveraged modulation of X-ray pulses using MEMS-based X-ray optics

DOEpatents

Lopez, Daniel; Shenoy, Gopal; Wang, Jin; Walko, Donald A.; Jung, Il-Woong; Mukhopadhyay, Deepkishore

2016-08-09

A method and apparatus are provided for implementing Bragg-diffraction leveraged modulation of X-ray pulses using MicroElectroMechanical systems (MEMS) based diffractive optics. An oscillating crystalline MEMS device generates a controllable time-window for diffraction of the incident X-ray radiation. The Bragg-diffraction leveraged modulation of X-ray pulses includes isolating a particular pulse, spatially separating individual pulses, and spreading a single pulse from an X-ray pulse-train.

X-ray Diffraction Study of Aluminum Carbide Powder to 50 GPa

DOE Office of Scientific and Technical Information (OSTI.GOV)

Ji, C.; Ma, Y; Chyu, M

2009-01-01

The crystal structure and equation of state (EOS) of aluminum carbide (Al{sub 4}C{sub 3}) have been determined directly up to 50.1 GPa at room temperature by the synchrotron x-ray diffraction techniques. The results indicate that Al{sub 4}C{sub 3} remained in rhombohedral structure under all tested pressure-temperature conditions and exhibited anisotropic compressibility, with the c-axis more compressible than the a-axis. Fitting the experimental data to third order Birch-Murnaghan EOS yields a bulk modulus of K{sub OT} = 233 {+-} 6 GPa with its pressure derivative K{sub OT}{prime} = 3.4 {+-} 0.4, while the second-order EOS yields K{sub OT} = 223 {+-}more » 2 GPa.« less

High-pressure studies on nanocrystalline borderline Co1-xFexS2 (x = 0.4 and 0.5) using Mössbauer spectroscopic and electrical resistivity techniques up to 8 GPa

NASA Astrophysics Data System (ADS)

Chandra, Usha; Sharma, Pooja; Parthasarathy, G.

2016-12-01

Like bulk, Co1-xFexS2 nanoparticles also display an anomaly at x = 0.5. The borderline contiguous Co1-xFexS2 (x = 0.4 and 0.5) nanoparticles were synthesized with colloidal method and characterized for pyrite structure using various techniques, viz., X-ray diffraction, energy dispersive X-ray analysis (EDAX), S K-edge X-ray absorption near edge spectra, transmission electron microscopy (TEM) and Fourier transformed infra-red spectroscopy. The report presents the effect of high pressure on the borderline compositions using the Mössbauer spectroscopic and electrical resistivity techniques. Magnetic measurements on the system showed drastic lowering of Tc due to nanosize of the particles. With increased pressure, quadrupole splitting showed an expected trend of increase to attain a peak representing a second-order phase transition between 4 and 5 GPa for both the compositions. The pressure coefficient of electrical resistivity varied from -0.02 GPa to -0.06 GPa across transition pressure indicating a sluggish nature of transition. This is the first report of pressure effect on nanosized borderline compositions.

Effect of Fe-site Substitution on Pressure-induced Spin Transition in SrFeO2

NASA Astrophysics Data System (ADS)

Kawakami, Takateru; Yamamoto, Takafumi; Yata, Kanami; Ishii, Minoru; Watanabe, Yoshitaka; Mizumaki, Masaichiro; Kawamura, Naomi; Ishimatsu, Naoki; Takahashi, Hiroki; Okada, Taku; Yagi, Takehiko; Kageyama, Hiroshi

2017-12-01

The effect of Fe-site substitution on structural and physical properties of the infinite layer iron oxide SrFeO2 was investigated under high pressure by 57Fe Mössbauer spectroscopy, X-ray diffraction, X-ray absorption spectroscopy, X-ray magnetic circular dichroism, and electrical resistance measurements using a diamond-anvil cell. Both 20% Mn- and Co-substituted samples exhibit spin transitions from a high-spin (S = 2) to an intermediate-spin (S = 1) state at Pc ˜ 32 GPa, which is much the same pressure 33 GPa observed in SrFeO2. This result indicates that the spin transition pressure is insensitive to the d-orbital electron counts [Mn2+ (d5), Fe2+ (d6), Co2+ (d7)], but is governed by the local structure around the Fe site.

Tungsten tetraboride, an inexpensive superhard material

PubMed Central

Mohammadi, Reza; Lech, Andrew T.; Xie, Miao; Weaver, Beth E.; Yeung, Michael T.; Tolbert, Sarah H.; Kaner, Richard B.

2011-01-01

Tungsten tetraboride (WB4) is an interesting candidate as a less expensive member of the growing group of superhard transition metal borides. WB4 was successfully synthesized by arc melting from the elements. Characterization using powder X-ray diffraction (XRD) and energy-dispersive X-ray spectroscopy (EDX) indicates that the as-synthesized material is phase pure. The zero-pressure bulk modulus, as measured by high-pressure X-ray diffraction for WB4, is 339 GPa. Mechanical testing using microindentation gives a Vickers hardness of 43.3 ± 2.9 GPa under an applied load of 0.49 N. Various ratios of rhenium were added to WB4 in an attempt to increase hardness. With the addition of 1 at.% Re, the Vickers hardness increased to approximately 50 GPa at 0.49 N. Powders of tungsten tetraboride with and without 1 at.% Re addition are thermally stable up to approximately 400 °C in air as measured by thermal gravimetric analysis. PMID:21690363

Analysis of synthetic diamond single crystals by X-ray topography and double-crystal diffractometry

DOE Office of Scientific and Technical Information (OSTI.GOV)

Prokhorov, I. A., E-mail: igor.prokhorov@mail.ru; Ralchenko, V. G.; Bolshakov, A. P.

2013-12-15

Structural features of diamond single crystals synthesized under high pressure and homoepitaxial films grown by chemical vapor deposition (CVD) have been analyzed by double-crystal X-ray diffractometry and topography. The conditions of a diffraction analysis of diamond crystals using Ge monochromators have been optimized. The main structural defects (dislocations, stacking faults, growth striations, second-phase inclusions, etc.) formed during crystal growth have been revealed. The nitrogen concentration in high-pressure/high-temperature (HPHT) diamond substrates is estimated based on X-ray diffraction data. The formation of dislocation bundles at the film-substrate interface in the epitaxial structures has been revealed by plane-wave topography; these dislocations are likelymore » due to the relaxation of elastic macroscopic stresses caused by the lattice mismatch between the substrate and film. The critical thicknesses of plastic relaxation onset in CVD diamond films are calculated. The experimental techniques for studying the real diamond structure in optimizing crystal-growth technology are proven to be highly efficient.« less

SYNCHROTRON RADIATION, FREE ELECTRON LASER, APPLICATION OF NUCLEAR TECHNOLOGY, ETC.: A new cell for X-ray absorption spectroscopy study under high pressure

NASA Astrophysics Data System (ADS)

Zheng, Li-Rong; Che, Rong-Zheng; Liu, Jing; Du, Yong-Hua; Zhou, Ying-Li; Hu, Tian-Dou

2009-08-01

X-ray absorption fine structure (XAFS) spectroscopy is a powerful technique for the investigation of the local environment around selected atoms in condensed matter. XAFS under pressure is an important method for the synchrotron source. We design a cell for a high pressure XAFS experiment. Sintered boron carbide is used as the anvils of this high pressure cell in order to obtain a full XAFS spectrum free from diffraction peaks. In addition, a hydraulic pump was adopted to make in-suit pressure modulation. High quality XAFS spectra of ZrH2 under high pressure (up to 13 GPa) were obtained by this cell.

Studying Pulsed Laser Deposition conditions for Ni/C-based multi-layers

NASA Astrophysics Data System (ADS)

Bollmann, Tjeerd R. J.

2018-04-01

Nickel carbon based multi-layers are a viable route towards future hard X-ray and soft γ-ray focusing telescopes. Here, we study the Pulsed Laser Deposition growth conditions of such bilayers by Reflective High Energy Electron Diffraction, X-ray Reflectivity and Diffraction, Atomic Force Microscopy, X-ray Photoelectron Spectroscopy and cross-sectional Transmission Electron Microscopy analysis, with emphasis on optimization of process pressure and substrate temperature during growth. The thin multi-layers are grown on a treated SiO substrate resulting in Ni and C layers with surface roughnesses (RMS) of ≤0.2 nm. Small droplets resulting during melting of the targets surface increase the roughness, however, and cannot be avoided. The sequential process at temperatures beyond 300 °C results into intermixing between the two layers, being destructive for the reflectivity of the multi-layer.

Dynamic X-ray diffraction observation of shocked solid iron up to 170 GPa

PubMed Central

Denoeud, Adrien; Ozaki, Norimasa; Benuzzi-Mounaix, Alessandra; Uranishi, Hiroyuki; Kondo, Yoshihiko; Kodama, Ryosuke; Brambrink, Erik; Ravasio, Alessandra; Bocoum, Maimouna; Boudenne, Jean-Michel; Harmand, Marion; Guyot, François; Mazevet, Stephane; Riley, David; Makita, Mikako; Sano, Takayoshi; Sakawa, Youichi; Inubushi, Yuichi; Gregori, Gianluca; Koenig, Michel; Morard, Guillaume

2016-01-01

Investigation of the iron phase diagram under high pressure and temperature is crucial for the determination of the composition of the cores of rocky planets and for better understanding the generation of planetary magnetic fields. Here we present X-ray diffraction results from laser-driven shock-compressed single-crystal and polycrystalline iron, indicating the presence of solid hexagonal close-packed iron up to pressure of at least 170 GPa along the principal Hugoniot, corresponding to a temperature of 4,150 K. This is confirmed by the agreement between the pressure obtained from the measurement of the iron volume in the sample and the inferred shock strength from velocimetry deductions. Results presented in this study are of the first importance regarding pure Fe phase diagram probed under dynamic compression and can be applied to study conditions that are relevant to Earth and super-Earth cores. PMID:27357672

Spiral chain structure of high pressure selenium-II{sup '} and sulfur-II from powder x-ray diffraction

DOE Office of Scientific and Technical Information (OSTI.GOV)

Fujihisa, Hiroshi; Yamawaki, Hiroshi; Sakashita, Mami

2004-10-01

The structure of high pressure phases, selenium-II{sup '} (Se-II{sup '}) and sulfur-II (S-II), for {alpha}-Se{sub 8} (monoclinic Se-I) and {alpha}-S{sub 8} (orthorhombic S-I) was studied by powder x-ray diffraction experiments. Se-II{sup '} and S-II were found to be isostructural and to belong to the tetragonal space group I4{sub 1}/acd, which is made up of 16 atoms in the unit cell. The structure consisted of unique spiral chains with both 4{sub 1} and 4{sub 3} screws. The results confirmed that the structure sequence of the pressure-induced phase transitions for the group VIb elements depended on the initial molecular form. The chemicalmore » bonds of the phases are also discussed from the interatomic distances that were obtained.« less

Strength of shock-loaded single-crystal tantalum [100] determined using in situ broadband x-ray Laue diffraction.

PubMed

Comley, A J; Maddox, B R; Rudd, R E; Prisbrey, S T; Hawreliak, J A; Orlikowski, D A; Peterson, S C; Satcher, J H; Elsholz, A J; Park, H-S; Remington, B A; Bazin, N; Foster, J M; Graham, P; Park, N; Rosen, P A; Rothman, S R; Higginbotham, A; Suggit, M; Wark, J S

2013-03-15

The strength of shock-loaded single crystal tantalum [100] has been experimentally determined using in situ broadband x-ray Laue diffraction to measure the strain state of the compressed crystal, and elastic constants calculated from first principles. The inferred strength reaches 35 GPa at a shock pressure of 181 GPa and is in excellent agreement with a multiscale strength model [N. R. Barton et al., J. Appl. Phys. 109, 073501 (2011)], which employs a hierarchy of simulation methods over a range of length scales to calculate strength from first principles.

X-ray diffraction studies of shocked lunar analogs

NASA Technical Reports Server (NTRS)

Hanss, R. E.

1979-01-01

The X-ray diffraction experiments on shocked rock and mineral analogs of particular significance to lunar geology are described. Materials naturally shocked by meteorite impact, nuclear-shocked, or artificially shocked in a flat plate accelerator were utilized. Four areas were outlined for investigation: powder diffractometer studies of shocked single crystal silicate minerals (quartz, orthoclase, oligoclase, pyroxene), powder diffractometer studies of shocked polycrystalline monomineralic samples (dunite), Debye-Scherrer studies of single grains of shocked granodiorite, and powder diffractometer studies of shocked whole rock samples. Quantitative interpretation of peak shock pressures experienced by materials found in lunar or terrestrial impact structures is presented.

Exploring hardness enhancement in superhard tungsten tetraboride-based solid solutions using radial X-ray diffraction

DOE PAGES

Xie, Miao; Mohammadi, Reza; Turner, Christopher L.; ...

2015-07-29

In this paper, we explore the hardening mechanisms in WB4-based solid solutions upon addition of Ta, Mn, and Cr using in situ radial X-ray diffraction techniques under nonhydrostatic pressure. By examining the lattice-supported differential strain, we provide insights into the mechanism for hardness increase in binary solid solutions at low dopant concentrations. Speculations on the combined effects of electronic structure and atomic size in ternary WB 4 solid solutions containing Ta with Mn or Cr are also included to understand the extremely high hardness of these materials.

High pressure study of a highly energetic nitrogen-rich carbon nitride, cyanuric triazide

DOE Office of Scientific and Technical Information (OSTI.GOV)

Laniel, Dominique; Desgreniers, Serge; Downie, Laura E.

Cyanuric triazide (CTA), a nitrogen-rich energetic material, was compressed in a diamond anvil cell up to 63.2 GPa. Samples were characterized by x-ray diffraction, Raman, and infrared spectroscopy. A phase transition occurring between 29.8 and 30.7 GPa was found by all three techniques. The bulk modulus and its pressure derivative of the low pressure phase were determined by fitting the 300 K isothermal compression data to the Birch-Murnaghan equation of state. Due to the strong photosensitivity of CTA, synchrotron generated x-rays and visible laser radiation both lead to the progressive conversion of CTA into a two dimensional amorphous C=N network,more » starting from 9.2 GPa. As a result of the conversion, increasingly weak and broad x-ray diffraction lines were recorded from crystalline CTA as a function of pressure. Hence, a definite structure could not be obtained for the high pressure phase of CTA. Results from infrared spectroscopy carried out to 40.5 GPa suggest the high pressure formation of a lattice built of tri-tetrazole molecular units. The decompression study showed stability of the high pressure phase down to 13.9 GPa. Finally, two CTA samples, one loaded with neon and the other with nitrogen, used as pressure transmitting media, were laser-heated to approximately 1100 K and 1500 K while compressed at 37.7 GPa and 42.0 GPa, respectively. In both cases CTA decomposed resulting in amorphous compounds, as recovered at ambient conditions.« less

Thermal equation of state of TiC: A synchrotron x-ray diffraction study

DOE Office of Scientific and Technical Information (OSTI.GOV)

Yu Xiaohui; National Lab for Condensed Matter Physics, Institute of Physics, CAS, Beijing 100080; Department of Physics, University of Science and Technology of China, Hefei 230026

2010-06-15

The pressure-volume-temperature measurements were carried out for titanium carbide (TiC) at pressures and temperatures up to 8.1 GPa and 1273 K using energy-dispersive synchrotron x-ray diffraction. Thermoelastic parameters were derived for TiC based on a modified high-temperature Birch-Murnaghan equation of state and a thermal pressure approach. With the pressure derivative of the bulk modulus, K{sub 0}{sup '}, fixed at 4.0, we obtain: the ambient bulk modulus K{sub 0}=268(6) GPa, which is comparable to previously reported value; temperature derivative of bulk modulus at constant pressure ({partial_derivative}K{sub T}/{partial_derivative}T){sub P}=-0.026(9) GPa K{sup -1}, volumetric thermal expansivity {alpha}{sub T}(K{sup -1})=a+bT with a=1.62(12)x10{sup -5} K{supmore » -1} and b=1.07(17)x10{sup -8} K{sup -2}, pressure derivative of thermal expansion ({partial_derivative}{alpha}/{partial_derivative}P){sub T}=(-3.62{+-}1.14)x10{sup -7} GPa{sup -1} K{sup -1}, and temperature derivative of bulk modulus at constant volume ({partial_derivative}K{sub T}/{partial_derivative}T){sub V}=-0.015(8) GPa K{sup -1}. These results provide fundamental thermophysical properties for TiC for the first time and are important to theoretical and computational modeling of transition metal carbides.« less

Thermal equation-of-state of TiC: a synchrotron x-ray diffraction study

DOE Office of Scientific and Technical Information (OSTI.GOV)

Yu, Xiaohui; Lin, Zhijun; Zhang, Jianzhong

2009-01-01

The pressure (P)-volume (V)-temperature (T) measurements were carried out for titanium carbide at pressures and temperatures up to 8.1 GPa and 1273 K using energy-dispersive synchrotron x-ray diffraction. Thermoelastic parameters were derived for TiC based on a modified high-temperature Birch-Murnaghan equation of state and a thermal-pressure approach. With the pressure derivative of the bulk modulus, K'{sub 0}, fixed at 4.0, we obtain: the ambient bulk modulus K{sub 0} = 268(6) GPa, temperature derivative of bulk modulus at constant pressure ({partial_derivative}K{sub T}/{partial_derivative}T){sub p} = -0.026(9) GPa K{sup -1}, volumetric thermal expansivity a{sub T}(K{sup -1}) = a + bT with a =more » 1.62(12) x 10{sup -5} K{sup -1} and b = 1.07(17) x 10{sup -8} K{sup -2}, pressure derivative of thermal expansion ({partial_derivative}a/{partial_derivative}P){sub T} = (-3.62 {+-} 1.14) x 10{sup -7} GPa{sup -1} K{sup -1}, and temperature derivative of bulk modulus at constant volume ({partial_derivative}K{sub T}/{partial_derivative}T){sub v} = -0.015 (8) GPa K{sup -1}. These results provide fundamental thermo physical properties for TiC and are important to theoretical and computational modeling of transition metal carbides.« less

Melting relations in the Fe-S-Si system at high pressure and temperature: implications for the planetary core

NASA Astrophysics Data System (ADS)

Sakairi, Takanori; Ohtani, Eiji; Kamada, Seiji; Sakai, Takeshi; Sakamaki, Tatsuya; Hirao, Naohisa

2017-12-01

The phase and melting relations in the Fe-S-Si system were determined up to 60 GPa by using a double-sided laser-heated diamond anvil cell combined with X-ray diffraction. On the basis of the X-ray diffraction patterns, we confirmed that hcp/fcc Fe-Si alloys and Fe3S are stable phases under subsolidus conditions in the Fe-S-Si system. Both solidus and liquidus temperatures are significantly lower than the melting temperature of pure Fe and both increase with pressure. The slopes of the Fe-S-Si liquidus and solidus curves determined here are smaller than the adiabatic temperature gradients of the liquid cores of Mercury and Mars. Thus, crystallization of their cores started at the core-mantle boundary region.

Simultaneous Pressure-Induced Magnetic and Valence Transitions in Type-I Clathrate Eu8Ga16Ge30

NASA Astrophysics Data System (ADS)

Onimaru, Takahiro; Tsutsui, Satoshi; Mizumaki, Masaichiro; Kawamura, Naomi; Ishimatsu, Naoki; Avila, Marcos A.; Yamamoto, Shuhei; Yamane, Haruki; Suekuni, Koichiro; Umeo, Kazunori; Kume, Tetsuji; Nakano, Satoshi; Takabatake, Toshiro

2014-01-01

We have performed X-ray magnetic circular dichroism (XMCD) and X-ray absorption spectroscopy (XAS) measurements at pressures up to 17 GPa for the clathrate Eu8Ga16Ge30 (Curie temperature TC = 36 K). The temperature dependence of the XMCD spectra agrees well with that of the DC magnetization at ambient pressure. The TC is gradually enhanced with increasing pressures up to 13.3 GPa, and the divalent state of the Eu ions with J = 7/2 remains stable, but at 17 GPa the XMCD intensity is strongly suppressed and a spectral weight corresponding to the trivalent state of Eu ions (with no magnetic moment) appears in the XAS spectrum. The concurrent change from the type-I clathrate structure to an amorphous phase has been observed by X-ray diffraction experiment. We conclude that the amorphization of this compound induces the mixed valence state, which collapses the ferromagnetism.

Beyond sixfold coordinated Si in SiO2 glass at ultrahigh pressures

PubMed Central

Prescher, Clemens; Prakapenka, Vitali B.; Stefanski, Johannes; Jahn, Sandro; Skinner, Lawrie B.; Wang, Yanbin

2017-01-01

We investigated the structure of SiO2 glass up to 172 GPa using high-energy X-ray diffraction. The combination of a multichannel collimator with diamond anvil cells enabled the measurement of structural changes in silica glass with total X-ray diffraction to previously unachievable pressures. We show that SiO2 first undergoes a change in Si–O coordination number from fourfold to sixfold between 15 and 50 GPa, in agreement with previous investigations. Above 50 GPa, the estimated coordination number continuously increases from 6 to 6.8 at 172 GPa. Si–O bond length shows first an increase due to the fourfold to sixfold coordination change and then a smaller linear decrease up to 172 GPa. We reconcile the changes in relation to the oxygen-packing fraction, showing that oxygen packing decreases at ultrahigh pressures to accommodate the higher than sixfold Si–O coordination. These results give experimental insight into the structural changes of silicate glasses as analogue materials for silicate melts at ultrahigh pressures. PMID:28874582

Beyond sixfold coordinated Si in SiO2 glass at ultrahigh pressures.

PubMed

Prescher, Clemens; Prakapenka, Vitali B; Stefanski, Johannes; Jahn, Sandro; Skinner, Lawrie B; Wang, Yanbin

2017-09-19

We investigated the structure of SiO 2 glass up to 172 GPa using high-energy X-ray diffraction. The combination of a multichannel collimator with diamond anvil cells enabled the measurement of structural changes in silica glass with total X-ray diffraction to previously unachievable pressures. We show that SiO 2 first undergoes a change in Si-O coordination number from fourfold to sixfold between 15 and 50 GPa, in agreement with previous investigations. Above 50 GPa, the estimated coordination number continuously increases from 6 to 6.8 at 172 GPa. Si-O bond length shows first an increase due to the fourfold to sixfold coordination change and then a smaller linear decrease up to 172 GPa. We reconcile the changes in relation to the oxygen-packing fraction, showing that oxygen packing decreases at ultrahigh pressures to accommodate the higher than sixfold Si-O coordination. These results give experimental insight into the structural changes of silicate glasses as analogue materials for silicate melts at ultrahigh pressures.

High pressure high temperature devitrification of Fe78B13Si9 metallic glass with simultaneous x-ray structural characterization

NASA Astrophysics Data System (ADS)

Stemshorn, Andrew K.; Vohra, Yogesh K.; Smith, Spencer J.

2018-06-01

Changes in bulk crystallization behavior following devitrification at high pressure are investigated for a Fe78B13Si9 composition metallic glass using in-situ energy dispersive x-ray powder diffraction. Crystallization with time was evaluated for a series of measurements to a maximum pressure of 5.63 ± 0.15 GPa for the Fe78B13Si9 glass. Pressure was found to strongly affect onset bulk crystallization temperature Tx. Crystallization at each pressure was found to progress in two stages. In the first stage, α-Fe precipitates and in the second Fe2B forms while α-Fe continues to crystallize. Complementary high pressure room temperature studies were conducted.

Chemistry through cocrystals: pressure-induced polymerization of C 2H 2·C 6H 6 to an extended crystalline hydrocarbon

DOE Office of Scientific and Technical Information (OSTI.GOV)

Ward, Matthew D.; Huang, Haw-Tyng; Zhu, Li

The 1:1 acetylene–benzene cocrystal, C 2H 2·C 6H 6, was synthesized under pressure in a diamond anvil cell (DAC) and its evolution under pressure was studied with single-crystal X-ray diffraction and Raman spectroscopy.

Chemistry through cocrystals: pressure-induced polymerization of C 2H 2·C 6H 6 to an extended crystalline hydrocarbon

DOE Office of Scientific and Technical Information (OSTI.GOV)

Ward, Matthew D.; Huang, Haw-Tyng; Zhu, Li

The 1 : 1 acetylene–benzene cocrystal, C 2H 2·C 6H 6, was synthesized under pressure in a diamond anvil cell (DAC) and its evolution under pressure was studied with single-crystal X-ray diffraction and Raman spectroscopy.

Pressure-induced anomalies and structural instability in compressed β-Sb 2 O 3

DOE Office of Scientific and Technical Information (OSTI.GOV)

Zou, Yongtao; Zhang, Wei; Li, Xuefei

2018-01-01

Here, we have discovered a new high-pressure phase of Sb 2 O 3 , and reported pressure-induced anomalies in orthorhombic β-Sb 2 O 3 (valentinite) by the combination of synchrotron in situ X-ray diffraction and first-principles theoretical calculations up to 40.5 GPa.

Micro X-ray diffraction analysis of thin films using grazing-exit conditions.

PubMed

Noma, T; Iida, A

1998-05-01

An X-ray diffraction technique using a hard X-ray microbeam for thin-film analysis has been developed. To optimize the spatial resolution and the surface sensitivity, the X-ray microbeam strikes the sample surface at a large glancing angle while the diffracted X-ray signal is detected with a small (grazing) exit angle. Kirkpatrick-Baez optics developed at the Photon Factory were used, in combination with a multilayer monochromator, for focusing X-rays. The focused beam size was about 10 x 10 micro m. X-ray diffraction patterns of Pd, Pt and their layered structure were measured. Using a small exit angle, the signal-to-background ratio was improved due to a shallow escape depth. Under the grazing-exit condition, the refraction effect of diffracted X-rays was observed, indicating the possibility of surface sensitivity.

Density and structure of jadeite melt at high pressure and high temperature

NASA Astrophysics Data System (ADS)

Sakamaki, T.; Yu, T.; Jing, Z.; Park, C.; Shen, G.; Wang, Y.

2011-12-01

Knowledge of density of magma is important for understanding magma-related processes such as volcanic activity and differentiation in the Earth's early history. Since these processes take place in Earth's interior, we need to measure the density of magma in situ at high pressures. It is also necessary to relate the density with the structure of silicate melts at high pressure and temperature and further understand the densification mechanism of magma with pressure. Here we report the density and structural data for jadeite melt up to 7 GPa,. The density measurements were carried out using a DIA-type cubic press at the 13-BM-D beamline at APS using monochromatic radiation tuned to the desired energy (~20 keV) with a Si (111) double-crystal monochromator. Intensities of the incident and transmitted X-rays were measured by two ion chambers placed before and after the press for X-ray absorption measurements. Incident and transmitted X-ray intensities were obtained by moving the incident slits perpendicular to the X-ray beam direction at 0.010 mm steps crosses the sample. Lambert-Beer law was then applied to the normalized intensities as a function of the sample position across the assembly. Density of jadeite melt was determined up to 7 GPa and 2300 K. For structural determination, high-pressure and high-temperature energy-dispersive XRD experiments were carried out by using a Paris-Edinburgh press installed at the 16-BM-B of APS. Incident X-rays were collimated by a vertical slit (0.5 mm) and a horizontal slit (0.1 mm) to irradiate the sample. Diffracted X-rays were detected by a Ge solid state detector with a 4k multi-channel analyzer, through a collimator and 5.0mm (V) by and 0.1mm (H) receiving slits. Diffraction patterns were collected until the highest intensity reached 2000 counts, at 12 angles (2theta=3, 4, 5, 7, 9, 11, 15, 20, 25, 30, 35, 39.5 degrees). The structural measurements were carried out in the pressure range from 1 to 5 GPa and at 1600 to 2000 K. Pressure and temperature dependence of density of jadeite melt will be presented, along with structure factor S(Q) and radial distribution function G(r) of jadeite melt at high pressure and high temperature. The density-structure relationships will be discussed.

Compression behavior of WC and WC-6%Co up to 50 GPa determined by synchrotron x-ray diffraction and ultrasonic techniques

DOE Office of Scientific and Technical Information (OSTI.GOV)

Amulele, George M.; Manghnani, Murli H.; Marriappan, Sekar

2008-07-23

The equations of state (pressure-volume relations) for WC and WC-6%Co have been determined by synchrotron x-ray diffraction measurements on polycrystalline powder samples loaded in a diamond anvil cell as well as by ultrasonic measurements on hot-pressed polycrystalline, cylindrical samples loaded in a multianvil high-pressure apparatus. The third-order Birch-Murnaghan equation of state fitted to the x-ray diffraction pressure-density sets of data, collected up to 50 GPa, yields ambient pressure isothermal bulk moduli of K{sub oT} = 411.8{+-}12.1 GPa and K{sub oT} = 402.4{+-}14.1 GPa, with pressure derivatives of K{sub oT}' = 5.45{+-}0.73 and K{sub oT}' = 7.50{+-}0.86 for WC and WC-6%Co,more » respectively. The ultrasonic measurements, conducted up to 14 GPa, enabled the determination of the pressure dependences of both bulk and shear moduli. Using Eulerian finite strain equations to fit the ultrasonic data, we obtain for WC an ambient pressure adiabatic bulk modulus of K{sub os} = 383.8{+-}0.8 GPa, and K{sub os}' = 2.61{+-}0.07 for its pressure derivative, while values of G{sub os} = 304.0{+-}0.3 GPa and G{sub os}' = 1.50{+-}0.09 were determined for the shear modulus and its pressure derivative, respectively. Meanwhile, for WC-6%Co, we obtain K{sub os} = 357.5{+-}1.0 GPa, K{sub os}' = 5.18{+-}0.14, G{sub os} = 253.5{+-}0.3 GPa, and G{sub os}' = 1.09{+-}0.09. The equations of state derived from the ultrasonic data are in good agreement with extrapolated results reported previously by Day and Ruoff [J. Appl. Phys. 44, 2447 (1973)] and Gerlich and Kennedy [J. Appl. Phys. 50, 3331 (1978)] who carried out measurements up to 0.2 and 1.0 GPa, respectively.« less

In situ X-ray ptychography imaging of high-temperature CO2 acceptor particle agglomerates

NASA Astrophysics Data System (ADS)

Høydalsvik, Kristin; Bø Fløystad, Jostein; Zhao, Tiejun; Esmaeili, Morteza; Diaz, Ana; Andreasen, Jens W.; Mathiesen, Ragnvald H.; Rønning, Magnus; Breiby, Dag W.

2014-06-01

Imaging nanoparticles under relevant reaction conditions of high temperature and gas pressure is difficult because conventional imaging techniques, like transmission electron microscopy, cannot be used. Here we demonstrate that the coherent diffractive imaging technique of X-ray ptychography can be used for in situ phase contrast imaging in structure studies at atmospheric pressure and elevated temperatures. Lithium zirconate, a candidate CO2 capture material, was studied at a pressure of one atmosphere in air and in CO2, at temperatures exceeding 600 °C. Images with a spatial resolution better than 200 nm were retrieved, and possibilities for improving the experiment are described.

Structural changes in shock compressed silicon observed using time-resolved x-ray diffraction at the Dynamic Compression Sector

NASA Astrophysics Data System (ADS)

Turneaure, Stefan; Zdanowicz, E.; Sinclair, N.; Graber, T.; Gupta, Y. M.

2015-06-01

Structural changes in shock compressed silicon were observed directly using time-resolved x-ray diffraction (XRD) measurements at the Dynamic Compression Sector at the Advanced Photon Source. The silicon samples were impacted by polycarbonate impactors accelerated to velocities greater than 5 km/s using a two-stage light gas gun resulting in impact stresses of about 25 GPa. The 23.5 keV synchrotron x-ray beam passed through the polycarbonate impactor, the silicon sample, and an x-ray window (polycarbonate or LiF) at an angle of 30 degrees relative to the impact plane. Four XRD frames (~ 100 ps snapshots) were obtained with 153.4 ns between frames near the time of impact. The XRD measurements indicate that in the peak shocked state, the silicon samples completely transformed to a high-pressure phase. XRD results for both shocked polycrystalline silicon and single crystal silicon will be presented and compared. Work supported by DOE/NNSA.

Complete agreement of the post-spinel transition with the 660-km seismic discontinuity.

PubMed

Ishii, Takayuki; Huang, Rong; Fei, Hongzhan; Koemets, Iuliia; Liu, Zhaodong; Maeda, Fumiya; Yuan, Liang; Wang, Lin; Druzhbin, Dmitry; Yamamoto, Takafumi; Bhat, Shrikant; Farla, Robert; Kawazoe, Takaaki; Tsujino, Noriyoshi; Kulik, Eleonora; Higo, Yuji; Tange, Yoshinori; Katsura, Tomoo

2018-04-20

The 660-km seismic discontinuity, which is a significant structure in the Earth's mantle, is generally interpreted as the post-spinel transition, as indicated by the decomposition of ringwoodite to bridgmanite + ferropericlase. All precise high-pressure and high-temperature experiments nevertheless report 0.5-2 GPa lower transition pressures than those expected at the discontinuity depth (i.e. 23.4 GPa). These results are inconsistent with the post-spinel transition hypothesis and, therefore, do not support widely accepted models of mantle composition such as the pyrolite and CI chondrite models. Here, we present new experimental data showing post-spinel transition pressures in complete agreement with the 660-km discontinuity depth obtained by high-resolution in situ X-ray diffraction in a large-volume high-pressure apparatus with a tightly controlled sample pressure. These data affirm the applicability of the prevailing mantle models. We infer that the apparently lower pressures reported by previous studies are experimental artefacts due to the pressure drop upon heating. The present results indicate the necessity of reinvestigating the position of mantle mineral phase boundaries previously obtained by in situ X-ray diffraction in high-pressure-temperature apparatuses.

Time-resolved structural dynamics of thin metal films heated with femtosecond optical pulses.

PubMed

Chen, Jie; Chen, Wei-Kan; Tang, Jau; Rentzepis, Peter M

2011-11-22

We utilize 100 fs optical pulses to induce ultrafast disorder of 35- to 150-nm thick single Au(111) crystals and observe the subsequent structural evolution using 0.6-ps, 8.04-keV X-ray pulses. Monitoring the picosecond time-dependent modulation of the X-ray diffraction intensity, width, and shift, we have measured directly electron/phonon coupling, phonon/lattice interaction, and a histogram of the lattice disorder evolution, such as lattice breath due to a pressure wave propagating at sonic velocity, lattice melting, and recrystallization, including mosaic formation. Results of theoretical simulations agree and support the experimental data of the lattice/liquid phase transition process. These time-resolved X-ray diffraction data provide a detailed description of all the significant processes induced by ultrafast laser pulses impinging on thin metallic single crystals.

Sb-related defects in Sb-doped ZnO thin film grown by pulsed laser deposition

NASA Astrophysics Data System (ADS)

Luo, Caiqin; Ho, Lok-Ping; Azad, Fahad; Anwand, Wolfgang; Butterling, Maik; Wagner, Andreas; Kuznetsov, Andrej; Zhu, Hai; Su, Shichen; Ling, Francis Chi-Chung

2018-04-01

Sb-doped ZnO films were fabricated on c-plane sapphire using the pulsed laser deposition method and characterized by Hall effect measurement, X-ray photoelectron spectroscopy, X-ray diffraction, photoluminescence, and positron annihilation spectroscopy. Systematic studies on the growth conditions with different Sb composition, oxygen pressure, and post-growth annealing were conducted. If the Sb doping concentration is lower than the threshold ˜8 × 1020 cm-3, the as-grown films grown with an appropriate oxygen pressure could be n˜4 × 1020 cm-3. The shallow donor was attributed to the SbZn related defect. Annealing these samples led to the formation of the SbZn-2VZn shallow acceptor which subsequently compensated for the free carrier. For samples with Sb concentration exceeding the threshold, the yielded as-grown samples were highly resistive. X-ray diffraction results showed that the Sb dopant occupied the O site rather than the Zn site as the Sb doping exceeded the threshold, whereas the SbO related deep acceptor was responsible for the high resistivity of the samples.

High-pressure x-ray diffraction study of YBO{sub 3}/Eu{sup 3+}, GdBO{sub 3}, and EuBO{sub 3}: Pressure-induced amorphization in GdBO{sub 3}

DOE Office of Scientific and Technical Information (OSTI.GOV)

Wang, Pei; Xu, Chao; Ren, Xiangting

2014-01-28

Angle-dispersive synchrotron X-ray diffraction measurements were performed on vaterite-type YBO{sub 3}/Eu{sup 3+}, GdBO{sub 3}, and EuBO{sub 3}, respectively, up to 41 GPa at room temperature using a diamond-anvil cell. Pressure-induced amorphization was observed in hexagonal GdBO{sub 3} with a significant compression along the c-axis. Compared to the ions of the distorted GdBO{sub 3} phase, its anions may lose their long-range order prior to the cations at high pressures. Based on the experimental pressure-volume data, the obtained bulk moduli of YBO{sub 3}/Eu{sup 3+} and GdBO{sub 3} are 329 and 321 GPa, respectively, which are more than 90% larger than that of EuBO{sub 3}more » (167 GPa) and are presumably attributed to Gd{sup 3+} and Y{sup 3+} with a high density of d valence electrons.« less

DOE Office of Scientific and Technical Information (OSTI.GOV)

Ferreira, A. S.; Rovani, P. R.; Lima, J. C. de, E-mail: joao.cardoso.lima@ufsc.br

A nanostructured Ti{sub 50}Ni{sub 25}Fe{sub 25} phase (B2) was formed by mechanical alloying and its structural stability was studied as a function of pressure. The changes were followed by X-ray diffraction. The B2 phase was observed up to 7 GPa; for larger pressures, the B2 phase transformed into a trigonal/hexagonal phase (B19) that was observed up to the highest pressure used (18 GPa). Besides B2 and B19, elemental Ni or a SS-(Fe,Ni) and FeNi{sub 3} were observed. With decompression, the B2 phase was recovered. Using in situ angle-dispersive X-ray diffraction patterns, the single line method was applied to obtain the apparent crystallitemore » size and the microstrain for both the B2 and the B19 phases as a function of the applied pressure. Values of the bulk modulus for the B2, B19, elemental Ni or SS-(Fe,Ni) and FeNi{sub 3} phases were obtained by fitting the pressure dependence of the volume to a Birch–Murnaghan equation of state (BMEOS)« less

Structure and stability of solid Xe(H 2) n

DOE PAGES

Somayazulu, Maddury; Dera, Przemyslaw; Smith, Jesse; ...

2015-03-10

Mixtures of xenon and molecular hydrogen form a series of hexagonal, van der Waals compounds at high pressures and at 300 K. Synchrotron, x-ray, single crystal diffraction studies reveal that below 7.5 GPa, Xe(H 2) 8 crystallizes in a P3¯m1 structure that displays pressure-induced occupancy changes of two pairs of xenon atoms located on the 2c and 2d sites (while the third pair on yet another 2c site remains fully occupied). The occupancy becomes 1 at the P3¯m1 to R3 transition and all the xenon atoms occupy the 3d sites in the high-pressure structure. These pressure-induced changes in occupancy coincidemore » with volume changes that maintain the average Xe:H 2 stoichiometry fixed at 1:8. Furthermore, the synchrotron x-ray diffraction and Raman measurements show that this unique hydrogen-bearing compound that can be synthesized at 4.2 GPa and 300 K, quenched at low temperatures to atmospheric pressure, and retained up to 90 K on subsequent warming.« less

In Situ X-ray Diffraction of Forsterite Under Shock Compression to 52 GPa: Time Resolved Observation of Changes in Crystal Structure and Phase

NASA Astrophysics Data System (ADS)

Akin, M. C.; Maddox, B.; Teruya, A.; Asimow, P. D.

2015-12-01

The Earth's mantle is composed primarily of ferromagnesian silicates, of which Forsterite (Fo) is the magnesium-rich end member of the dominant upper mantle phase, olivine. Fo is thought to undergo a chemical decomposition associated with a structural phase transition when dynamically loaded to 40-71 GPa, but previous inferences about such decomposition have been based only on pressure-density data with no direct phase identification. To obtain direct data on the phase evolution of shocked Fo, synthetic single crystal samples of Mg2SiO4 Fo were loaded to pressures of 52 GPa using a two stage light gas gun. X-ray diffraction (XRD) patterns were collected on the static and the loaded samples in situ using a single pulse Mo Kα anode to provide a 17 keV X-ray source. X-ray polycapillary optics were used to couple the source to the sample. Clear Laue spots were observed in the static images, while the dynamic images show the appearance of new spots at early times and powder-like rings at late times. The angles of the dynamically driven spots and rings overlap with each other and indicate the change in phase of forsterite under pressure through a process that begins with the formation of single crystals and ends with polycrystalline material. Efforts are underway to identify the high-pressure phases from among the library of dense magnesium silicates, and further experiments covering a larger pressure range will be completed shortly. This work performed under the auspices of the U.S. Department of Energy by Lawrence Livermore National Laboratory under Contract DE-AC52-07NA27344.

Heteroepitaxial Growth of Ferromagnetic MnSb(0001) Films on Ge/Si(111) Virtual Substrates.

PubMed

Burrows, Christopher W; Dobbie, Andrew; Myronov, Maksym; Hase, Thomas P A; Wilkins, Stuart B; Walker, Marc; Mudd, James J; Maskery, Ian; Lees, Martin R; McConville, Christopher F; Leadley, David R; Bell, Gavin R

2013-11-06

Molecular beam epitaxial growth of ferromagnetic MnSb(0001) has been achieved on high quality, fully relaxed Ge(111)/Si(111) virtual substrates grown by reduced pressure chemical vapor deposition. The epilayers were characterized using reflection high energy electron diffraction, synchrotron hard X-ray diffraction, X-ray photoemission spectroscopy, and magnetometry. The surface reconstructions, magnetic properties, crystalline quality, and strain relaxation behavior of the MnSb films are similar to those of MnSb grown on GaAs(111). In contrast to GaAs substrates, segregation of substrate atoms through the MnSb film does not occur, and alternative polymorphs of MnSb are absent.

A structural investigation into the compaction behavior of pharmaceutical composites using powder X-ray diffraction and total scattering analysis.

PubMed

Moore, Michael D; Steinbach, Alison M; Buckner, Ira S; Wildfong, Peter L D

2009-11-01

To use advanced powder X-ray diffraction (PXRD) to characterize the structure of anhydrous theophylline following compaction, alone, and as part of a binary mixture with either alpha-lactose monohydrate or microcrystalline cellulose. Compacts formed from (1) pure theophylline and (2) each type of binary mixture were analyzed intact using PXRD. A novel mathematical technique was used to accurately separate multi-component diffraction patterns. The pair distribution function (PDF) of isolated theophylline diffraction data was employed to assess structural differences induced by consolidation and evaluated by principal components analysis (PCA). Changes induced in PXRD patterns by increasing compaction pressure were amplified by the PDF. Simulated data suggest PDF dampening is attributable to molecular deviations from average crystalline position. Samples compacted at different pressures were identified and differentiated using PCA. Samples compacted at common pressures exhibited similar inter-atomic correlations, where excipient concentration factored in the analyses involving lactose. Practical real-space structural analysis of PXRD data by PDF was accomplished for intact, compacted crystalline drug with and without excipient. PCA was used to compare multiple PDFs and successfully differentiated pattern changes consistent with compaction-induced disordering of theophylline as a single component and in the presence of another material.

Single-pulse x-ray diffraction using polycapillary optics for in situ dynamic diffraction

DOE Office of Scientific and Technical Information (OSTI.GOV)

Maddox, B. R., E-mail: maddox3@llnl.gov; Akin, M. C., E-mail: akin1@llnl.gov; Teruya, A.

2016-08-15

Diagnostic use of single-pulse x-ray diffraction (XRD) at pulsed power facilities can be challenging due to factors such as the high flux and brightness requirements for diffraction and the geometric constraints of experimental platforms. By necessity, the x-ray source is usually positioned very close, within a few inches of the sample. On dynamic compression platforms, this puts the x-ray source in the debris field. We coupled x-ray polycapillary optics to a single-shot needle-and-washer x-ray diode source using a laser-based alignment scheme to obtain high-quality x-ray diffraction using a single 16 ns x-ray pulse with the source >1 m from themore » sample. The system was tested on a Mo sample in reflection geometry using 17 keV x-rays from a Mo anode. We also identified an anode conditioning effect that increased the x-ray intensity by 180%. Quantitative measurements of the x-ray focal spot produced by the polycapillary yielded a total x-ray flux on the sample of 3.3 ± 0.5 × 10{sup 7} molybdenum Kα photons.« less

Thermal Equation of State of TiC: A Synchrotron X-ray Diffraction

DOE Office of Scientific and Technical Information (OSTI.GOV)

Yu, X.; Lin, Z; Zhang, J

2010-01-01

The pressure-volume-temperature measurements were carried out for titanium carbide (TiC) at pressures and temperatures up to 8.1 GPa and 1273 K using energy-dispersive synchrotron x-ray diffraction. Thermoelastic parameters were derived for TiC based on a modified high-temperature Birch-Murnaghan equation of state and a thermal pressure approach. With the pressure derivative of the bulk modulus, K{prime}{sub 0}, fixed at 4.0, we obtain: the ambient bulk modulus K{sub 0} = 268(6) GPa, which is comparable to previously reported value; temperature derivative of bulk modulus at constant pressure ({partial_derivative}K{sub T}/{partial_derivative}T){sub P} = -0.026(9) GPa K{sup -1}, volumetric thermal expansivity {alpha}{sub T}(K{sup -1}) =more » a+b T with a = 1.62(12) x 10{sup -5} K{sup -1} and b = 1.07(17) x 10{sup -8}K{sup -2}, pressure derivative of thermal expansion ({partial_derivative}{sub {alpha}}/{partial_derivative}{sub P}){sub T} = (-3.62 {+-} 1.14) x 10{sup -7} GPa{sup -1} K{sup -1}, and temperature derivative of bulk modulus at constant volume ({partial_derivative}K{sub T}/{partial_derivative}T){sub V} = -0.015(8) GPa K{sup -1}. These results provide fundamental thermophysical properties for TiC for the first time and are important to theoretical and computational modeling of transition metal carbides.« less

Simultaneous multiscale measurements on dynamic deformation of a magnesium alloy with synchrotron x-ray imaging and diffraction

DOE Office of Scientific and Technical Information (OSTI.GOV)

Lu, L.; Sun, T.; Fezzaa, K.

Dynamic split Hopkinson pressure bar experiments with in situ synchrotron x-ray imaging and diffraction are conducted on a rolled magnesium alloy at high strain rates of ~5500 s-1. High speed multiscale measurements including stress–strain curves (macroscale), strain fields (mesoscale), and diffraction patterns (microscale) are obtained simultaneously, revealing strong anisotropy in deformation across different length scales. {1012} extension twinning induces homogenized strain fields and gives rise to rapid increase in strain hardening rate, while dislocation motion leads to inhomogeneous deformation and a decrease in strain hardening rate. During the early stage of plastic deformation, twinning is dominant in dynamic compression, whilemore » dislocation motion prevails in quasi-static loading, manifesting a strain-rate dependence of deformation.« less

Oxidized nanocrystalline Fe-Cu pseudoalloy subjected to high pressure and electrodischarge pulses: Mössbauer and x-ray investigations

NASA Astrophysics Data System (ADS)

Gavriliuk, A. G.; Voitkovsky, V. S.; Sidorov, V. A.; Filonenko, V. P.; Tsiok, O. B.; Khvostantsev, L. G.

1998-05-01

Nanocrystalline Fe15Cu85 pseudoalloy has been subjected to pulsed heating up to 1500 K at high pressure (8 GPa). Two regimes were studied: the direct heating using electrodischarge through the sample and indirect heating with the use of cylindrical heater around the sample. The temperature and time conditions in both types of experiments were adjusted to be equivalent. The discharge parameters (stored energy, discharge time, and magnitude of current pulse) were sufficient to move defects by conduction electrons, but insufficient to melt the sample. The properties of treated samples were studied using Mössbauer absorption spectra and x-ray diffraction for three types of samples: (a) primary powder treated by high pressure up to 8 GPa, (b) powder subjected to indirect pulsed heating at 8 GPa, (c) powder treated by electrical pulses at 8 GPa. The x-ray diffraction pattern of primary powder exhibits peaks of copper, iron, and copper oxide (CuO). The Mössbauer spectrum of primary powder exhibits six peaks of alpha iron and some peaks near zero velocity due to the small iron clusters in the copper matrix and ultrafine clusters of paramagnetic phase x-Fe2O3. The transformation of CuO to Cu2O takes place in the course of indirect heating, the Mössbauer spectrum being almost unchanged. The direct electrodischarge heating causes the appearance of new magnetic phase with the magnetic field on iron nucleus 505 kOe, which corresponds to α-Fe2O3. The formation of α-Fe2O3 was confirmed by x-ray diffraction. At the same time the transformation of CuO to Cu2O is incomplete. These experiments demonstrate that high density current pulses, causing the electron wind, can be a useful tool to influence the structure of nanocrystalline powder.

X-Ray Diffraction Apparatus

NASA Technical Reports Server (NTRS)

Blake, David F. (Inventor); Bryson, Charles (Inventor); Freund, Friedmann (Inventor)

1996-01-01

An x-ray diffraction apparatus for use in analyzing the x-ray diffraction pattern of a sample is introduced. The apparatus includes a beam source for generating a collimated x-ray beam having one or more discrete x-ray energies, a holder for holding the sample to be analyzed in the path of the beam, and a charge-coupled device having an array of pixels for detecting, in one or more selected photon energy ranges, x-ray diffraction photons produced by irradiating such a sample with said beam. The CCD is coupled to an output unit which receives input information relating to the energies of photons striking each pixel in the CCD, and constructs the diffraction pattern of photons within a selected energy range striking the CCD.

The hydrothermal decomposition of calcium monosulfoaluminate 14-hydrate to katoite hydrogarnet and β-anhydrite: An in-situ synchrotron X-ray diffraction study

NASA Astrophysics Data System (ADS)

Meller, Nicola; Kyritsis, Konstantinos; Hall, Christopher

2009-10-01

We apply in-situ synchrotron X-ray diffraction to study the transformation of calcium monosulfoaluminate 14-hydrate Ca 4Al 2O 6(SO 4)·14H 2O [monosulfate-14] to hydrogarnet Ca 3Al 2(OH) 12 on the saturated water vapor pressure curve up to 250 °C. We use an aqueous slurry of synthetic ettringite Ca 6Al 2(SO 4) 3(OH) 12·26H 2O as the starting material; on heating, this decomposes at about 115 °C to form monosulfate-14 and bassanite CaSO 4·0.5H 2O. Above 170 °C monosulfate-14 diffraction peaks slowly diminish in intensity, perhaps as a result of loss of crystallinity and the formation of an X-ray amorphous meta-monosulfate. Hydrogarnet nucleates only at temperatures above 210 °C. Bassanite transforms to β-anhydrite (insoluble anhydrite) at about 230 °C and this transformation is accompanied by a second burst of hydrogarnet growth. The transformation pathway is more complex than previously thought. The mapping of the transformation pathway shows the value of rapid in-situ time-resolved synchrotron diffraction.

Probing the structure of heterogeneous diluted materials by diffraction tomography.

PubMed

Bleuet, Pierre; Welcomme, Eléonore; Dooryhée, Eric; Susini, Jean; Hodeau, Jean-Louis; Walter, Philippe

2008-06-01

The advent of nanosciences calls for the development of local structural probes, in particular to characterize ill-ordered or heterogeneous materials. Furthermore, because materials properties are often related to their heterogeneity and the hierarchical arrangement of their structure, different structural probes covering a wide range of scales are required. X-ray diffraction is one of the prime structural methods but suffers from a relatively poor detection limit, whereas transmission electron analysis involves destructive sample preparation. Here we show the potential of coupling pencil-beam tomography with X-ray diffraction to examine unidentified phases in nanomaterials and polycrystalline materials. The demonstration is carried out on a high-pressure pellet containing several carbon phases and on a heterogeneous powder containing chalcedony and iron pigments. The present method enables a non-invasive structural refinement with a weight sensitivity of one part per thousand. It enables the extraction of the scattering patterns of amorphous and crystalline compounds with similar atomic densities and compositions. Furthermore, such a diffraction-tomography experiment can be carried out simultaneously with X-ray fluorescence, Compton and absorption tomographies, enabling a multimodal analysis of prime importance in materials science, chemistry, geology, environmental science, medical science, palaeontology and cultural heritage.

DOE Office of Scientific and Technical Information (OSTI.GOV)

Zhang, Fei; Wu, Yuan; Lou, Hongbo

Polymorphism, which describes the occurrence of different lattice structures in a crystalline material, is a critical phenomenon in materials science and condensed matter physics. Recently, configuration disorder was compositionally engineered into single lattices, leading to the discovery of high-entropy alloys and high-entropy oxides. For these novel entropy-stabilized forms of crystalline matter with extremely high structural stability, is polymorphism still possible? Here by employing in situ high-pressure synchrotron radiation X-ray diffraction, we reveal a polymorphic transition from face-centred-cubic (fcc) structure to hexagonal-close-packing (hcp) structure in the prototype CoCrFeMnNi high-entropy alloy. The transition is irreversible, and our in situ high-temperature synchrotron radiationmore » X-ray diffraction experiments at different pressures of the retained hcp high-entropy alloy reveal that the fcc phase is a stable polymorph at high temperatures, while the hcp structure is more thermodynamically favourable at lower temperatures. Lastly, as pressure is increased, the critical temperature for the hcp-to-fcc transformation also rises.« less

Equations of state of anhydrous AlF3 and AlI3: Modeling of extreme condition halide chemistry

NASA Astrophysics Data System (ADS)

Stavrou, Elissaios; Zaug, Joseph M.; Bastea, Sorin; Crowhurst, Jonathan C.; Goncharov, Alexander F.; Radousky, Harry B.; Armstrong, Michael R.; Roberts, Sarah K.; Plaue, Jonathan W.

2015-06-01

Pressure dependent angle-dispersive x-ray powder diffraction measurements of alpha-phase aluminum trifluoride (α-AlF3) and separately, aluminum triiodide (AlI3) were conducted using a diamond-anvil cell. Results at 295 K extend to 50 GPa. The equations of state of AlF3 and AlI3 were determined through refinements of collected x-ray diffraction patterns. The respective bulk moduli and corresponding pressure derivatives are reported for multiple orders of the Birch-Murnaghan (B-M), finite-strain (F-f), and higher pressure finite-strain (G-g) EOS analysis models. Aluminum trifluoride exhibits an apparent isostructural phase transition at approximately 12 GPa. Aluminum triiodide also undergoes a second-order atomic rearrangement: applied stress transformed a monoclinically distorted face centered cubic (fcc) structure into a standard fcc structural arrangement of iodine atoms. Results from semi-empirical thermochemical computations of energetic materials formulated with fluorine containing reactants were obtained with the aim of predicting the yield of halogenated products.

Polymorphism in a high-entropy alloy

DOE PAGES

Zhang, Fei; Wu, Yuan; Lou, Hongbo; ...

2017-06-01

Polymorphism, which describes the occurrence of different lattice structures in a crystalline material, is a critical phenomenon in materials science and condensed matter physics. Recently, configuration disorder was compositionally engineered into single lattices, leading to the discovery of high-entropy alloys and high-entropy oxides. For these novel entropy-stabilized forms of crystalline matter with extremely high structural stability, is polymorphism still possible? Here by employing in situ high-pressure synchrotron radiation X-ray diffraction, we reveal a polymorphic transition from face-centred-cubic (fcc) structure to hexagonal-close-packing (hcp) structure in the prototype CoCrFeMnNi high-entropy alloy. The transition is irreversible, and our in situ high-temperature synchrotron radiationmore » X-ray diffraction experiments at different pressures of the retained hcp high-entropy alloy reveal that the fcc phase is a stable polymorph at high temperatures, while the hcp structure is more thermodynamically favourable at lower temperatures. Lastly, as pressure is increased, the critical temperature for the hcp-to-fcc transformation also rises.« less

Stability and melting of Fe3C at high pressure and temperature: Implication for the carbon in the Earth's core

NASA Astrophysics Data System (ADS)

Takahashi, S.; Ohtani, E.; Sakai, T.; Hirao, N.; Ohishi, Y.

2012-12-01

The Earth's core is regarded as an Fe-Ni alloy but its density is lower than that of pure Fe at the core conditions. Therefore, the Earth's core is supposed to contain light elements and carbon is one of the candidates of the light elements to explain the density deficit of the Earth's core. Nakajima et al. (2009) reported the melting temperature of Fe3C up to around 30 GPa based on textual observations, the chemical analysis of the quenched run products and in situ X-ray diffraction experiments using a Kawai-type multi anvil apparatus. Lord et al. (2009) reported melting temperatures of Fe3C up to 70 GPa, which was determined by the temperature plateau during increasing laser power using a laser-heated diamond anvil cell. They also suggested Fe+Fe7C3 is a stable subsolidus phase. There are obvious discrepancies between the melting curve and the stable subsolidus phase reported by Nakajima et al. (2009) and those reported by Lord et al. (2009). In this study, the melting temperatures of Fe3C and a subsolidus phase relation were determined based on in situ X-ray diffraction experiments. This study aims to reveal the stability field of Fe3C and the melting temperature of Fe3C and to discuss the behaviors of carbon in the Earth's core. We have performed experiments using a laser-heated diamond anvil cell combined with in situ X-ray diffraction experiment at BL10XU beamline, SPring-8 synchrotron facility. An NaCl powder and a rhenium or tungsten foil were used for the insulator and gasket, respectively. Melting of the sample was determined by disappearance of the X-ray diffraction peaks. We determined the melting relation of Fe3C up to 145 GPa by in situ X-ray diffraction experiments. Present results are close to Nakajima et al. (2009) up to 30 GPa but become close to that reported by Lord et al. (2009) at higher pressure conditions. The solidus temperature extrapolated to the ICB pressure, 330 GPa, is 5400 K. We also confirmed that Fe3C is stable as a subsolidus phase at least up to 237 GPa and 4100 K. This strongly suggests that Fe3C is a potential candidate of the Earth's inner core although we need further studies at the inner core conditions.

Real-time X-ray Diffraction: Applications to Materials Characterization

NASA Technical Reports Server (NTRS)

Rosemeier, R. G.

1984-01-01

With the high speed growth of materials it becomes necessary to develop measuring systems which also have the capabilities of characterizing these materials at high speeds. One of the conventional techniques of characterizing materials was X-ray diffraction. Film, which is the oldest method of recording the X-ray diffraction phenomenon, is not quite adequate in most circumstances to record fast changing events. Even though conventional proportional counters and scintillation counters can provide the speed necessary to record these changing events, they lack the ability to provide image information which may be important in some types of experiment or production arrangements. A selected number of novel applications of using X-ray diffraction to characterize materials in real-time are discussed. Also, device characteristics of some X-ray intensifiers useful in instantaneous X-ray diffraction applications briefly presented. Real-time X-ray diffraction experiments with the incorporation of image X-ray intensification add a new dimension in the characterization of materials. The uses of real-time image intensification in laboratory and production arrangements are quite unlimited and their application depends more upon the ingenuity of the scientist or engineer.

Advanced Spectral Analysis Program (ASAP) for High-Pressure X-ray Diffraction

NASA Astrophysics Data System (ADS)

Montgomery, Jeffrey

A program for analyzing large powder diffraction data sets has been developed. This tool enables the user to fit any type of crystal structure by indexing peaks in multiple files simultaneously by manually selecting them from a 2D plot of peak positions. The program has tools for automatic peak fitting and pressure determination using various equations of state. The interface is useful for correlating information from various types of spectral data, and so tools have been added for analyzing common fluorescence markers such as ruby, strontium tetraborate, and diamond. The program operation is demonstrated by the analysis of high-pressure powder x-ray diffraction data taken on a sample of vanadium metal at the Advanced Photon Source 16-BMD beamline. Samples were compressed in three runs to a pressure of 70 GPa in an attempt to measure the phase transition from bcc to orthorhombic in hydrostatic and non-hydrostatic conditions. Using ASAP to analyze this data provides a fast and accurate tool for observation of such a subtle transition, which is characterized primarily by a narrow splitting of the bcc 110 and 112 peaks. This work was performed under the auspices of the U.S. Department of Energy by Lawrence Livermore National Laboratory under Contract DE-AC52-07NA27344.

PSICHE: a new beamline dedicated to X-ray diffraction and tomography at high pressure at synchrotron SOLEIL

NASA Astrophysics Data System (ADS)

Guignot, N.; Itié, J.; Zerbino, P.; Delmotte, A.; Moreno, T.

2013-12-01

The PSICHE beamline (for 'Pressure, Structure and Imaging by Contrast at High Energy') is a new facility opened for high pressure experiments at synchrotron SOLEIL (St-Aubin, France). With its source, optics, detectors and 3 experimental stations, it can handle a large variety of experimental setups. High energy photons are produced with an in-vacuum wiggler. The white beam obtained, with photons energy ranging continuously from 15 to 80 keV (from a 2.75 GeV machine), is used on the first experimental station for energy dispersive X-ray diffraction (EDX) measurements using different pressure cells. The main setup is a 1200 tons load capacity multi-anvil press featuring a (100) DIA compression module with a 15° horizontal aperture, allowing measurements up to 30° in 2theta by rotating the press. Other setups are a Paris-Edinburgh (PE) large volume press and diamond anvil cells (DACs). On the detection side we have a rotating Ge detector, based on the CAESAR design described by Wang et al. (2004) (combination of EDX and angular dispersive X-ray diffraction, ADX). One of the difficulties when building such setups is the rotation mechanism which cannot be physically attached to the rotation axis, potentially leading to large circle of confusions on the horizontal position of this axis. Thanks to translation corrections done at each angle step, the circle of confusion is minimized to 3x6 μm2 along the 35° travel, making possible measurements on very small objects. Combining EDX and ADX has a lot of advantages and we will present our first results obtained using this setup. The PSICHE focusing optics and monochromator are also used to focus monochromatic beams (up to 52 keV) on 2 different experimental stations. The first focal point at 31 m gives a beam size of 100x50 μm2 (HxV) and is useful for low pressure experiments and experiments done with the PE press associated with Soller slits. A PerkinElmer flatpanel detector can be precisely scanned in 3 directions, making ADX measurements at the highest possible resolution on this beamline. This station will also be used for diffraction tomography experiments. The second focal point at 37.6 m is located behind KB mirrors on the third experimental station. 10x10 μm2 beam sizes (full width) are expected. This station will be used for DAC experiments, with or without our future laser heating setup. Finally, parallel beams can be produced with sizes up to 15x5 mm2 (HxV) for tomography experiments, in pink (filtered white) beam or monochromatic beam. We plan to use rotating anvils presses such as the rotoPEc (J. Philippe et al., 2013) to take full advantage of this beam mode, but it can be opened to other techniques. The PSICHE beamline is opened for users since July 2013. Some stations are not available yet, and will be opened through 2014 and 2015. References X. Dong et al., Ray tracing application in hard x-ray optical development: Soleil first wiggler beamline (PSICHÉ) case" (2011), Proc. SPIE 8141, 814113 Y. Wang et al., A new technique for angle-dispersive powder diffraction using an energy-dispersive setup and synchrotron radiation (2004), J. Appl. Cryst. 37, 947-956 J. Philippe, Y. Le Godec, F. Bergame et M. Morand, Patent INPI 11 62335 (2013)

Radiation damage free ghost diffraction with atomic resolution

DOE PAGES

Li, Zheng; Medvedev, Nikita; Chapman, Henry N.; ...

2017-12-21

The x-ray free electron lasers can enable diffractive structural determination of protein nanocrystals and single molecules that are too small and radiation-sensitive for conventional x-ray diffraction. However the electronic form factor may be modified during the ultrashort x-ray pulse due to photoionization and electron cascade caused by the intense x-ray pulse. For general x-ray imaging techniques, the minimization of the effects of radiation damage is of major concern to ensure reliable reconstruction of molecular structure. Here in this paper, we show that radiation damage free diffraction can be achieved with atomic spatial resolution by using x-ray parametric down-conversion and ghostmore » diffraction with entangled photons of x-ray and optical frequencies. We show that the formation of the diffraction patterns satisfies a condition analogous to the Bragg equation, with a resolution that can be as fine as the crystal lattice length scale of several Ångstrom. Since the samples are illuminated by low energy optical photons, they can be free of radiation damage.« less

Radiation damage free ghost diffraction with atomic resolution

DOE Office of Scientific and Technical Information (OSTI.GOV)

Li, Zheng; Medvedev, Nikita; Chapman, Henry N.

The x-ray free electron lasers can enable diffractive structural determination of protein nanocrystals and single molecules that are too small and radiation-sensitive for conventional x-ray diffraction. However the electronic form factor may be modified during the ultrashort x-ray pulse due to photoionization and electron cascade caused by the intense x-ray pulse. For general x-ray imaging techniques, the minimization of the effects of radiation damage is of major concern to ensure reliable reconstruction of molecular structure. Here in this paper, we show that radiation damage free diffraction can be achieved with atomic spatial resolution by using x-ray parametric down-conversion and ghostmore » diffraction with entangled photons of x-ray and optical frequencies. We show that the formation of the diffraction patterns satisfies a condition analogous to the Bragg equation, with a resolution that can be as fine as the crystal lattice length scale of several Ångstrom. Since the samples are illuminated by low energy optical photons, they can be free of radiation damage.« less

Synchrotron Radiation X-ray Diffraction Techniques Applied to Insect Flight Muscle.

PubMed

Iwamoto, Hiroyuki

2018-06-13

X-ray fiber diffraction is a powerful tool used for investigating the molecular structure of muscle and its dynamics during contraction. This technique has been successfully applied not only to skeletal and cardiac muscles of vertebrates but also to insect flight muscle. Generally, insect flight muscle has a highly ordered structure and is often capable of high-frequency oscillations. The X-ray diffraction studies on muscle have been accelerated by the advent of 3rd-generation synchrotron radiation facilities, which can generate brilliant and highly oriented X-ray beams. This review focuses on some of the novel experiments done on insect flight muscle by using synchrotron radiation X-rays. These include diffraction recordings from single myofibrils within a flight muscle fiber by using X-ray microbeams and high-speed diffraction recordings from the flight muscle during the wing-beat of live insects. These experiments have provided information about the molecular structure and dynamic function of flight muscle in unprecedented detail. Future directions of X-ray diffraction studies on muscle are also discussed.

Effect of chemical pressure on the electronic phase transition in Ca 1-x Sr x Mn 7 O 12 films

DOE Office of Scientific and Technical Information (OSTI.GOV)

Huon, A.; Lee, D.; Herklotz, A.

Here, we demonstrate how chemical pressure affects the structural and electronic phase transitions of the quadruple perovskite CaMn 7O 12 by Sr doping, a compound that exhibits a charge-ordering transition above room temperature making it a candidate for oxide electronics. We also have synthesized Ca 1-xSr xMn 7O 12 (0 ≤ x ≤ 0.6) thin films by oxide molecular beam epitaxy on (LaAlO 3) 0.3(SrAl 0.5Ta 0.5O 3) 0.7 (LSAT) substrates. The substitution of Sr for Ca results in a linear expansion of the lattice, as revealed by X-ray diffraction. Temperature-dependent resistivity and X-ray diffraction measurements are used to demonstratemore » that the coupled charge-ordering and structural phase transitions can be tuned with Sr doping. An increase in Sr concentration acts to decrease the phase transition temperature (T*) from 426 K at x = 0 to 385 K at x = 0.6. Furthemore, the presence of a tunable electronic phase transition, above room temperature, points to the potential applicability of Ca 1-xSr xMn 7O 12 in sensors or oxide electronics, for example, via charge doping.« less

Effect of chemical pressure on the electronic phase transition in Ca 1-x Sr x Mn 7 O 12 films

DOE PAGES

Huon, A.; Lee, D.; Herklotz, A.; ...

2017-09-18

Here, we demonstrate how chemical pressure affects the structural and electronic phase transitions of the quadruple perovskite CaMn 7O 12 by Sr doping, a compound that exhibits a charge-ordering transition above room temperature making it a candidate for oxide electronics. We also have synthesized Ca 1-xSr xMn 7O 12 (0 ≤ x ≤ 0.6) thin films by oxide molecular beam epitaxy on (LaAlO 3) 0.3(SrAl 0.5Ta 0.5O 3) 0.7 (LSAT) substrates. The substitution of Sr for Ca results in a linear expansion of the lattice, as revealed by X-ray diffraction. Temperature-dependent resistivity and X-ray diffraction measurements are used to demonstratemore » that the coupled charge-ordering and structural phase transitions can be tuned with Sr doping. An increase in Sr concentration acts to decrease the phase transition temperature (T*) from 426 K at x = 0 to 385 K at x = 0.6. Furthemore, the presence of a tunable electronic phase transition, above room temperature, points to the potential applicability of Ca 1-xSr xMn 7O 12 in sensors or oxide electronics, for example, via charge doping.« less

Phase diagram of the Pr-Mn-O system in composition-temperature-oxygen pressure coordinates

NASA Astrophysics Data System (ADS)

Vedmid', L. B.; Yankin, A. M.; Fedorova, O. M.; Kozin, V. M.

2016-05-01

The phase relations in the Pr-Mn-O system were studied by the static method at lowered oxygen pressure in combination with thermal analysis and high-temperature X-ray diffraction. The equilibrium oxygen pressure in dissociation of PrMn2O5 and PrMnO3 was measured, and the thermodynamic characteristics of formation of these compounds from elements were calculated. The P- T- x phase diagram of the Pr-Mn-O system was constructed in the "composition-oxygen pressure-temperature" coordinates.

In situ X-ray ptychography imaging of high-temperature CO{sub 2} acceptor particle agglomerates

DOE Office of Scientific and Technical Information (OSTI.GOV)

Høydalsvik, Kristin; Bø Fløystad, Jostein; Esmaeili, Morteza

2014-06-16

Imaging nanoparticles under relevant reaction conditions of high temperature and gas pressure is difficult because conventional imaging techniques, like transmission electron microscopy, cannot be used. Here we demonstrate that the coherent diffractive imaging technique of X-ray ptychography can be used for in situ phase contrast imaging in structure studies at atmospheric pressure and elevated temperatures. Lithium zirconate, a candidate CO{sub 2} capture material, was studied at a pressure of one atmosphere in air and in CO{sub 2}, at temperatures exceeding 600 °C. Images with a spatial resolution better than 200 nm were retrieved, and possibilities for improving the experiment are described.

Observation of an Ultrahard Phase of Graphite Quenched from High-pressure

DTIC Science & Technology

2011-02-01

Polycrystalline NaCl at High Pressures and 300 °K. J. Geophys. Res. 1978, 83, 1257–1268. 23. Selvi , E.; Ma, Y.; Askoy, R.; Ertas, A.; White, A. High...Pressure X-ray Diffraction Study of Tungsten Disulfide. J. Phys. Chem. Solids 2006, 67, 2183–2186. 24. Askoy, R.; Ma, Y.; Selvi , E.; Chyu, M. C

High-pressure phase transition and phase diagram of gallium arsenide

NASA Astrophysics Data System (ADS)

Besson, J. M.; Itié, J. P.; Polian, A.; Weill, G.; Mansot, J. L.; Gonzalez, J.

1991-09-01

Under hydrostatic pressure, cubic GaAs-I undergoes phase transitions to at least two orthorhombic structures. The initial phase transition to GaAs-II has been investigated by optical-transmittance measurements, Raman scattering, and x-ray absorption. The structure of pressurized samples, which are retrieved at ambient, has been studied by x-ray diffraction and high-resolution diffraction microscopy. Various criteria that define the domain of stability of GaAs-I are examined, such as the occurrence of crystalline defects, the local variation in atomic coordination number, or the actual change in crystal structure. These are shown not to occur at the same pressure at 300 K, the latter being observable only several GPa above the actual thermodynamic instability pressure of GaAs-I. Comparison of the evolution of these parameters on increasing and decreasing pressure locates the thermodynamic transition region GaAs-I-->GaAs-II at 12+/-1.5 GPa and at 300 K that is lower than generally reported. The use of thermodynamic relations around the triple point, and of regularities in the properties of isoelectronic and isostructural III-V compounds, yields a phase diagram for GaAs which is consistent with this value.

Externally controlled pressure and temperature microreactor for in situ x-ray diffraction, visual and spectroscopic reaction investigations under supercritical and subcritical conditions

DOE Office of Scientific and Technical Information (OSTI.GOV)

Diefenbacher, Jason; McKelvy, Michael; Chizmeshya, Andrew V.G.

2005-01-01

A microreactor has been developed for in situ, spectroscopic investigations of materials and reaction processes with full external pressure and temperature control from ambient conditions to 400 deg. C and 310 bar. The sample chamber is in direct contact with an external manifold, whereby gases, liquids or fluids can be injected and their activities controlled prior to and under investigation conditions. The microreactor employs high strength, single crystal moissanite windows which allow direct probe beam interaction with a sample to investigate in situ reaction processes and other materials properties. The relatively large volume of the cell, along with full opticalmore » accessibility and external temperature and pressure control, make this reaction cell well suited for experimental investigations involving any combination of gas, fluid, and solid interactions. The microreactor's capabilities are demonstrated through an in situ x-ray diffraction study of the conversion of a meta-serpentine sample to magnesite under high pressure and temperature. Serpentine is one of the mineral candidates for the implementation of mineral carbonation, an intriguing carbon sequestration candidate technology.« less

Externally controlled pressure and temperature microreactor for in situ x-ray diffraction, visual and spectroscopic reaction investigations under supercritical and subcritial conditions

DOE Office of Scientific and Technical Information (OSTI.GOV)

Diefenbacher, J.; McKelvy, M.; Chizemeshya, A.V.

2010-07-13

A microreactor has been developed for in situ, spectroscopic investigations of materials and reaction processes with full external pressure and temperature control from ambient conditions to 400 C and 310 bar. The sample chamber is in direct contact with an external manifold, whereby gases, liquids or fluids can be injected and their activities controlled prior to and under investigation conditions. The microreactor employs high strength, single crystal moissanite windows which allow direct probe beam interaction with a sample to investigate in situ reaction processes and other materials properties. The relatively large volume of the cell, along with full optical accessibilitymore » and external temperature and pressure control, make this reaction cell well suited for experimental investigations involving any combination of gas, fluid, and solid interactions. The microreactor's capabilities are demonstrated through an in situ x-ray diffraction study of the conversion of a meta-serpentine sample to magnesite under high pressure and temperature. Serpentine is one of the mineral candidates for the implementation of mineral carbonation, an intriguing carbon sequestration candidate technology.« less

Combining experiment and optical simulation in coherent X-ray nanobeam characterization of Si/SiGe semiconductor heterostructures

DOE PAGES

Tilka, J. A.; Park, J.; Ahn, Y.; ...

2016-07-06

Here, the highly coherent and tightly focused x-ray beams produced by hard x-ray light sources enable the nanoscale characterization of the structure of electronic materials but are accompanied by significant challenges in the interpretation of diffraction and scattering patterns. X-ray nanobeams exhibit optical coherence combined with a large angular divergence introduced by the x-ray focusing optics. The scattering of nanofocused x-ray beams from intricate semiconductor heterostructures produces a complex distribution of scattered intensity. We report here an extension of coherent xray optical simulations of convergent x-ray beam diffraction patterns to arbitrary x-ray incident angles to allow the nanobeam diffraction patternsmore » of complex heterostructures to be simulated faithfully. These methods are used to extract the misorientation of lattice planes and the strain of individual layers from synchrotron x-ray nanobeam diffraction patterns of Si/SiGe heterostructures relevant to applications in quantum electronic devices. The systematic interpretation of nanobeam diffraction patterns from semiconductor heterostructures presents a new opportunity in characterizing and ultimately designing electronic materials.« less

X-ray diffraction investigation of amorphous calcium phosphate and hydroxyapatite under ultra-high hydrostatic pressure

NASA Astrophysics Data System (ADS)

Lam, Elisa; Gu, Qinfen; Swedlund, Peter J.; Marchesseau, Sylvie; Hemar, Yacine

2015-11-01

The changes in the crystal structures of synthetically prepared amorphous calcium phosphate (ACP) and hydroxyapatite (HAP) in water (1:1 mass ratio) were studied by synchrotron X-ray diffraction (XRD) under ultra-high hydrostatic pressures as high as 2.34 GPa for ACP and 4 GPa for HAP. At ambient pressure, the XRD patterns of the ACP and HAP samples in capillary tubes and their environmental scanning electron micrographs indicated amorphous and crystalline characteristics for ACP and HAP, respectively. At pressures greater than 0.25 GPa, an additional broad peak was observed in the XRD pattern of the ACP phase, indicating a partial phase transition from an amorphous phase to a new high-pressure amorphous phase. The peak areas and positions of the ACP phase, as obtained through fitting of the experimental data, indicated that the ACP exhibited increased pseudo-crystalline behavior at pressures greater than 0.96 GPa. Conversely, no structural changes were observed for the HAP phase up to the highest applied pressure of 4 GPa. For HAP, a unit-cell reduction during compression was evidenced by a reduction in both refined lattice parameters a and c. Both ACP and HAP reverted to their original structures when the pressure was fully released to ambient pressure.

High-Pressure Polymorph of NaBiO3.

PubMed

Naa, Octavianti; Kumada, Nobuhiro; Miura, Akira; Takei, Takahiro; Azuma, Masaki; Kusano, Yoshihiro; Oka, Kengo

2016-06-20

A new high-pressure polymorph of NaBiO3 (hereafter β-NaBiO3) was synthesized under the conditions of 6 GPa and 600 °C. The powder X-ray diffraction pattern of this new phase was indexed with a hexagonal cell of a = 9.968(1) Å and c = 3.2933(4) Å. Crystal structure refinement using synchrotron powder X-ray diffraction data led to RWP = 8.53% and RP = 5.55%, and the crystal structure was closely related with that of Ba2SrY6O12. No photocatalytic activity for phenol decomposition was observed under visible-light irradiation in spite of a good performance for its mother compound, NaBiO3. The optical band-gap energy of β-NaBiO3 was narrower than that of NaBiO3, which was confirmed with density of states curves simulated by first-principles density functional theory calculation.

Positron annihilation and X-ray diffraction studies on tin oxide thin films

NASA Astrophysics Data System (ADS)

Prabakar, K.; Abhaya, S.; Krishnan, R.; Kalavathi, S.; Dash, S.; Jayapandian, J.; Amarendra, G.

2009-04-01

Positron annihilation spectroscopy along with glancing incidence X-ray diffraction have been used to investigate tin oxide thin films grown on Si by pulsed laser deposition. The films were prepared at room temperature and at 670 K under oxygen partial pressure. As-grown samples are amorphous and are found to contain large concentration of open volume sites (vacancy defects). Post-deposition annealing of as-grown samples at 970 K is found to drastically reduce the number of open volume sites and the film becomes crystalline. However, film grown under elevated temperature and under partial pressure of oxygen is found to exhibit a lower S-parameter, indicating lower defect concentration. Based on the analysis of experimental positron annihilation results, the defect-sensitive S-parameter and the overlayer thickness of tin oxide thin films are deduced. S- W correlation plots exhibit distinct positron trapping defect states in three samples.

Conducting linear chains of sulphur inside carbon nanotubes

PubMed Central

Fujimori, Toshihiko; Morelos-Gómez, Aarón; Zhu, Zhen; Muramatsu, Hiroyuki; Futamura, Ryusuke; Urita, Koki; Terrones, Mauricio; Hayashi, Takuya; Endo, Morinobu; Young Hong, Sang; Chul Choi, Young; Tománek, David; Kaneko, Katsumi

2013-01-01

Despite extensive research for more than 200 years, the experimental isolation of monatomic sulphur chains, which are believed to exhibit a conducting character, has eluded scientists. Here we report the synthesis of a previously unobserved composite material of elemental sulphur, consisting of monatomic chains stabilized in the constraining volume of a carbon nanotube. This one-dimensional phase is confirmed by high-resolution transmission electron microscopy and synchrotron X-ray diffraction. Interestingly, these one-dimensional sulphur chains exhibit long domain sizes of up to 160 nm and high thermal stability (~800 K). Synchrotron X-ray diffraction shows a sharp structural transition of the one-dimensional sulphur occurring at ~450–650 K. Our observations, and corresponding electronic structure and quantum transport calculations, indicate the conducting character of the one-dimensional sulphur chains under ambient pressure. This is in stark contrast to bulk sulphur that needs ultrahigh pressures exceeding ~90 GPa to become metallic. PMID:23851903

Automated X-Ray Diffraction of Irradiated Materials

DOE PAGES

Rodman, John; Lin, Yuewei; Sprouster, David; ...

2017-10-26

Synchrotron-based X-ray diffraction (XRD) and small-angle Xray scattering (SAXS) characterization techniques used on unirradiated and irradiated reactor pressure vessel steels yield large amounts of data. Machine learning techniques, including PCA, offer a novel method of analyzing and visualizing these large data sets in order to determine the effects of chemistry and irradiation conditions on the formation of radiation induced precipitates. In order to run analysis on these data sets, preprocessing must be carried out to convert the data to a usable format and mask the 2-D detector images to account for experimental variations. Once the data has been preprocessed, itmore » can be organized and visualized using principal component analysis (PCA), multi-dimensional scaling, and k-means clustering. In conclusion, from these techniques, it is shown that sample chemistry has a notable effect on the formation of the radiation induced precipitates in reactor pressure vessel steels.« less

Modeling and measurements of XRD spectra of extended solids under high pressure

NASA Astrophysics Data System (ADS)

Batyrev, I. G.; Coleman, S. P.; Stavrou, E.; Zaug, J. M.; Ciezak-Jenkins, J. A.

2017-06-01

We present results of evolutionary simulations based on density functional calculations of various extended solids: N-Si and N-H using variable and fixed concentration methods of USPEX. Predicted from the evolutionary simulations structures were analyzed in terms of thermo-dynamical stability and agreement with experimental X-ray diffraction spectra. Stability of the predicted system was estimated from convex-hull plots. X-ray diffraction spectra were calculated using a virtual diffraction algorithm which computes kinematic diffraction intensity in three-dimensional reciprocal space before being reduced to a two-theta line profile. Calculations of thousands of XRD spectra were used to search for a structure of extended solids at certain pressures with best fits to experimental data according to experimental XRD peak position, peak intensity and theoretically calculated enthalpy. Comparison of Raman and IR spectra calculated for best fitted structures with available experimental data shows reasonable agreement for certain vibration modes. Part of this work was performed by LLNL, Contract DE-AC52-07NA27344. We thank the Joint DoD / DOE Munitions Technology Development Program, the HE C-II research program at LLNL and Advanced Light Source, supported by BES DOE, Contract No. DE-AC02-05CH112.

Synchrotron powder X-ray diffraction and structural analysis of Eu0.5La0.5FBiS2-x Se x

NASA Astrophysics Data System (ADS)

Nagasaka, K.; Jinno, G.; Miura, O.; Miura, A.; Moriyoshi, C.; Kuroiwa, Y.; Mizuguchi, Y.

2017-07-01

Eu0.5La0.5FBiS2-x Se x is a new BiS2-based superconductor system. In Eu0.5La0.5FBiS2-x Se x , electron carriers are doped to the BiS2 layer by the substitution of Eu by La. Bulk superconductivity in this system is induced by increasing the in-plane chemical pressure, which is controlled by the Se concentration (x). In this study, we have analysed the crystal structure of Eu0.5La0.5FBiS2-x Se x using synchrotron powder diffraction and the Rietveld refinement. The precise determination of the structural parameters and thermal factors suggest that the emergence of bulk superconductivity in Eu0.5La0.5FBiS2-x Se x is achieved by the enhanced in-plane chemical pressure and the decrease in in-plane disorder.

Fabrication and testing of a newly designed slit system for depth-resolved X-ray diffraction measurements

DOE PAGES

Sinsheimer, John; Bouet, Nathalie; Ghose, Sanjit; ...

2016-10-06

A new system of slits called `spiderweb slits' have been developed for depth-resolved powder or polycrystalline X-ray diffraction measurements. The slits act on diffracted X-rays to select a particular gauge volume of sample, while absorbing diffracted X-rays from outside of this volume. Although the slit geometry is to some extent similar to that of previously developed conical slits or spiral slits, this new design has advantages over the previous ones in use for complex heterogeneous materials and in situ and operando diffraction measurements. For example, the slits can measure a majority of any diffraction cone for any polycrystalline material, overmore » a continuous range of diffraction angles, and work for X-ray energies of tens to hundreds of kiloelectronvolts. In addition, the design is generated and optimized using ray-tracing simulations, and fabricated through laser micromachining. The first prototype was successfully tested at the X17A beamline at the National Synchrotron Light Source, and shows similar performance to simulations, demonstrating gauge volume selection for standard powders, for all diffraction peaks over angles of 2–10°. A similar, but improved, design will be implemented at the X-ray Powder Diffraction beamline at the National Synchrotron Light Source II.« less

Increasing dissolution of trospium chloride by co-crystallization with urea

NASA Astrophysics Data System (ADS)

Skořepová, Eliška; Hušák, Michal; Čejka, Jan; Zámostný, Petr; Kratochvíl, Bohumil

2014-08-01

The search for various solid forms of an active pharmaceutical ingredient (API) is an important step in drug development. Our aim was to prepare co-crystals of trospium chloride, an anticholinergic drug used for the treatment of incontinence, and to investigate if they have advantageous properties for drug formulation. Phase identification was done by powder X-ray diffraction and single-crystal X-ray diffraction. The chemical composition was verified by solution NMR and the dissolution rate of the prepared phases was studied by IDR (intrinsic dissolution rate). For further analysis of phase stability and transitions, combined thermal analysis and temperature-resolved X-ray powder diffraction were used. Urea was selected as a co-crystallization partner. Trospium chloride urea (1:1) co-crystal was prepared by a solvent evaporation. From single-crystal data, the co-crystal structure was solved in a space group P21/c and compared to previously published structures of trospium chloride. Intrinsic dissolution rate revealed that the co-crystal dissolves 32% faster than pure API. However, its low thermal and pressure stability makes it a challenging choice for the final drug formulation.

Direct Observations of a Dynamically Driven Phase Transition with in situ X-Ray Diffraction in a Simple Ionic Crystal

NASA Astrophysics Data System (ADS)

Kalita, Patricia; Specht, Paul; Root, Seth; Sinclair, Nicholas; Schuman, Adam; White, Melanie; Cornelius, Andrew L.; Smith, Jesse; Sinogeikin, Stanislav

2017-12-01

We report real-time observations of a phase transition in the ionic solid CaF2 , a model A B2 structure in high-pressure physics. Synchrotron x-ray diffraction coupled with dynamic loading to 27.7 GPa, and separately with static compression, follows, in situ, the fluorite to cotunnite structural phase transition, both on nanosecond and on minute time scales. Using Rietveld refinement techniques, we examine the kinetics and hysteresis of the transition. Our results give insight into the kinetic time scale of the fluorite-cotunnite phase transition under shock compression, which is relevant to a number of isomorphic compounds.

High-temperature/high-pressure x-ray diffraction: Recent developments

DOE Office of Scientific and Technical Information (OSTI.GOV)

Schiferl, D.; Johnson, S.W.; Zinn, A.S.

1989-01-01

We have developed two Merrill-Bassett diamond-anvil cells for specialized high-temperature uses. The first is constructed largely of rhenium to provide uniform, constant P and T on the order of 20 GPa at 1200 K for extended periods. The second is for single-crystal x-ray diffraction, but can be heated to 630 K at 20 GPa to grow single-crystal samples which cannot be produced at room temperature. With this cell, the crystal structure of /var epsilon/-O/sub 2/ was shown to be monoclinic with a = 3.649 A, b = 5.493 A, c = 7.701 A, and /Beta/ = 116.11/degree/ at 19.7 GPa.more » 15 refs.« less

Direct Observations of a Dynamically Driven Phase Transition with in situ X-Ray Diffraction in a Simple Ionic Crystal

DOE PAGES

Kalita, Patricia E.; Specht, Paul Elliot; Root, Seth; ...

2017-12-21

Here, we report real-time observations of a phase transition in the ionic solid CaF 2, a model AB 2 structure in high-pressure physics. Synchrotron x-ray diffraction coupled with dynamic loading to 27.7 GPa, and separately with static compression, follows, in situ, the fluorite to cotunnite structural phase transition, both on nanosecond and on minute time scales. Using Rietveld refinement techniques, we examine the kinetics and hysteresis of the transition. Our results give insight into the kinetic time scale of the fluorite-cotunnite phase transition under shock compression, which is relevant to a number of isomorphic compounds.

Dynamical scattering in coherent hard x-ray nanobeam Bragg diffraction

NASA Astrophysics Data System (ADS)

Pateras, A.; Park, J.; Ahn, Y.; Tilka, J. A.; Holt, M. V.; Kim, H.; Mawst, L. J.; Evans, P. G.

2018-06-01

Unique intensity features arising from dynamical diffraction arise in coherent x-ray nanobeam diffraction patterns of crystals having thicknesses larger than the x-ray extinction depth or exhibiting combinations of nanoscale and mesoscale features. We demonstrate that dynamical scattering effects can be accurately predicted using an optical model combined with the Darwin theory of dynamical x-ray diffraction. The model includes the highly divergent coherent x-ray nanobeams produced by Fresnel zone plate focusing optics and accounts for primary extinction, multiple scattering, and absorption. The simulation accurately reproduces the dynamical scattering features of experimental diffraction patterns acquired from a GaAs/AlGaAs epitaxial heterostructure on a GaAs (001) substrate.

Coherent x-ray diffraction imaging with nanofocused illumination.

PubMed

Schroer, C G; Boye, P; Feldkamp, J M; Patommel, J; Schropp, A; Schwab, A; Stephan, S; Burghammer, M; Schöder, S; Riekel, C

2008-08-29

Coherent x-ray diffraction imaging is an x-ray microscopy technique with the potential of reaching spatial resolutions well beyond the diffraction limits of x-ray microscopes based on optics. However, the available coherent dose at modern x-ray sources is limited, setting practical bounds on the spatial resolution of the technique. By focusing the available coherent flux onto the sample, the spatial resolution can be improved for radiation-hard specimens. A small gold particle (size <100 nm) was illuminated with a hard x-ray nanobeam (E=15.25 keV, beam dimensions approximately 100 x 100 nm2) and is reconstructed from its coherent diffraction pattern. A resolution of about 5 nm is achieved in 600 s exposure time.

DynAMITe: a prototype large area CMOS APS for breast cancer diagnosis using x-ray diffraction measurements

NASA Astrophysics Data System (ADS)

Konstantinidis, A.; Anaxagoras, T.; Esposito, M.; Allinson, N.; Speller, R.

2012-03-01

X-ray diffraction studies are used to identify specific materials. Several laboratory-based x-ray diffraction studies were made for breast cancer diagnosis. Ideally a large area, low noise, linear and wide dynamic range digital x-ray detector is required to perform x-ray diffraction measurements. Recently, digital detectors based on Complementary Metal-Oxide- Semiconductor (CMOS) Active Pixel Sensor (APS) technology have been used in x-ray diffraction studies. Two APS detectors, namely Vanilla and Large Area Sensor (LAS), were developed by the Multidimensional Integrated Intelligent Imaging (MI-3) consortium to cover a range of scientific applications including x-ray diffraction. The MI-3 Plus consortium developed a novel large area APS, named as Dynamically Adjustable Medical Imaging Technology (DynAMITe), to combine the key characteristics of Vanilla and LAS with a number of extra features. The active area (12.8 × 13.1 cm2) of DynaMITe offers the ability of angle dispersive x-ray diffraction (ADXRD). The current study demonstrates the feasibility of using DynaMITe for breast cancer diagnosis by identifying six breast-equivalent plastics. Further work will be done to optimize the system in order to perform ADXRD for identification of suspicious areas of breast tissue following a conventional mammogram taken with the same sensor.

X-ray diffraction and reflectivity validation of the depletion attraction in the competitive adsorption of lung surfactant and albumin.

PubMed

Stenger, Patrick C; Wu, Guohui; Miller, Chad E; Chi, Eva Y; Frey, Shelli L; Lee, Ka Yee C; Majewski, Jaroslaw; Kjaer, Kristian; Zasadzinski, Joseph A

2009-08-05

Lung surfactant (LS) and albumin compete for the air-water interface when both are present in solution. Equilibrium favors LS because it has a lower equilibrium surface pressure, but the smaller albumin is kinetically favored by faster diffusion. Albumin at the interface creates an energy barrier to subsequent LS adsorption that can be overcome by the depletion attraction induced by polyethylene glycol (PEG) in solution. A combination of grazing incidence x-ray diffraction (GIXD), x-ray reflectivity (XR), and pressure-area isotherms provides molecular-resolution information on the location and configuration of LS, albumin, and polymer. XR shows an average electron density similar to that of albumin at low surface pressures, whereas GIXD shows a heterogeneous interface with coexisting LS and albumin domains at higher surface pressures. Albumin induces a slightly larger lattice spacing and greater molecular tilt, similar in effect to a small decrease in the surface pressure. XR shows that adding PEG to the LS-albumin subphase restores the characteristic LS electron density profile at the interface, and confirms that PEG is depleted near the interface. GIXD shows the same LS Bragg peaks and Bragg rods as on a pristine interface, but with a more compact lattice corresponding to a small increase in the surface pressure. These results confirm that albumin adsorption creates a physical barrier that inhibits LS adsorption, and that PEG in the subphase generates a depletion attraction between the LS aggregates and the interface that enhances LS adsorption without substantially altering the structure or properties of the LS monolayer.

Resolution enhancement in coherent x-ray diffraction imaging by overcoming instrumental noise.

PubMed

Kim, Chan; Kim, Yoonhee; Song, Changyong; Kim, Sang Soo; Kim, Sunam; Kang, Hyon Chol; Hwu, Yeukuang; Tsuei, Ku-Ding; Liang, Keng San; Noh, Do Young

2014-11-17

We report that reference objects, strong scatterers neighboring weak phase objects, enhance the phase retrieval and spatial resolution in coherent x-ray diffraction imaging (CDI). A CDI experiment with Au nano-particles exhibited that the reference objects amplified the signal-to-noise ratio in the diffraction intensity at large diffraction angles, which significantly enhanced the image resolution. The interference between the diffracted x-ray from reference objects and a specimen also improved the retrieval of the phase of the diffraction signal. The enhancement was applied to image NiO nano-particles and a mitochondrion and confirmed in a simulation with a bacteria phantom. We expect that the proposed method will be of great help in imaging weakly scattering soft matters using coherent x-ray sources including x-ray free electron lasers.

Measuring twinning and slip in shock-compressed Ta from in-situ x-ray diffraction

NASA Astrophysics Data System (ADS)

Wehrenberg, Christopher; McGonegle, David; Sliwa, Marcin; Suggit, Matt; Wark, Justin; Lee, Hae Ja; Nagler, Bob; Tavella, Franz; Remington, Bruce; Rudd, Rob; Lazicki, Amy; Park, Hye-Sook; Swift, Damian; Zepeda-Ruiz, Louis; Higginbotham, Andrew; Bolme, Cindy

2017-06-01

A fundamental understanding of high-pressure and high-strain-rate deformation rests on grasping the underlying microstructural processes, such as twinning and dislocation generation and transport (slip), yet simulations and ex-post-facto recovery experiments provide conflicting answers to these basic issues. Here, we report direct, in-situ observation of twinning and slip in shock compressed Ta using in-situ x-ray diffraction. A series of shock experiments were performed on the Matter in Extreme Conditions end station at LCLS. Direct laser ablation was used to drive a shock, ranging in pressure from 10-300 GPa, into a Ta sample with an initial (110) fiber texture. The subsequent changes in texture were observed in-situ by examining the azimuthal distribution of the diffraction intensity and found to match twinning and lattice rotation. Measurements of the twin fraction and lattice rotation were used to calculate the equivalent plastic strain from twinning and slip. This work was performed under the auspices of the U.S. Department of Energy by Lawrence Livermore National Laboratory under Contract No. DE-AC52-07NA27344.

XRD and XAS structural study of CuAlO2 under high pressure.

PubMed

Pellicer-Porres, J; Segura, A; Ferrer-Roca, Ch; Polian, A; Munsch, P; Kim, D

2013-03-20

We present the results of x-ray diffraction and x-ray absorption spectroscopy experiments in CuAlO(2) under high pressure. We discuss the polarization dependence of the x-ray absorption near-edge structure at the Cu K-edge. XRD under high pressure evidences anisotropic compression, the a-axis being more compressible than the c-axis. EXAFS yields the copper-oxygen bond length, from which the only internal parameter of the delafossite structure is deduced. The combination of anisotropic compression and the internal parameter decrease results in a regularization of the AlO(6) octahedra. The anisotropic compression is related to the chemical trends observed in the lattice parameters when Al is substituted by other trivalent cations. Both experiments evidence the existence of an irreversible phase transition that clearly manifests at 35 ± 2 GPa. The structure of the high-pressure polymorph could not be determined, but it implies a change of the Cu environment, which remains anisotropic. Precursor effects are observed from the lowest pressures, which are possibly related to crystal breaking at a submicroscopic scale with partial reorientation of the crystallites.

XRD and XAS structural study of CuAlO2 under high pressure

NASA Astrophysics Data System (ADS)

Pellicer-Porres, J.; Segura, A.; Ferrer-Roca, Ch; Polian, A.; Munsch, P.; Kim, D.

2013-03-01

We present the results of x-ray diffraction and x-ray absorption spectroscopy experiments in CuAlO2 under high pressure. We discuss the polarization dependence of the x-ray absorption near-edge structure at the Cu K-edge. XRD under high pressure evidences anisotropic compression, the a-axis being more compressible than the c-axis. EXAFS yields the copper-oxygen bond length, from which the only internal parameter of the delafossite structure is deduced. The combination of anisotropic compression and the internal parameter decrease results in a regularization of the AlO6 octahedra. The anisotropic compression is related to the chemical trends observed in the lattice parameters when Al is substituted by other trivalent cations. Both experiments evidence the existence of an irreversible phase transition that clearly manifests at 35 ± 2 GPa. The structure of the high-pressure polymorph could not be determined, but it implies a change of the Cu environment, which remains anisotropic. Precursor effects are observed from the lowest pressures, which are possibly related to crystal breaking at a submicroscopic scale with partial reorientation of the crystallites.

Self catalytic growth of indium oxide (In2O3) nanowires by resistive thermal evaporation.

PubMed

Kumar, R Rakesh; Rao, K Narasimha; Rajanna, K; Phani, A R

2014-07-01

Self catalytic growth of Indium Oxide (In2O3) nanowires (NWs) have been grown by resistive thermal evaporation of Indium (In) in the presence of oxygen without use of any additional metal catalyst. Nanowires growth took place at low substrate temperature of 370-420 degrees C at an applied current of 180-200 A to the evaporation boat. Morphology, microstructures, and compositional studies of the grown nanowires were performed by employing field emission scanning electron microscopy (FESEM), X-Ray diffraction (XRD), transmission electron microscopy (TEM), energy dispersive X-ray spectroscopy (EDS) and X-ray photoelectron spectroscopy (XPS) respectively. Nanowires were uniformly grown over the entire Si substrate and each of the nanowire is capped with a catalyst particle at their end. X-ray diffraction study reveals the crystalline nature of the grown nanowires. Transmission electron microscopy study on the nanowires further confirmed the single crystalline nature of the nanowires. Energy dispersive X-ray analysis on the nanowires and capped nanoparticle confirmed that Indium act as catalyst for In2O3 nanowires growth. A self catalytic Vapor-Liquid-Solid (VLS) growth mechanism was responsible for the growth of In2O3 nanowires. Effect of oxygen partial pressure variation and variation of applied currents to the evaporation boat on the nanowires growth was systematically studied. These studies concluded that at oxygen partial pressure in the range of 4 x 10(-4), 6 x 10(-4) mbar at applied currents to the evaporation boat of 180-200 A were the best conditions for good nanowires growth. Finally, we observed another mode of VLS growth along with the standard VLS growth mode for In2O3 nanowires similar to the growth mechanism reported for GaAs nanowires.

Fabrication and testing of a newly designed slit system for depth-resolved X-ray diffraction measurements

DOE Office of Scientific and Technical Information (OSTI.GOV)

Sinsheimer, John; Bouet, Nathalie; Ghose, Sanjit

2016-10-06

A new system of slits called `spiderweb slits' have been developed for depth-resolved powder or polycrystalline X-ray diffraction measurements. The slits act on diffracted X-rays to select a particular gauge volume of sample, while absorbing diffracted X-rays from outside of this volume. Although the slit geometry is to some extent similar to that of previously developed conical slits or spiral slits, this new design has advantages over the previous ones in use for complex heterogeneous materials andin situandoperandodiffraction measurements. For example, the slits can measure a majority of any diffraction cone for any polycrystalline material, over a continuous range ofmore » diffraction angles, and work for X-ray energies of tens to hundreds of kiloelectronvolts. The design is generated and optimized using ray-tracing simulations, and fabricated through laser micromachining. The first prototype was successfully tested at the X17A beamline at the National Synchrotron Light Source, and shows similar performance to simulations, demonstrating gauge volume selection for standard powders, for all diffraction peaks over angles of 2–10°. A similar, but improved, design will be implemented at the X-ray Powder Diffraction beamline at the National Synchrotron Light Source II.« less

Investigation of the commensurate magnetic structure in the heavy-fermion compound CePt 2 In 7 using magnetic resonant x-ray diffraction

DOE Office of Scientific and Technical Information (OSTI.GOV)

Gauthier, Nicolas; Wermeille, Didier; Casati, Nicola

In this paper, we investigated the magnetic structure of the heavy-fermion compound CePt 2In 7 below T N = 5.34 (2) K using magnetic resonant x-ray diffraction at ambient pressure. The magnetic order is characterized by a commensurate propagation vector k 1/2 = (1/2, 1/2, 1/2) with spins lying in the basal plane. Our measurements did not reveal the presence of an incommensurate order propagating along the high-symmetry directions in reciprocal space but cannot exclude other incommensurate modulations or weak scattering intensities. The observed commensurate order can be described equivalently by either a single-k structure or by a multi-k structure.more » Furthermore we explain how a commensurate-only ordering may explain the broad distribution of internal fields observed in nuclear quadrupolar resonance experiments [Sakai et al., Phys. Rev. B 83, 140408 (2011)] that was previously attributed to an incommensurate order. We also report powder x-ray diffraction showing that the crystallographic structure of CePt 2In 7 changes monotonically with pressure up to P = 7.3 GPa at room temperature. The determined bulk modulus B 0 = 81.1 (3) GPa is similar to those of the Ce-115 family. Broad diffraction peaks confirm the presence of pronounced strain in polycrystalline samples of CePt 2In 7. Lastly, we discuss how strain effects can lead to different electronic and magnetic properties between polycrystalline and single crystal samples.« less

Investigation of the commensurate magnetic structure in the heavy-fermion compound CePt 2 In 7 using magnetic resonant x-ray diffraction

DOE PAGES

Gauthier, Nicolas; Wermeille, Didier; Casati, Nicola; ...

2017-08-10

In this paper, we investigated the magnetic structure of the heavy-fermion compound CePt 2In 7 below T N = 5.34 (2) K using magnetic resonant x-ray diffraction at ambient pressure. The magnetic order is characterized by a commensurate propagation vector k 1/2 = (1/2, 1/2, 1/2) with spins lying in the basal plane. Our measurements did not reveal the presence of an incommensurate order propagating along the high-symmetry directions in reciprocal space but cannot exclude other incommensurate modulations or weak scattering intensities. The observed commensurate order can be described equivalently by either a single-k structure or by a multi-k structure.more » Furthermore we explain how a commensurate-only ordering may explain the broad distribution of internal fields observed in nuclear quadrupolar resonance experiments [Sakai et al., Phys. Rev. B 83, 140408 (2011)] that was previously attributed to an incommensurate order. We also report powder x-ray diffraction showing that the crystallographic structure of CePt 2In 7 changes monotonically with pressure up to P = 7.3 GPa at room temperature. The determined bulk modulus B 0 = 81.1 (3) GPa is similar to those of the Ce-115 family. Broad diffraction peaks confirm the presence of pronounced strain in polycrystalline samples of CePt 2In 7. Lastly, we discuss how strain effects can lead to different electronic and magnetic properties between polycrystalline and single crystal samples.« less

Local terahertz field enhancement for time-resolved x-ray diffraction

DOE PAGES

Kozina, M.; Pancaldi, M.; Bernhard, C.; ...

2017-02-20

We report local field strength enhancement of single-cycle terahertz (THz) pulses in an ultrafast time-resolved x-ray diffraction experiment. We show that patterning the sample with gold microstructures increases the THz field without changing the THz pulse shape or drastically affecting the quality of the x-ray diffraction pattern. Lastly, we find a five-fold increase in THz-induced x-ray diffraction intensity change in the presence of microstructures on a SrTiO 3 thin-film sample.

Local terahertz field enhancement for time-resolved x-ray diffraction

DOE Office of Scientific and Technical Information (OSTI.GOV)

Kozina, M.; Pancaldi, M.; Bernhard, C.

We report local field strength enhancement of single-cycle terahertz (THz) pulses in an ultrafast time-resolved x-ray diffraction experiment. We show that patterning the sample with gold microstructures increases the THz field without changing the THz pulse shape or drastically affecting the quality of the x-ray diffraction pattern. Lastly, we find a five-fold increase in THz-induced x-ray diffraction intensity change in the presence of microstructures on a SrTiO 3 thin-film sample.

Hydrogen-bearing iron peroxide and its implications to the deep Earth

NASA Astrophysics Data System (ADS)

Liu, J.; Hu, Q.; Kim, D. Y.; Wu, Z.; Wang, W.; Alp, E. E.; Yang, L.; Xiao, Y.; Meng, Y.; Chow, P.; Greenberg, E.; Prakapenka, V. B.; Mao, H. K.; Mao, W. L.

2017-12-01

Hydrous materials subducted into the deep mantle may play a significant role in the geophysical and geochemical processes of the lower mantle through geological time, but their roles have not become clear yet in the region. Hydrogen-bearing iron peroxide (FeO2Hx) was recently discovered to form through dehydrogenation of goethite (e.g., FeOOH) and the reaction between hematite (Fe2O3) and water under deep lower mantle conditions. We conducted synchrotron Mössbauer, X-ray absorption, and X-ray emission spectroscopy measurements to investigate the electronic spin and valence states of iron in hydrogen-bearing iron peroxide (FeO2Hx) in-situ at high pressures. Combined with theoretical calculations and other high-pressure experiments (i.e., nuclear resonant inelastic x-ray scattering spectroscopy and X-ray diffraction coupled with laser-heated diamond-anvil cell techniques), we find that the intriguing properties of FeO2Hx could shed light on the origin of a number of the observed geochemical and geophysical anomalies in the deep Earth.

Thermal x-ray diffraction and near-field phase contrast imaging

NASA Astrophysics Data System (ADS)

Li, Zheng; Classen, Anton; Peng, Tao; Medvedev, Nikita; Wang, Fenglin; Chapman, Henry N.; Shih, Yanhua

2017-10-01

Using higher-order coherence of thermal light sources, the resolution power of standard x-ray imaging techniques can be enhanced. In this work, we applied the higher-order measurement to far-field x-ray diffraction and near-field phase contrast imaging (PCI), in order to achieve superresolution in x-ray diffraction and obtain enhanced intensity contrast in PCI. The cost of implementing such schemes is minimal compared to the methods that achieve similar effects by using entangled x-ray photon pairs.

Thermal x-ray diffraction and near-field phase contrast imaging

DOE PAGES

Li, Zheng; Classen, Anton; Peng, Tao; ...

2017-12-27

Using higher-order coherence of thermal light sources, the resolution power of standard x-ray imaging techniques can be enhanced. Here in this work, we applied the higher-order measurement to far-field x-ray diffraction and near-field phase contrast imaging (PCI), in order to achieve superresolution in x-ray diffraction and obtain enhanced intensity contrast in PCI. The cost of implementing such schemes is minimal compared to the methods that achieve similar effects by using entangled x-ray photon pairs.

Pressure-Induced Structural Phase Transition in CeNi: X-ray and Neutron Scattering Studies and First-Principles Calculations

DOE PAGES

Mirmelstein, A.; Podlesnyak, Andrey A.; dos Santos, Antonio M.; ...

2015-08-03

The pressure-induced structural phase transition in the intermediate-valence compound CeNi has been investigated by x-ray and neutron powder diffraction techniques. It is shown that the structure of the pressure-induced CeNi phase (phases) can be described in terms of the Pnma space group. Equations of state for CeNi on both sides of the phase transition are derived and an approximate P-T phase diagram is suggested for P<8 GPa and T<300 K. The observed Cmcm→Pnma structural transition is then analyzed using density functional theory calculations, which successfully reproduce the ground state volume, the phase transition pressure, and the volume collapse associated withmore » the phase transition.« less

An image focusing means by using an opaque object to diffract x-rays

DOEpatents

Sommargren, Gary E.; Weaver, H. Joseph

1991-01-01

The invention provides a method and apparatus for focusing and imaging x-rays. An opaque sphere is used as a diffractive imaging element to diffract x-rays from an object so that the divergent x-ray wavefronts are transformed into convergent wavefronts and are brought to focus to form an image of the object with a large depth of field.

Pressure-induced half-collapsed-tetragonal phase in CaKFe 4 As 4

DOE Office of Scientific and Technical Information (OSTI.GOV)

Kaluarachchi, Udhara S.; Taufour, Valentin; Sapkota, Aashish

Here, we report the temperature-pressure phase diagram of CaKFe 4As 4 established using high-pressure electrical resistivity, magnetization, and high-energy x-ray diffraction measurements up to 6 GPa. With increasing pressure, both resistivity and magnetization data show that the bulk superconducting transition of CaKFe 4As 4 is suppressed and then disappears at p ≳ 4 GPa. High-pressure x-ray data clearly indicate a phase transition to a collapsed tetragonal phase in CaKFe 4As 4 under pressure that coincides with the abrupt loss of bulk superconductivity near 4 GPa. The x-ray data, combined with resistivity data, indicate that the collapsed tetragonal transition line ismore » essentially independent of pressure, occurring at 4.0(5) GPa for temperatures below 150 K. Density functional theory calculations also find a sudden transition to a collapsed tetragonal state near 4 GPa, as As-As bonding develops across the Ca layer. Bonding across the K layer only occurs for p ≥ 12 GPa. These findings demonstrate a different type of collapsed tetragonal phase in CaKFe 4As 4 as compared to CaFe 2As 2: a half-collapsed tetragonal phase.« less

Pressure-induced half-collapsed-tetragonal phase in CaKFe 4 As 4

DOE PAGES

Kaluarachchi, Udhara S.; Taufour, Valentin; Sapkota, Aashish; ...

2017-10-02

Here, we report the temperature-pressure phase diagram of CaKFe 4As 4 established using high-pressure electrical resistivity, magnetization, and high-energy x-ray diffraction measurements up to 6 GPa. With increasing pressure, both resistivity and magnetization data show that the bulk superconducting transition of CaKFe 4As 4 is suppressed and then disappears at p ≳ 4 GPa. High-pressure x-ray data clearly indicate a phase transition to a collapsed tetragonal phase in CaKFe 4As 4 under pressure that coincides with the abrupt loss of bulk superconductivity near 4 GPa. The x-ray data, combined with resistivity data, indicate that the collapsed tetragonal transition line ismore » essentially independent of pressure, occurring at 4.0(5) GPa for temperatures below 150 K. Density functional theory calculations also find a sudden transition to a collapsed tetragonal state near 4 GPa, as As-As bonding develops across the Ca layer. Bonding across the K layer only occurs for p ≥ 12 GPa. These findings demonstrate a different type of collapsed tetragonal phase in CaKFe 4As 4 as compared to CaFe 2As 2: a half-collapsed tetragonal phase.« less

Pressure-induced half-collapsed-tetragonal phase in CaKFe4As4

NASA Astrophysics Data System (ADS)

Kaluarachchi, Udhara S.; Taufour, Valentin; Sapkota, Aashish; Borisov, Vladislav; Kong, Tai; Meier, William R.; Kothapalli, Karunakar; Ueland, Benjamin G.; Kreyssig, Andreas; Valentí, Roser; McQueeney, Robert J.; Goldman, Alan I.; Bud'ko, Sergey L.; Canfield, Paul C.

2017-10-01

We report the temperature-pressure phase diagram of CaKFe4As4 established using high-pressure electrical resistivity, magnetization, and high-energy x-ray diffraction measurements up to 6 GPa. With increasing pressure, both resistivity and magnetization data show that the bulk superconducting transition of CaKFe4As4 is suppressed and then disappears at p ≳4 GPa. High-pressure x-ray data clearly indicate a phase transition to a collapsed tetragonal phase in CaKFe4As4 under pressure that coincides with the abrupt loss of bulk superconductivity near 4 GPa. The x-ray data, combined with resistivity data, indicate that the collapsed tetragonal transition line is essentially independent of pressure, occurring at 4.0(5) GPa for temperatures below 150 K. Density functional theory calculations also find a sudden transition to a collapsed tetragonal state near 4 GPa, as As-As bonding develops across the Ca layer. Bonding across the K layer only occurs for p ≥12 GPa. These findings demonstrate a different type of collapsed tetragonal phase in CaKFe4As4 as compared to CaFe2As2 : a half-collapsed tetragonal phase.

Soft X-Ray Diffraction Microscopy of a Frozen Hydrated Yeast Cell

DOE PAGES

Huang, Xiaojing; Nelson, Johanna; Kirz, Janos; ...

2009-11-01

We report the first image of an intact, frozen hydrated eukaryotic cell using x-ray diffraction microscopy, or coherent x-ray diffraction imaging. By plunge freezing the specimen in liquid ethane and maintaining it below -170 °C, artifacts due to dehydration, ice crystallization, and radiation damage are greatly reduced. In this example, coherent diffraction data using 520 eV x rays were recorded and reconstructed to reveal a budding yeast cell at a resolution better than 25 nm. This demonstration represents an important step towards high resolution imaging of cells in their natural, hydrated state, without limitations imposed by x-ray optics.

Application of focused-beam flat-sample method to synchrotron powder X-ray diffraction with anomalous scattering effect

NASA Astrophysics Data System (ADS)

Tanaka, M.; Katsuya, Y.; Matsushita, Y.

2013-03-01

The focused-beam flat-sample method (FFM), which is a method for high-resolution and rapid synchrotron X-ray powder diffraction measurements by combination of beam focusing optics, a flat shape sample and an area detector, was applied for diffraction experiments with anomalous scattering effect. The advantages of FFM for anomalous diffraction were absorption correction without approximation, rapid data collection by an area detector and good signal-to-noise ratio data by focusing optics. In the X-ray diffraction experiments of CoFe2O4 and Fe3O4 (By FFM) using X-rays near the Fe K absorption edge, the anomalous scattering effect between Fe/Co or Fe2+/Fe3+ can be clearly detected, due to the change of diffraction intensity. The change of observed diffraction intensity as the incident X-ray energy was consistent with the calculation. The FFM is expected to be a method for anomalous powder diffraction.

Rietveld analysis using powder diffraction data with anomalous scattering effect obtained by focused beam flat sample method

DOE Office of Scientific and Technical Information (OSTI.GOV)

Tanaka, Masahiko, E-mail: masahiko@spring8.or.jp; Katsuya, Yoshio, E-mail: katsuya@spring8.or.jp; Sakata, Osami, E-mail: SAKATA.Osami@nims.go.jp

2016-07-27

Focused-beam flat-sample method (FFM) is a new trial for synchrotron powder diffraction method, which is a combination of beam focusing optics, flat shape powder sample and area detectors. The method has advantages for X-ray diffraction experiments applying anomalous scattering effect (anomalous diffraction), because of 1. Absorption correction without approximation, 2. High intensity X-rays of focused incident beams and high signal noise ratio of diffracted X-rays 3. Rapid data collection with area detectors. We applied the FFM to anomalous diffraction experiments and collected synchrotron X-ray powder diffraction data of CoFe{sub 2}O{sub 4} (inverse spinel structure) using X-rays near Fe K absorptionmore » edge, which can distinguish Co and Fe by anomalous scattering effect. We conducted Rietveld analyses with the obtained powder diffraction data and successfully determined the distribution of Co and Fe ions in CoFe{sub 2}O{sub 4} crystal structure.« less

High-pressure polymorphism of the electrochemically active organic molecule tetrahydroxy-p-benzoquinone

DOE PAGES

Ciezak-Jenkins, Jennifer A.

2016-04-22

We have studied the structural and chemical response of tetrahydroxy-p-benzoquinone to isothermal compression to near 20 GPa using powder x-ray diffraction and vibrational spectroscopy. Compression beyond 11.5 GPa resulted in the appearance of several new peaks in the x-ray patterns, changes in the peak distribution and intensities, as well as the disappearance of features observed at lower pressures, which when coupled with concomitant changes in the infrared spectrum are indicative of a phase transition. Further analysis of the infrared spectra suggest this phase transition results in an increase in the anharmonicity of the system. Finally, Raman spectroscopic experiments indicate themore » high-pressure phase to be highly photosensitive and easily polymerized.« less

Characterization of monoclinic crystals in tablets by pattern-fitting procedure using X-ray powder diffraction data.

PubMed

Yamamura, Shigeo; Momose, Yasunori

2003-06-18

The purpose of this study is to characterize the monoclinic crystals in tablets by using X-ray powder diffraction data and to evaluate the deformation feature of crystals during compression. The monoclinic crystals of acetaminophen and benzoic acid were used as the samples. The observed X-ray diffraction intensities were fitted to the analytic expression, and the fitting parameters, such as the lattice parameters, the peak-width parameters, the preferred orientation parameter and peak asymmetric parameter were optimized by a non-linear least-squares procedure. The Gauss and March distribution functions were used to correct the preferred orientation of crystallites in the tablet. The March function performed better in correcting the modification of diffraction intensity by preferred orientation of crystallites, suggesting that the crystallites in the tablets had fiber texture with axial orientation. Although a broadening of diffraction peaks was observed in acetaminophen tablets with an increase of compression pressure, little broadening was observed in the benzoic tablets. These results suggest that "acetaminophen is a material consolidating by fragmentation of crystalline particles and benzoic acid is a material consolidating by plastic deformation then occurred rearrangement of molecules during compression". A pattern-fitting procedure is the superior method for characterizing the crystalline drugs of monoclinic crystals in the tablets, as well as orthorhombic isoniazid and mannitol crystals reported in the previous paper.

Compressibility of Cs2SnBr6 by X-ray diffraction and Raman spectroscopy

NASA Astrophysics Data System (ADS)

Yuan, Guan; Huang, Shengxuan; Niu, Jingjing; Qin, Shan; Wu, Xiang; Ding, Hongrui; Lu, Anhuai

2018-07-01

Cs2SnBr6, one promising material applied in perovskite solar cells, has been investigated up to 20 GPa by synchrotron X-ray diffraction and Raman spectroscopy. Both experimental data demonstrate that no phase transition occurs up to 20 GPa. By fitting the third-order Birch-Murnaghan equation of state, we have obtained V0 = 1288 (14) Å3, K0 = 11 (1) GPa and K0‧ = 7 (1). The ultralow value of bulk modulus K0 demonstrates the soft nature of Cs2SnBr6. Combining calculated values with experimental results, we find that x coordinate of Sn (x,0,0) atoms increases and Snsbnd Br bond lengths get shortened on compression. We have assigned vibrational peaks of Cs2SnBr6 in Raman measurements, and all the three Raman bands present nonlinear correlations with pressure.

Sound velocity measurements of dhcp-FeHx up to 70 GPa using inelastic X-ray scattering: Implications for the abundance of hydrogen in the Earth's core

NASA Astrophysics Data System (ADS)

Shibazaki, Y.; Ohtani, E.; Fukui, H.; Sakai, T.; Kamada, S.; Baron, A. Q.; Nishitani, N.; Hirao, N.; Takemura, K.

2011-12-01

The Earth's interior has been directly investigated by seismic wave propagation and normal mode oscillation. In particular, the distributions of density and sound velocity are available to study the Earth's core (e.g. PREM). The inner core, which is solid state, is approximately 3 % less dense than pure iron (a core density deficit), and it is considered that the core consists of iron and light elements, such as hydrogen, carbon, oxygen, silicon, and sulfur. In this work, in order to constrain the abundance of hydrogen in the Earth's core by matching the density and sound velocity of FeHx to those of PREM, we determined the compressional sound velocity of iron hydride at high pressure using inelastic X-ray scattering (IXS). The IXS experiments and in situ X-ray diffraction (XRD) experiments were conducted up to 70 GPa and room temperature. High-pressure conditions were generated using a symmetric diamond anvil cell (DAC) with tungsten gaskets. Hydrogen initially pressurized to 0.18 GPa was loaded to the sample chamber. The IXS experiments were performed at BL35XU of the SPring-8 facility in Japan. The XRD experiments at high pressure were carried out by the angle dispersive method at BL10XU of the SPring-8 facility in Japan. The each XRD pattern of FeHx was collected after each IXS measurement in order to obtain directly the density of FeHx. Over the range of pressure studied, the diffraction lines of double-hexagonal close-packed (dhcp)-FeHx were observed and there were no diffraction lines of iron. We show that FeHx follows Birch's law for Vp above 37 GPa, namely a linear dependence between velocity and density. The estimated Vp, extrapolated to core conditions, is compared with PREM. Our results provide that the Earth's inner core could contain about 0.2 wt% hydrogen.

Magnetic interactions in NiO at ultrahigh pressure

DOE PAGES

Potapkin, Vasily; Dubrovinsky, Leonid; Sergueev, I.; ...

2016-05-24

Here, magnetic properties of NiO have been studied in the multimegabar pressure range by nuclear forward scattering of synchrotron radiation using the 67.4 keV M ssbauer transition of 61Ni. The observed magnetic hyperfine splitting confirms the antiferromagnetic state of NiO up to 280 GPa, the highest pressure where magnetism has been observed so far, in any material. Remarkably, the hyperfine field increases from 8.47 T at ambient pressure to ~24 T at the highest pressure, ruling out the possibility of a magnetic collapse. A joint x-ray diffraction and extended x-ray-absorption fine structure investigation reveals that NiO remains in a distortedmore » sodium chloride structure in the entire studied pressure range. Ab initio calculations support the experimental observations, and further indicate a complete absence of Mott transition in NiO up to at least 280 GPa.« less

Homogeneity of CdZnTe detectors

NASA Astrophysics Data System (ADS)

Hermon, H.; Schieber, M.; James, R. B.; Lund, J.; Antolak, A. J.; Morse, D. H.; Kolesnikov, N. N. P.; Ivanov, Y. N.; Goorsky, M. S.; Yoon, H.; Toney, J.; Schlesinger, T. E.

1998-02-01

We describe the current state of nuclear radiation detectors produced from single crystals of Cd 1- xZn xTe(CZT), with 0.04 < x < 0.4, grown by the vertical high pressure Bridgman (VHPB) method. The crystals investigated were grown commercially both in the USA and at the Institute of Solid State Physics, Chernogolska, Russia. The CZT was evaluated by Sandia National Laboratories and the UCLA and CMU groups using proton-induced X-ray emission (PIXE), X-ray diffraction (XRD), photoluminescence (PL), infrared (IR) transmission microscopy, leakage current measurements and response to nuclear radiation. We discuss the homogeneity of the various CZT crystals based on the results from these measurement techniques.

Spin quenching assisted by a strongly anisotropic compression behavior in MnP

DOE Office of Scientific and Technical Information (OSTI.GOV)

Han, Fei; Wang, Di; Wang, Yonggang

We studied the crystal structure and spin state of MnP under high pressure with synchrotron X-ray diffraction and X-ray emission spectroscopy. MnP has an exceedingly strong anisotropy in compressibility, with the primary compressible direction along the b axis of the Pnma structure. X-ray emission spectroscopy reveals a pressure-driven quenching of the spin state in MnP. First-principles calculations suggest that the strongly anisotropic compression behavior significantly enhances the dispersion of the Mn d-orbitals and the splitting of the d-orbital levels compared to the hypothetical isotropic compression behavior. Thus, we propose spin quenching results mainly from the significant enhancement of the itinerancymore » of d electrons and partly from spin rearrangement occurring in the split d-orbital levels near the Fermi level. This explains the fast suppression of magnetic ordering in MnP under high pressure. The spin quenching lags behind the occurrence of superconductivity at ~8 GPa implying that spin fluctuations govern the electron pairing for superconductivity.« less

Dynamical effects in Bragg coherent x-ray diffraction imaging of finite crystals

NASA Astrophysics Data System (ADS)

Shabalin, A. G.; Yefanov, O. M.; Nosik, V. L.; Bushuev, V. A.; Vartanyants, I. A.

2017-08-01

We present simulations of Bragg coherent x-ray diffractive imaging (CXDI) data from finite crystals in the frame of the dynamical theory of x-ray diffraction. The developed approach is based on a numerical solution of modified Takagi-Taupin equations and can be applied for modeling of a broad range of x-ray diffraction experiments with finite three-dimensional crystals of arbitrary shape also in the presence of strain. We performed simulations for nanocrystals of a cubic and hemispherical shape of different sizes and provided a detailed analysis of artifacts in the Bragg CXDI reconstructions introduced by the dynamical diffraction. Based on our theoretical analysis we developed an analytical procedure to treat effects of refraction and absorption in the reconstruction. Our results elucidate limitations for the kinematical approach in the Bragg CXDI and suggest a natural criterion to distinguish between kinematical and dynamical cases in coherent x-ray diffraction on a finite crystal.

Chemical characterization of 4140 steel implanted by nitrogen ions

NASA Astrophysics Data System (ADS)

Niño, E. D. V.; Pinto, J. L.; Dugar-Zhabon, V.; Henao, J. A.

2012-06-01

AISI SAE 4140 steel samples of different surface roughness which are implanted with 20 keV and 30 keV nitrogen ions at a dose of 1017 ions/cm2 are studied. The crystal phases of nitrogen compositions of the implanted samples, obtained with help of an x-ray diffraction method, are confronted with the data reported by the International Centre for Diffraction Data (ICDD) PDF-2. The implantation treatment is realized in high-voltage pulsed discharges at low pressures. The crystal structure of the implanted solid surfaces is analyzed by the x-ray diffraction technique which permits to identify the possible newly formed compounds and to identify any change in the surface structure of the treated samples. A decrease in the intensity of the plane (110), a reduction of the cell unity in values of 2-theta and a diminishing of the crystallite dimensions in comparison with non-implanted samples are observed.

High-pressure structural parameters and equation of state of osmium to 207 GPa

DOE PAGES

Perreault, Christopher S.; Velisavljevic, Nenad; Vohra, Yogesh K.; ...

2017-09-08

We studied the most incompressible transition metal osmium (Os) under high pressure. There is significant interest in Os because of the structural anomalies attributed to topological transitions in the Fermi surface for valence electrons in the hexagonal close-packed phase. We report on measurements of structural parameters and equation of state on Os metal to a pressure of 207 GPa at ambient temperature using platinum as a pressure standard. We also obtained angle-dispersive X-ray diffraction data at a synchrotron source with closely spaced pressure intervals to observe any discontinuities or anomalies in the axial c/a ratio at high pressures. Rietveld refinementsmore » of X-ray diffraction data show a slowly varying axial ratio (c/a) with a broad minimum at 75 GPa. Our data do not provide any evidence of anomalous behavior in the c/a ratio in Os at 25 or 150 GPa as have been reported in previous studies. These experimental results are in agreement with theoretical calculations that do not predict any anomalous behavior in c/a ratio in Os under extreme conditions. We present an equation of state for Os to 207 GPa (V/V 0 = 0.761) at ambient temperature and compare our results with the previously published data.« less

High-pressure structural parameters and equation of state of osmium to 207 GPa

DOE Office of Scientific and Technical Information (OSTI.GOV)

Perreault, Christopher S.; Velisavljevic, Nenad; Vohra, Yogesh K.

We studied the most incompressible transition metal osmium (Os) under high pressure. There is significant interest in Os because of the structural anomalies attributed to topological transitions in the Fermi surface for valence electrons in the hexagonal close-packed phase. We report on measurements of structural parameters and equation of state on Os metal to a pressure of 207 GPa at ambient temperature using platinum as a pressure standard. We also obtained angle-dispersive X-ray diffraction data at a synchrotron source with closely spaced pressure intervals to observe any discontinuities or anomalies in the axial c/a ratio at high pressures. Rietveld refinementsmore » of X-ray diffraction data show a slowly varying axial ratio (c/a) with a broad minimum at 75 GPa. Our data do not provide any evidence of anomalous behavior in the c/a ratio in Os at 25 or 150 GPa as have been reported in previous studies. These experimental results are in agreement with theoretical calculations that do not predict any anomalous behavior in c/a ratio in Os under extreme conditions. We present an equation of state for Os to 207 GPa (V/V 0 = 0.761) at ambient temperature and compare our results with the previously published data.« less

Equations of state of anhydrous AlF 3 and AlI 3 : Modeling of extreme condition halide chemistry

DOE Office of Scientific and Technical Information (OSTI.GOV)

Stavrou, Elissaios; Zaug, Joseph M.; Bastea, Sorin

Pressure dependent angle-dispersive x-ray powder diffraction measurements of alpha-phase aluminum trifluoride (α-AlF 3) and separately, aluminum triiodide (AlI 3) were conducted using a diamond-anvil cell. Results at 295 K extend to 50 GPa. The equations of state of AlF 3 and AlI 3 were determined through refinements of collected x-ray diffraction patterns. The respective bulk moduli and corresponding pressure derivatives are reported for multiple orders of the Birch-Murnaghan (B-M), finite-strain (F-f), and higher pressure finite-strain (G-g) EOS analysis models. Aluminum trifluoride exhibits an apparent isostructural phase transition at approximately 12 GPa. Aluminum triiodide also undergoes a second-order atomic rearrangement: appliedmore » stress transformed a monoclinically distorted face centered cubic (fcc) structure into a standard fcc structural arrangement of iodine atoms. In conclusion, results from semi-empirical thermochemical computations of energetic materials formulated with fluorine containing reactants were obtained with the aim of predicting the yield of halogenated products.« less

Equations of state of anhydrous AlF{sub 3} and AlI{sub 3}: Modeling of extreme condition halide chemistry

DOE Office of Scientific and Technical Information (OSTI.GOV)

Stavrou, Elissaios, E-mail: stavrou1@llnl.gov; Lawrence Livermore National Laboratory, Physical and Life Sciences Directorate, P.O. Box 808 L-350, Livermore, California 94550; Zaug, Joseph M., E-mail: zaug1@llnl.gov

Pressure dependent angle-dispersive x-ray powder diffraction measurements of alpha-phase aluminum trifluoride (α-AlF{sub 3}) and separately, aluminum triiodide (AlI{sub 3}) were conducted using a diamond-anvil cell. Results at 295 K extend to 50 GPa. The equations of state of AlF{sub 3} and AlI{sub 3} were determined through refinements of collected x-ray diffraction patterns. The respective bulk moduli and corresponding pressure derivatives are reported for multiple orders of the Birch-Murnaghan (B-M), finite-strain (F-f), and higher pressure finite-strain (G-g) EOS analysis models. Aluminum trifluoride exhibits an apparent isostructural phase transition at approximately 12 GPa. Aluminum triiodide also undergoes a second-order atomic rearrangement: appliedmore » stress transformed a monoclinically distorted face centered cubic (fcc) structure into a standard fcc structural arrangement of iodine atoms. Results from semi-empirical thermochemical computations of energetic materials formulated with fluorine containing reactants were obtained with the aim of predicting the yield of halogenated products.« less

Equations of state of anhydrous AlF 3 and AlI 3 : Modeling of extreme condition halide chemistry

DOE PAGES

Stavrou, Elissaios; Zaug, Joseph M.; Bastea, Sorin; ...

2015-06-04

Pressure dependent angle-dispersive x-ray powder diffraction measurements of alpha-phase aluminum trifluoride (α-AlF 3) and separately, aluminum triiodide (AlI 3) were conducted using a diamond-anvil cell. Results at 295 K extend to 50 GPa. The equations of state of AlF 3 and AlI 3 were determined through refinements of collected x-ray diffraction patterns. The respective bulk moduli and corresponding pressure derivatives are reported for multiple orders of the Birch-Murnaghan (B-M), finite-strain (F-f), and higher pressure finite-strain (G-g) EOS analysis models. Aluminum trifluoride exhibits an apparent isostructural phase transition at approximately 12 GPa. Aluminum triiodide also undergoes a second-order atomic rearrangement: appliedmore » stress transformed a monoclinically distorted face centered cubic (fcc) structure into a standard fcc structural arrangement of iodine atoms. In conclusion, results from semi-empirical thermochemical computations of energetic materials formulated with fluorine containing reactants were obtained with the aim of predicting the yield of halogenated products.« less

Microscopic structural change in a liquid Fe-C alloy of ~5 GPa

DOE PAGES

Shibazaki, Yuki; Kono, Yoshio; Fei, Yingwei

2015-07-04

The structure of a liquid Fe-3.5 wt% C alloy is examined for up to 7.2 GPa via multiangle energy-dispersive X-ray diffraction using a Paris-Edinburgh type large-volume press. X-ray diffraction data show clear changes in the pressure-dependent peak positions of structure factor and reduced pair distribution function at 5GPa. These results suggest that the liquid Fe-3.5wt%C alloys change structurally at approximately 5GPa. This finding serves as a microscopic explanation for the alloy’s previously observed density change at the same pressure. The pressure dependencies of the nearest and second neighbor distances of the liquid Fe-3.5 wt% C alloy are similar to thosemore » of liquid Fe which exhibits a structural change near the bcc-fcc-liquid triple point (5.2GPa and 1991 K). Here, similarities between Fe-3.5wt% C and Fe suggest that a density change also occurs in liquid Fe and that this structural change extends to other Fe-light element alloys.« less

Development and Characterization of a 16.3 keV X-Ray Source at the National Ignition Facility

NASA Astrophysics Data System (ADS)

Fournier, K. B.; Barrios, M. A.; Schneider, M. B.; Khan, S.; Chen, H.; Coppari, F.; Rygg, R.; Hohenberger, M.; Albert, F.; Moody, J.; Ralph, J.; Kemp, G. E.; Regan, S. P.

2014-10-01

X-ray sources at the National Ignition Facility are needed for radiography of in-flight capsules in inertial confinement fusion experiments and for diffraction studies of materials at high pressures. In the former case, we want to optimize signal to noise and signal over background ratios for the radiograph, in the latter case, we want to minimize high-energy emission from the backlighter that creates background on the diffraction data. Four interleaved shots at NIF were taken in one day, with laser irradiances on a Zr backlighter target ranging from 5 to 14 × 1015 W/cm2. Two shots were for source optimization as a function of laser irradiance. X-ray fluxes were measured with the time-resolved NIF X-ray Spectrometer (NXS) and the DANTE array of calibrated, filtered diodes. Two shots were optimized to make backscatter measurements with the FABS and NBI optical power systems. The backscatter levels are investigated to look for correlation with hot electron populations inferred from high-energy x rays measured with the FFLEX broadband spectrometer. Results from all shots are presented and compared with models. Work performed under the auspices of the U.S. DOE by LLNL under Contract No. DE-AC52-07NA27344.

Instrument and method for X-ray diffraction, fluorescence, and crystal texture analysis without sample preparation

NASA Technical Reports Server (NTRS)

Gendreau, Keith (Inventor); Martins, Jose Vanderlei (Inventor); Arzoumanian, Zaven (Inventor)

2010-01-01

An X-ray diffraction and X-ray fluorescence instrument for analyzing samples having no sample preparation includes a X-ray source configured to output a collimated X-ray beam comprising a continuum spectrum of X-rays to a predetermined coordinate and a photon-counting X-ray imaging spectrometer disposed to receive X-rays output from an unprepared sample disposed at the predetermined coordinate upon exposure of the unprepared sample to the collimated X-ray beam. The X-ray source and the photon-counting X-ray imaging spectrometer are arranged in a reflection geometry relative to the predetermined coordinate.

Terapascal static pressure generation with ultrahigh yield strength nanodiamond.

PubMed

Dubrovinskaia, Natalia; Dubrovinsky, Leonid; Solopova, Natalia A; Abakumov, Artem; Turner, Stuart; Hanfland, Michael; Bykova, Elena; Bykov, Maxim; Prescher, Clemens; Prakapenka, Vitali B; Petitgirard, Sylvain; Chuvashova, Irina; Gasharova, Biliana; Mathis, Yves-Laurent; Ershov, Petr; Snigireva, Irina; Snigirev, Anatoly

2016-07-01

Studies of materials' properties at high and ultrahigh pressures lead to discoveries of unique physical and chemical phenomena and a deeper understanding of matter. In high-pressure research, an achievable static pressure limit is imposed by the strength of available strong materials and design of high-pressure devices. Using a high-pressure and high-temperature technique, we synthesized optically transparent microballs of bulk nanocrystalline diamond, which were found to have an exceptional yield strength (~460 GPa at a confining pressure of ~70 GPa) due to the unique microstructure of bulk nanocrystalline diamond. We used the nanodiamond balls in a double-stage diamond anvil cell high-pressure device that allowed us to generate static pressures beyond 1 TPa, as demonstrated by synchrotron x-ray diffraction. Outstanding mechanical properties (strain-dependent elasticity, very high hardness, and unprecedented yield strength) make the nanodiamond balls a unique device for ultrahigh static pressure generation. Structurally isotropic, homogeneous, and made of a low-Z material, they are promising in the field of x-ray optical applications.

Terapascal static pressure generation with ultrahigh yield strength nanodiamond

PubMed Central

Dubrovinskaia, Natalia; Dubrovinsky, Leonid; Solopova, Natalia A.; Abakumov, Artem; Turner, Stuart; Hanfland, Michael; Bykova, Elena; Bykov, Maxim; Prescher, Clemens; Prakapenka, Vitali B.; Petitgirard, Sylvain; Chuvashova, Irina; Gasharova, Biliana; Mathis, Yves-Laurent; Ershov, Petr; Snigireva, Irina; Snigirev, Anatoly

2016-01-01

Studies of materials’ properties at high and ultrahigh pressures lead to discoveries of unique physical and chemical phenomena and a deeper understanding of matter. In high-pressure research, an achievable static pressure limit is imposed by the strength of available strong materials and design of high-pressure devices. Using a high-pressure and high-temperature technique, we synthesized optically transparent microballs of bulk nanocrystalline diamond, which were found to have an exceptional yield strength (~460 GPa at a confining pressure of ~70 GPa) due to the unique microstructure of bulk nanocrystalline diamond. We used the nanodiamond balls in a double-stage diamond anvil cell high-pressure device that allowed us to generate static pressures beyond 1 TPa, as demonstrated by synchrotron x-ray diffraction. Outstanding mechanical properties (strain-dependent elasticity, very high hardness, and unprecedented yield strength) make the nanodiamond balls a unique device for ultrahigh static pressure generation. Structurally isotropic, homogeneous, and made of a low-Z material, they are promising in the field of x-ray optical applications. PMID:27453944

High-pressure high-temperature phase diagram of gadolinium studied using a boron-doped heater anvil

DOE Office of Scientific and Technical Information (OSTI.GOV)

Montgomery, J. M.; Samudrala, G. K.; Velisavljevic, N.

A boron-doped designer heater anvil is used in conjunction with powder x-ray diffraction to collect structural information on a sample of quasi-hydrostatically loaded gadolinium metal up to pressures above 8 GPa and 600 K. The heater anvil consists of a natural diamond anvil that has been surface modified with a homoepitaxially-grown chemical-vapor-deposited layer of conducting boron-doped diamond, and is used as a DC heating element. Internally insulating both diamond anvils with sapphire support seats allows for heating and cooling of the high pressure area on the order of a few tens of seconds. This device is then used to scanmore » the phase diagram of the sample by oscillating the temperature while continuously increasing the externally applied pressure and collecting in situ time-resolved powder diffraction images. In the pressure-temperature range covered in the experiment the gadolinium sample is observed in its hcp, αSm, and dhcp phases. Under this temperature cycling, the hcp→αSm transition proceeds in discontinuous steps at points along the expected phase boundary. Additionally, the unit cell volumes of each phase deviate from the expected thermal expansion behavior just before each transition is observed from the diffraction data. From these measurements (representing only one hour of synchrotron x-ray collection time), a single-experiment equation of state and phase diagram of each phase of gadolinium is presented for the range of 0 - 10 GPa and 300 - 650 K.« less

High-pressure high-temperature phase diagram of gadolinium studied using a boron-doped heater anvil

DOE PAGES

Montgomery, J. M.; Samudrala, G. K.; Velisavljevic, N.; ...

2016-04-07

A boron-doped designer heater anvil is used in conjunction with powder x-ray diffraction to collect structural information on a sample of quasi-hydrostatically loaded gadolinium metal up to pressures above 8 GPa and 600 K. The heater anvil consists of a natural diamond anvil that has been surface modified with a homoepitaxially-grown chemical-vapor-deposited layer of conducting boron-doped diamond, and is used as a DC heating element. Internally insulating both diamond anvils with sapphire support seats allows for heating and cooling of the high pressure area on the order of a few tens of seconds. This device is then used to scanmore » the phase diagram of the sample by oscillating the temperature while continuously increasing the externally applied pressure and collecting in situ time-resolved powder diffraction images. In the pressure-temperature range covered in the experiment the gadolinium sample is observed in its hcp, αSm, and dhcp phases. Under this temperature cycling, the hcp→αSm transition proceeds in discontinuous steps at points along the expected phase boundary. Additionally, the unit cell volumes of each phase deviate from the expected thermal expansion behavior just before each transition is observed from the diffraction data. From these measurements (representing only one hour of synchrotron x-ray collection time), a single-experiment equation of state and phase diagram of each phase of gadolinium is presented for the range of 0 - 10 GPa and 300 - 650 K.« less

Philip A. Parilla | NREL

Science.gov Websites

atomic layer deposition for applications. He also manages the majority of X-ray characterization equipment at NREL, specifically X-ray diffraction and X-ray fluorescence instrumentation. Additionally, he for EERE's Hydrogen Storage program. He is also an expert in X-ray diffraction and X-ray fluorescence

Single-Crystal X-Ray Diffraction of Pyrope Garnet to 84 GPa

NASA Astrophysics Data System (ADS)

Finkelstein, G. J.; Dera, P. K.; Duffy, T. S.

2012-12-01

Garnets are characteristic minerals of many metamorphic and igneous rocks, and are also important upper-mantle constituents. Mg-rich (pyrope) garnets occur in both peridotite and eclogite compositions in the upper mantle. At high temperatures and pressures above 25 GPa, garnets transform to the perovskite structure. The post-garnet transition kinetics are sluggish, and in cold subducting slabs garnets could persist metastably at temperatures as high as 1700 K on geological timescales. These phases could add positive buoyancy to a subducting slab, inhibiting subduction. There has been minimal previous work on the 300 K compression behavior of aluminosilicate garnets at pressures higher than 10 GPa. In this work, we have collected single-crystal X-ray diffraction data on near end-member natural pyrope (Dora Maira pyrope) to 84 GPa. By extending the compression of pyrope to much higher pressures, we can better constrain the equation of state while also characterizing the structural response to such extreme pressures for the first time. Crystals were polished to ~5-10 μm in thickness, and loaded in a diamond anvil cell with gold foil and ruby balls as pressure calibrants. Helium was used as a pressure-transmitting medium. High-pressure single-crystal X-ray diffraction experiments were performed at the GSECARS 13-ID-D beamline of the Advanced Photon Source and the 12.2.2 beamline of the Advanced Light Source. Structure refinements were carried out successfully to the highest pressure using Shelx-97, extending the range over which the compression behavior of this material has been characterized by a factor of nearly three. Pyrope exhibits smooth compression behavior and no phase transitions over the investigated pressure range. A preliminary 3rd order Birch-Murnaghan equation of state was successfully fit to data up to 52 GPa. If the bulk modulus is fixed to 170 GPa, a value consistent with previous Brillouin and Ultrasonic studies, our data yields a pressure derivative of the bulk modulus of 4.33(2). The equation of state fitting will be extended to include data up to 84 GPa. The compression mechanisms observed for pyrope are consistent with those reported at lower pressures by Zhang et al., 1998. A detailed description of the structural response of pyrope to high pressures will be reported.

X-ray-diffraction study of californium metal to 16 GPa

DOE Office of Scientific and Technical Information (OSTI.GOV)

Peterson, J.R.; Benedict, U.; Dufour, C.

1983-01-01

The first series of measurements to determine the structural behavior of californium (Cf) metal under pressure has been carried out. The initial dhcp structure transformed sluggishly with increasing pressure to a fcc structure. A bulk modulus of 50(5) GPa was derived for dhcp Cf metal from the relative volume (V/V/sub 0/) data to 10 GPa.

Simulations of X-ray diffraction of shock-compressed single-crystal tantalum with synchrotron undulator sources.

PubMed

Tang, M X; Zhang, Y Y; E, J C; Luo, S N

2018-05-01

Polychromatic synchrotron undulator X-ray sources are useful for ultrafast single-crystal diffraction under shock compression. Here, simulations of X-ray diffraction of shock-compressed single-crystal tantalum with realistic undulator sources are reported, based on large-scale molecular dynamics simulations. Purely elastic deformation, elastic-plastic two-wave structure, and severe plastic deformation under different impact velocities are explored, as well as an edge release case. Transmission-mode diffraction simulations consider crystallographic orientation, loading direction, incident beam direction, X-ray spectrum bandwidth and realistic detector size. Diffraction patterns and reciprocal space nodes are obtained from atomic configurations for different loading (elastic and plastic) and detection conditions, and interpretation of the diffraction patterns is discussed.

Simulations of X-ray diffraction of shock-compressed single-crystal tantalum with synchrotron undulator sources

DOE Office of Scientific and Technical Information (OSTI.GOV)

Tang, M. X.; Zhang, Y. Y.; E, J. C.

Polychromatic synchrotron undulator X-ray sources are useful for ultrafast single-crystal diffraction under shock compression. Here, simulations of X-ray diffraction of shock-compressed single-crystal tantalum with realistic undulator sources are reported, based on large-scale molecular dynamics simulations. Purely elastic deformation, elastic–plastic two-wave structure, and severe plastic deformation under different impact velocities are explored, as well as an edge release case. Transmission-mode diffraction simulations consider crystallographic orientation, loading direction, incident beam direction, X-ray spectrum bandwidth and realistic detector size. Diffraction patterns and reciprocal space nodes are obtained from atomic configurations for different loading (elastic and plastic) and detection conditions, and interpretation of themore » diffraction patterns is discussed.« less

Pressure-induced structural transformations of the Zintl phase sodium silicide

DOE Office of Scientific and Technical Information (OSTI.GOV)

Cabrera, Raul Quesada; Salamat, Ashkan; Barkalov, Oleg I.

The high-pressure behaviour of NaSi has been studied using Raman spectroscopy and angle-dispersive synchrotron X-ray diffraction to observe the onset of structural phase transformations and potential oligomerisation into anionic Si nanoclusters with extended dimensionality. Our studies reveal a first structural transformation occurring at 8-10 GPa, followed by irreversible amorphisation above 15 GPa, suggesting the formation of Si-Si bonds with oxidation of the Si{sup -} species and reduction of Na{sup +} to metallic sodium. We have combined our experimental studies with DFT calculations to assist in the analysis of the structural behaviour of NaSi at high pressure. - Abstract: The high-pressuremore » behaviour of NaSi has been studied using Raman spectroscopy and angle-dispersive synchrotron X-ray diffraction. Our studies reveal a first structural transformation occurring at 8-10 GPa, followed by irreversible amorphisation, suggesting the formation of Si-Si bonds with oxidation of the Si{sup -} species and reduction of Na{sup +} to metallic sodium. We have combined our experimental studies with DFT calculations to assist in the analysis of the structural behaviour of NaSi at high pressure. Display Omitted« less

Coherent X-ray diffraction imaging of nanoengineered polymeric capsules

NASA Astrophysics Data System (ADS)

Erokhina, S.; Pastorino, L.; Di Lisa, D.; Kiiamov, A. G.; Faizullina, A. R.; Tayurskii, D. A.; Iannotta, S.; Erokhin, V.

2017-10-01

For the first time, nanoengineered polymeric capsules and their architecture have been studied with coherent X-ray diffraction imaging technique. The use of coherent X-ray diffraction imaging technique allowed us to analyze the samples immersed in a liquid. We report about the significant difference between polymeric capsule architectures under dry and liquid conditions.

A high-transparency, micro-patternable chip for X-ray diffraction analysis of microcrystals under native growth conditions

DOE Office of Scientific and Technical Information (OSTI.GOV)

Murray, Thomas D.; Johns Hopkins University School of Medicine, Baltimore, MD 21205; Lyubimov, Artem Y.

A highly X-ray-transparent, silicon nitride-based device has been designed and fabricated to harvest protein microcrystals for high-resolution X-ray diffraction data collection using microfocus beamlines and XFELs. Microcrystals present a significant impediment to the determination of macromolecular structures by X-ray diffraction methods. Although microfocus synchrotron beamlines and X-ray free-electron lasers (XFELs) can enable the collection of interpretable diffraction data from microcrystals, there is a need for efficient methods of harvesting small volumes (<2 µl) of microcrystals grown under common laboratory formats and delivering them to an X-ray beam source under native growth conditions. One approach that shows promise in overcoming themore » challenges intrinsic to microcrystal analysis is to pair so-called ‘fixed-target’ sample-delivery devices with microbeam-based X-ray diffraction methods. However, to record weak diffraction patterns it is necessary to fabricate devices from X-ray-transparent materials that minimize background scattering. Presented here is the design of a new micro-diffraction device consisting of three layers fabricated from silicon nitride, photoresist and polyimide film. The chip features low X-ray scattering and X-ray absorption properties, and uses a customizable blend of hydrophobic and hydrophilic surface patterns to help localize microcrystals to defined regions. Microcrystals in their native growth conditions can be loaded into the chips with a standard pipette, allowing data collection at room temperature. Diffraction data collected from hen egg-white lysozyme microcrystals (10–15 µm) loaded into the chips yielded a complete, high-resolution (<1.6 Å) data set sufficient to determine a high-quality structure by molecular replacement. The features of the chip allow the rapid and user-friendly analysis of microcrystals grown under virtually any laboratory format at microfocus synchrotron beamlines and XFELs.« less

Universal amorphous-amorphous transition in GexSe100-x glasses under pressure

NASA Astrophysics Data System (ADS)

Yildirim, Can; Micoulaut, Matthieu; Boolchand, Punit; Kantor, Innokenty; Mathon, Olivier; Gaspard, Jean-Pierre; Irifune, Tetsuo; Raty, Jean-Yves

2016-06-01

Pressure induced structural modifications in vitreous GexSe100-x (where 10 ≤ x ≤ 25) are investigated using X-ray absorption spectroscopy (XAS) along with supplementary X-ray diffraction (XRD) experiments and ab initio molecular dynamics (AIMD) simulations. Universal changes in distances and angle distributions are observed when scaled to reduced densities. All compositions are observed to remain amorphous under pressure values up to 42 GPa. The Ge-Se interatomic distances extracted from XAS data show a two-step response to the applied pressure; a gradual decrease followed by an increase at around 15-20 GPa, depending on the composition. This increase is attributed to the metallization event that can be traced with the red shift in Ge K edge energy which is also identified by the principal peak position of the structure factor. The densification mechanisms are studied in details by means of AIMD simulations and compared to the experimental results. The evolution of bond angle distributions, interatomic distances and coordination numbers are examined and lead to similar pressure-induced structural changes for any composition.

X-Ray Structure determination of the Glycine Cleavage System Protein H of Mycobacterium tuberculosis Using An Inverse Compton Synchrotron X-Ray Source

PubMed Central

Abendroth, Jan; McCormick, Michael S.; Edwards, Thomas E.; Staker, Bart; Loewen, Roderick; Gifford, Martin; Rifkin, Jeff; Mayer, Chad; Guo, Wenjin; Zhang, Yang; Myler, Peter; Kelley, Angela; Analau, Erwin; Hewitt, Stephen Nakazawa; Napuli, Alberto J.; Kuhn, Peter; Ruth, Ronald D.; Stewart, Lance J.

2010-01-01

Structural genomics discovery projects require ready access to both X-ray and NMR instrumentation which support the collection of experimental data needed to solve large numbers of novel protein structures. The most productive X-ray crystal structure determination laboratories make extensive frequent use of tunable synchrotron X-ray light to solve novel structures by anomalous diffraction methods. This requires that frozen cryo-protected crystals be shipped to large government-run synchrotron facilities for data collection. In an effort to eliminate the need to ship crystals for data collection, we have developed the first laboratory-scale synchrotron light source capable of performing many of the state-of-the-art synchrotron applications in X-ray science. This Compact Light Source is a first-in-class device that uses inverse Compton scattering to generate X-rays of sufficient flux, tunable wavelength and beam size to allow high-resolution X-ray diffraction data collection from protein crystals. We report on benchmarking tests of X-ray diffraction data collection with hen egg white lysozyme, and the successful high-resolution X-ray structure determination of the Glycine cleavage system protein H from Mycobacterium tuberculosis using diffraction data collected with the Compact Light Source X-ray beam. PMID:20364333

Femtosecond X-ray Diffraction: Applications for Laser-Irradiated Materials

DOE Office of Scientific and Technical Information (OSTI.GOV)

Wark, Justin S.

2009-09-10

Over the past few years short pulse x-ray diffraction at the nanosecond and picosecond level has become an established technique in many high-power laser laboratories for interrogating the lattice response of laser-perturbed and shocked matter, and is now finding applications in diagnosing the state of crystalline materials subject to quasi-isentropic compression. We review some of the previous results obtained in this area, for example the direct observation of coherent phonons, the first direct confirmation of the alpha-epsilon transition in shocked iron, and recent measurements indicating that the strength of matter can be measured at shock pressures exceeding a Mbar. Themore » majority of sources used to date have been laser-plasma based, with some work being performed using 3{sup rd} generation synchrotron sources. However, the development of 4{sup th} generation x-ray free-electron lasers, such as LCLS, afford many new opportunities, with pulse lengths in the femtosecond regime. The extremely low divergence and monochromatic nature of the LCLS beam make it well suited to study compressed polycrystalline matter, especially samples with small grain sizes. At extremely short pulse lengths, such that the pulse is shorter than an x-ray extinction depth traversal time, the diffraction process itself becomes time-dependent, and in certain cases the full wave-field solution will be required, particularly if the matter itself is being rapidly perturbed, as will occur if the intense x-ray radiation is used to create warm dense matter, as in recent experiments on FLASH at DESY.« less

Pressure-induced collapsed-tetragonal phase in SrCo2As2

NASA Astrophysics Data System (ADS)

Jayasekara, W. T.; Kaluarachchi, U. S.; Ueland, B. G.; Pandey, Abhishek; Lee, Y. B.; Taufour, V.; Sapkota, A.; Kothapalli, K.; Sangeetha, N. S.; Fabbris, G.; Veiga, L. S. I.; Feng, Yejun; dos Santos, A. M.; Bud'ko, S. L.; Harmon, B. N.; Canfield, P. C.; Johnston, D. C.; Kreyssig, A.; Goldman, A. I.

2015-12-01

We present high-energy x-ray diffraction data under applied pressures up to p =29 GPa , neutron diffraction measurements up to p =1.1 GPa , and electrical resistance measurements up to p =5.9 GPa , on SrCo2As2 . Our x-ray diffraction data demonstrate that there is a first-order transition between the tetragonal (T) and collapsed-tetragonal (cT) phases, with an onset above approximately 6 GPa at T =7 K . The pressure for the onset of the cT phase and the range of coexistence between the T and cT phases appears to be nearly temperature independent. The compressibility along the a axis is the same for the T and cT phases, whereas, along the c axis, the cT phase is significantly stiffer, which may be due to the formation of an As-As bond in the cT phase. Our resistivity measurements found no evidence of superconductivity in SrCo2As2 for p ≤5.9 GPa and T ≥ 1.8 K. The resistivity data also show signatures consistent with a pressure-induced phase transition for p ≳5.5 GPa. Single-crystal neutron diffraction measurements performed up to 1.1 GPa in the T phase found no evidence of stripe-type or A-type antiferromagnetic ordering down to 10 K. Spin-polarized total-energy calculations demonstrate that the cT phase is the stable phase at high pressure with a c/a ratio of 2.54. Furthermore, these calculations indicate that the cT phase of SrCo2As2 should manifest either A-type antiferromagnetic or ferromagnetic order.

Electronic and structural ground state of heavy alkali metals at high pressure

DOE PAGES

Fabbris, G.; Lim, J.; Veiga, L. S. I.; ...

2015-02-17

Here, alkali metals display unexpected properties at high pressure, including emergence of low symmetry crystal structures, that appear to occur due to enhanced electronic correlations among the otherwise nearly-free conduction electrons. We investigate the high pressure electronic and structural ground state of K, Rb, and Cs using x-ray absorption spectroscopy and x-ray diffraction measurements together with ab initio theoretical calculations. The sequence of phase transitions under pressure observed at low temperature is similar in all three heavy alkalis except for the absence of the oC84 phase in Cs. Both the experimental and theoretical results point to pressure-enhanced localization of themore » valence electrons characterized by pseudo-gap formation near the Fermi level and strong spd hybridization. Although the crystal structures predicted to host magnetic order in K are not observed, the localization process appears to drive these alkalis closer to a strongly correlated electron state.« less

The ice VII-ice X phase transition with implications for planetary interiors

NASA Astrophysics Data System (ADS)

Aarestad, B.; Frank, M. R.; Scott, H.; Bricker, M.; Prakapenka, V.

2008-12-01

A significant amount of research on the high pressure polymorphs of H2O have detailed the lattice structure and density of these phases, namely ice VI, ice VII, and ice X. These high pressure ices are noteworthy as they may comprise a considerable part of the interior of large icy planets and satellites. However, there is a dearth of data on how the incorporation of an impurity, charged or non-charged, affects the ice VII-ice X transition. This study examined the ice VII-ice X transition that occurs at approximately 62 GPa with a pure system and two select impure systems. Solutions of pure H2O, 1.6 mole percent NaCl in H2O, and 1.60 mole percent CH3OH in H2O were compressed in a diamond anvil cell (DAC). The experiments were performed at the GSECARS 13-BM-D beam line at the Advanced Photon Source at Argonne National Laboratory. Powder diffraction data of the ice samples were collected using monochromatic X-ray radiation, 0.2755 Å, and a MAR 345 online imaging system at intervals of approximately 2 GPa up to ~71.5, ~74.5, and ~68 GPa, respectively. Analyses of the data provided volume-pressure relations (at 298 K) which were used to detail the ice VII-ice X phase transition. The pressure of the phase transition, based upon an interpretation of the X-ray diffraction data, was found to vary as a function of the impurity type. Thus, the depth of the ice VII-ice X phase transition within an ice-rich planetary body can be influenced by trace-level impurities.

Anti-contamination device for cryogenic soft X-ray diffraction microscopy

DOE PAGES

Huang, Xiaojing; Miao, Huijie; Nelson, Johanna; ...

2011-05-01

Cryogenic microscopy allows one to view frozen hydrated biological and soft matter specimens with good structural preservation and a high degree of stability against radiation damage. We describe a liquid nitrogen-cooled anti-contamination device for cryogenic X-ray diffraction microscopy. The anti-contaminator greatly reduces the buildup of ice layers on the specimen due to condensation of residual water vapor in the experimental vacuum chamber. We show by coherent X-ray diffraction measurements that this leads to fivefold reduction of background scattering, which is important for far-field X-ray diffraction microscopy of biological specimens.

Synchrotron x-ray high energy PDF and tomography studies for gallium melts under high-pressure conditions

NASA Astrophysics Data System (ADS)

Liu, H.; Liu, L. L.; Li, R.; Li, L.

2015-12-01

Liquid gallium exhibits unusual and unique physical properties. A rich polymorphism and metastable modifications of solid Ga have been discovered and a number of studies of liquid gallium under high pressure conditions were reported. However, some fundamental properties, such as the equation of state (EoS) of Ga melt under extreme conditions remain unclear. To compare to the previous reports, we performed the pair distribution function (PDF) study using diamond anvil cell, in which synchrotron high-energy x-ray total scattering data, combined with reverse Monte Carlo simulation, was used to study the microstructure and EoS of liquid gallium under high pressure at room temperature conditions. The EoS of Ga melt, which was measured from synchrotron x-ray tomography method at room temperature, was used to avoid the potential relatively big errors for the density estimation from the reverse Monte Carlo simulation with the mathematical fit to the measured structure factor data. The volume change of liquid gallium have been studied as a function of pressure and temperature up to 5 GPa at 370 K using synchrotron x-ray microtomography combined with energy dispersive x-ray diffraction (EDXRD) techniques using Drickamer press. The directly measured P-V-T curves were obtained from 3D tomography reconstruction data. The existence of possible liquid-liquid phase transition regions is proposed based on the abnormal compressibility and local structure change in Ga melts.

Observation of electromigration in a Cu thin line by in situ coherent x-ray diffraction microscopy

NASA Astrophysics Data System (ADS)

Takahashi, Yukio; Nishino, Yoshinori; Furukawa, Hayato; Kubo, Hideto; Yamauchi, Kazuto; Ishikawa, Tetsuya; Matsubara, Eiichiro

2009-06-01

Electromigration (EM) in a 1-μm-thick Cu thin line was investigated by in situ coherent x-ray diffraction microscopy (CXDM). Characteristic x-ray speckle patterns due to both EM-induced voids and thermal deformation in the thin line were observed in the coherent x-ray diffraction patterns. Both parts of the voids and the deformation were successfully visualized in the images reconstructed from the diffraction patterns. This result not only represents the first demonstration of the visualization of structural changes in metallic materials by in situ CXDM but is also an important step toward studying the structural dynamics of nanomaterials using x-ray free-electron lasers in the near future.

Synchrotron X-ray Diffraction and High-Pressure Electrical Resistivity Studies for High-Tc Candidate Nd3.5Sm0.5Ni3O8

NASA Astrophysics Data System (ADS)

Uehara, Masatomo; Kobayashi, Kai; Yamamoto, Hiroki; Nakata, Akitoshi; Wakiya, Kazuhei; Umehara, Izuru; Gouchi, Jun; Uwatoko, Yoshiya

2017-11-01

Ln4Ni3O8 (Ln = La, Nd, Sm) has attracted much attention as a candidate for high-Tc superconductor due to its close structural and electrical similarities with high-Tc cuprates. However, Ln4Ni3O8 is not a superconductor and shows semiconducting behavior. Our recent work has revealed that Nd3.5Sm0.5Ni3O8 displays metallic behavior down to 20-40 K upon intercalation and subsequent deintercalation treatments with sulfur, followed by a weak semiconducting tendency at lower temperatures. A synchrotron X-ray diffraction experiment suggests that the structural change induced by sulfur treatment can be explained electrostatically by the removal of additional apical oxygen. High-pressure electrical resistivity measurements up to 8 GPa on a metallic sample show the enhancement of the semiconducting tendency at low temperatures, suggesting that the removal of additional apical oxygen is not totally completed under the present conditions of sulfur treatment.

Osmotically Induced Reversible Transitions in Lipid-DNA Mesophases

PubMed Central

Danino, Dganit; Kesselman, Ellina; Saper, Gadiel; Petrache, Horia I.; Harries, Daniel

2009-01-01

We follow the effect of osmotic pressure on isoelectric complexes that self-assemble from mixtures of DNA and mixed neutral and cationic lipids. Using small angle x-ray diffraction and freeze-fracture cryo-electron microscopy, we find that lamellar complexes known to form in aqueous solutions can reversibly transition to hexagonal mesophases under high enough osmotic stress exerted by adding a neutral polymer. Using molecular spacings derived from x-ray diffraction, we estimate the reversible osmotic pressure-volume (Π-V) work needed to induce this transition. We find that the transition free energy is comparable to the work required to elastically bend lipid layers around DNA. Consistent with this, the required work is significantly lowered by an addition of hexanol, which is known to soften lipid bilayers. Our findings not only help to resolve the free-energy contributions associated with lipid-DNA complex formation, but they also demonstrate the importance that osmotic stress can have to the macromolecular phase geometry in realistic biological environments. PMID:19348739

Experimental evidence of low-density liquid water upon rapid decompression

PubMed Central

Lin, Chuanlong; Smith, Jesse S.; Sinogeikin, Stanislav V.; Shen, Guoyin

2018-01-01

Water is an extraordinary liquid, having a number of anomalous properties which become strongly enhanced in the supercooled region. Due to rapid crystallization of supercooled water, there exists a region that has been experimentally inaccessible for studying deeply supercooled bulk water. Using a rapid decompression technique integrated with in situ X-ray diffraction, we show that a high-pressure ice phase transforms to a low-density noncrystalline (LDN) form upon rapid release of pressure at temperatures of 140–165 K. The LDN subsequently crystallizes into ice-Ic through a diffusion-controlled process. Together with the change in crystallization rate with temperature, the experimental evidence indicates that the LDN is a low-density liquid (LDL). The measured X-ray diffraction data show that the LDL is tetrahedrally coordinated with the tetrahedral network fully developed and clearly linked to low-density amorphous ices. On the other hand, there is a distinct difference in structure between the LDL and supercooled water or liquid water in terms of the tetrahedral order parameter. PMID:29440411

In situ X-Ray Diffraction of Shock-Compressed Fused Silica

NASA Astrophysics Data System (ADS)

Tracy, Sally June; Turneaure, Stefan J.; Duffy, Thomas S.

2018-03-01

Because of its widespread applications in materials science and geophysics, SiO2 has been extensively examined under shock compression. Both quartz and fused silica transform through a so-called "mixed-phase region" to a dense, low compressibility high-pressure phase. For decades, the nature of this phase has been a subject of debate. Proposed structures include crystalline stishovite, another high-pressure crystalline phase, or a dense amorphous phase. Here we use plate-impact experiments and pulsed synchrotron x-ray diffraction to examine the structure of fused silica shock compressed to 63 GPa. In contrast to recent laser-driven compression experiments, we find that fused silica adopts a dense amorphous structure at 34 GPa and below. When compressed above 34 GPa, fused silica transforms to untextured polycrystalline stishovite. Our results can explain previously ambiguous features of the shock-compression behavior of fused silica and are consistent with recent molecular dynamics simulations. Stishovite grain sizes are estimated to be ˜5 - 30 nm for compression over a few hundred nanosecond time scale.

Real-time observation of X-ray diffraction patterns with the Lixiscope

NASA Technical Reports Server (NTRS)

Chung, D. Y.; Tsang, T.; Yin, L. I.; Anderson, J. R.

1981-01-01

The feasibility of the Lixiscope (Low Intensity X-ray Imaging Scope) is demonstrated for real-time observation of transmission Laue patterns. Making use of the high-gain capability of microchannel plate (MCP) visible-light image intensifier tubes, X-ray images are converted to visible-light images by a scintillator. Pb discs are taped to the center of the Lixiscope input face, and crystal samples are held on a goniometer stage with modeling clay. With a compact size to facilitate off axis viewing, and real-time viewing to allow instantaneous response, the Lixiscope may prove useful in dynamic studies of the effects of plastic flows, stresses, high pressures, and low temperatures.

Stress distribution during cold compression of a quartz aggregate using synchrotron X-ray diffraction: Observed yielding, damage, and grain crushing: STRESS DISTRIBUTION OF QUARTZ AGGREGATE

DOE Office of Scientific and Technical Information (OSTI.GOV)

Cheung, C. S. N.; Weidner, D. J.; Li, L.

We report new experimental results that quantify the stress distribution within a quartz aggregate during pore collapse and grain crushing. The samples were probed with synchrotron X-ray diffraction as they were compressed in a multianvil deformation apparatus at room temperature from low pressure (tens of megapascal) to pressures of a few gigapascal. In such a material, stress is likely to concentrate at grain-to-grain contacts and vanish where grains are bounded by open porosity. Therefore, internal stress is likely to vary significantly from point to point in such an aggregate, and hence, it is important to understand both the heterogeneity andmore » anisotropy of such variation with respect to the externally applied stress. In our quartz aggregate (grain size of ~4 μm), the measured diffraction peaks broaden asymmetrically at low pressure (tens of megapascal), suggesting that open pores are still a dominant characteristic of grain boundaries. In contrast, a reference sample of novaculite (a highly dense quartz polycrystal, grain size of ~6–9 μm) showed virtually no peak broadening with increasing pressure. In the quartz aggregate, we observed significant deviation in the pressure-volume curves in the range of P = 400–600 MPa. We suggest that this marks the onset of grain crushing (generally denoted as P* in the rock mechanic literature), which is commonly reported to occur in sandstones at pressures of this order, in general agreement with a Hertzian analysis of fracturing at grain contacts.« less

Note: application of a pixel-array area detector to simultaneous single crystal X-ray diffraction and X-ray absorption spectroscopy measurements.

PubMed

Sun, Cheng-Jun; Zhang, Bangmin; Brewe, Dale L; Chen, Jing-Sheng; Chow, G M; Venkatesan, T; Heald, Steve M

2014-04-01

X-ray diffraction (XRD) and X-ray absorption spectroscopy (XAS) are two main x-ray techniques in synchrotron radiation facilities. In this Note, we present an experimental setup capable of performing simultaneous XRD and XAS measurements by the application of a pixel-array area detector. For XRD, the momentum transfer in specular diffraction was measured by scanning the X-ray energy with fixed incoming and outgoing x-ray angles. By selecting a small fixed region of the detector to collect the XRD signal, the rest of the area was available for collecting the x-ray fluorescence for XAS measurements. The simultaneous measurement of XRD and X-ray absorption near edge structure for Pr0.67Sr0.33MnO3 film was demonstrated as a proof of principle for future time-resolved pump-probe measurements. A static sample makes it easy to maintain an accurate overlap of the X-ray spot and laser pump beam.

X-Ray Diffraction Wafer Mapping Method for Rhombohedral Super-Hetero-Epitaxy

NASA Technical Reports Server (NTRS)

Park, Yoonjoon; Choi, Sang Hyouk; King, Glen C.; Elliott, James R.; Dimarcantonio, Albert L.

2010-01-01

A new X-ray diffraction (XRD) method is provided to acquire XY mapping of the distribution of single crystals, poly-crystals, and twin defects across an entire wafer of rhombohedral super-hetero-epitaxial semiconductor material. In one embodiment, the method is performed with a point or line X-ray source with an X-ray incidence angle approximating a normal angle close to 90 deg, and in which the beam mask is preferably replaced with a crossed slit. While the wafer moves in the X and Y direction, a narrowly defined X-ray source illuminates the sample and the diffracted X-ray beam is monitored by the detector at a predefined angle. Preferably, the untilted, asymmetric scans are of {440} peaks, for twin defect characterization.

Diffraction based method to reconstruct the spectrum of the Thomson scattering x-ray source

NASA Astrophysics Data System (ADS)

Chi, Zhijun; Yan, Lixin; Zhang, Zhen; Zhou, Zheng; Zheng, Lianmin; Wang, Dong; Tian, Qili; Wang, Wei; Nie, Zan; Zhang, Jie; Du, Yingchao; Hua, Jianfei; Shi, Jiaru; Pai, Chihao; Lu, Wei; Huang, Wenhui; Chen, Huaibi; Tang, Chuanxiang

2017-04-01

As Thomson scattering x-ray sources based on the collision of intense laser and relativistic electrons have drawn much attention in various scientific fields, there is an increasing demand for the effective methods to reconstruct the spectrum information of the ultra-short and high-intensity x-ray pulses. In this paper, a precise spectrum measurement method for the Thomson scattering x-ray sources was proposed with the diffraction of a Highly Oriented Pyrolytic Graphite (HOPG) crystal and was demonstrated at the Tsinghua Thomson scattering X-ray source. The x-ray pulse is diffracted by a 15 mm (L) ×15 mm (H)× 1 mm (D) HOPG crystal with 1° mosaic spread. By analyzing the diffraction pattern, both x-ray peak energies and energy spectral bandwidths at different polar angles can be reconstructed, which agree well with the theoretical value and simulation. The higher integral reflectivity of the HOPG crystal makes this method possible for single-shot measurement.

Diffraction based method to reconstruct the spectrum of the Thomson scattering x-ray source.

PubMed

Chi, Zhijun; Yan, Lixin; Zhang, Zhen; Zhou, Zheng; Zheng, Lianmin; Wang, Dong; Tian, Qili; Wang, Wei; Nie, Zan; Zhang, Jie; Du, Yingchao; Hua, Jianfei; Shi, Jiaru; Pai, Chihao; Lu, Wei; Huang, Wenhui; Chen, Huaibi; Tang, Chuanxiang

2017-04-01

As Thomson scattering x-ray sources based on the collision of intense laser and relativistic electrons have drawn much attention in various scientific fields, there is an increasing demand for the effective methods to reconstruct the spectrum information of the ultra-short and high-intensity x-ray pulses. In this paper, a precise spectrum measurement method for the Thomson scattering x-ray sources was proposed with the diffraction of a Highly Oriented Pyrolytic Graphite (HOPG) crystal and was demonstrated at the Tsinghua Thomson scattering X-ray source. The x-ray pulse is diffracted by a 15 mm (L) ×15 mm (H)× 1 mm (D) HOPG crystal with 1° mosaic spread. By analyzing the diffraction pattern, both x-ray peak energies and energy spectral bandwidths at different polar angles can be reconstructed, which agree well with the theoretical value and simulation. The higher integral reflectivity of the HOPG crystal makes this method possible for single-shot measurement.

Gas gun shock experiments with single-pulse x-ray phase contrast imaging and diffraction at the Advanced Photon Source

NASA Astrophysics Data System (ADS)

Luo, S. N.; Jensen, B. J.; Hooks, D. E.; Fezzaa, K.; Ramos, K. J.; Yeager, J. D.; Kwiatkowski, K.; Shimada, T.

2012-07-01

The highly transient nature of shock loading and pronounced microstructure effects on dynamic materials response call for in situ, temporally and spatially resolved, x-ray-based diagnostics. Third-generation synchrotron x-ray sources are advantageous for x-ray phase contrast imaging (PCI) and diffraction under dynamic loading, due to their high photon fluxes, high coherency, and high pulse repetition rates. The feasibility of bulk-scale gas gun shock experiments with dynamic x-ray PCI and diffraction measurements was investigated at the beamline 32ID-B of the Advanced Photon Source. The x-ray beam characteristics, experimental setup, x-ray diagnostics, and static and dynamic test results are described. We demonstrate ultrafast, multiframe, single-pulse PCI measurements with unprecedented temporal (<100 ps) and spatial (˜2 μm) resolutions for bulk-scale shock experiments, as well as single-pulse dynamic Laue diffraction. The results not only substantiate the potential of synchrotron-based experiments for addressing a variety of shock physics problems, but also allow us to identify the technical challenges related to image detection, x-ray source, and dynamic loading.

Synthesis and photocatalytic properties of TiO{sub 2} nanostructures

DOE Office of Scientific and Technical Information (OSTI.GOV)

Xia, X.H.; Liang, Y.; Wang, Z.

2008-08-04

TiO{sub 2} particles, rods, flowers and sheets were prepared by hydrothermal method via adjusting the temperature, the pressure and the concentration of TiCl{sub 4}. The as-prepared TiO{sub 2} powders were characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM), X-ray photoelectron spectroscopy (XPS), UV-vis diffuse reflectance spectra and N{sub 2} adsorption-desorption measurements. It was found that pressure is the most important factor influencing the morphology of TiO{sub 2}. The photocatalytic activity of the products was evaluated by the photodegradation of aqueous brilliant red X-3B solution under UV light. Among the as-prepared nanostructures, the flower-like TiO{sub 2}more » exhibited the highest photocatalytic activity.« less

Structural Studies on Dy to 119 GPa and Applications to Lanthanide Systematics

DOE Office of Scientific and Technical Information (OSTI.GOV)

Patterson, J; Akella, J

2005-05-31

The Rare Earth elements (REE) are known to undergo crystallographic as well as electronic structure changes with applied pressure. On increasing pressure, the trivalent lanthanides follow the sequence hcp {yields} Sm-type {yields} dhcp {yields} fcc {yields} dfcc. In this report we present room-temperature high-pressure x-ray diffraction data for Dy as well as our observations on the post-dfcc phases and concomitant volume changes in the heavy REE.

Polaron hopping in olivine phosphates studied by nuclear resonant scattering

NASA Astrophysics Data System (ADS)

Tracy, Sally June

Valence fluctuations of Fe2+ and Fe3+ were studied in a solid solution of LixFePO4 by nuclear resonant forward scattering of synchrotron x rays while the sample was heated in a diamond-anvil pressure cell. The spectra acquired at different temperatures and pressures were analyzed for the frequencies of valence changes using the Blume-Tjon model of a system with a fluctuating Hamiltonian. These frequencies were analyzed to obtain activation energies and an activation volume for polaron hopping. There was a large suppression of hopping frequency with pressure, giving an anomalously large activation volume. This large, positive value is typical of ion diffusion, which indicates correlated motions of polarons, and Li+ ions that alter the dynamics of both. In a parallel study of NaxFePO4, the interplay between sodium ordering and electron mobility was investigated using a combination of synchrotron x-ray diffraction and nuclear resonant scattering. Conventional Mossbauer spectra were collected while the sample was heated in a resistive furnace. An analysis of the temperature evolution of the spectral shapes was used to identify the onset of fast electron hopping and determine the polaron hopping rate. Synchrotron x-ray diffraction measurements were carried out in the same temperature range. Reitveld analysis of the diffraction patterns was used to determine the temperature of sodium redistribution on the lattice. The diffraction analysis also provides new information about the phase stability of the system. The temperature evolution of the iron site occupancies from the Mossbauer measurements, combined with the synchrotron diffraction results give strong evidence for a relationship between the onset of fast electron dynamics and the redistribution of sodium in the lattice. Measurements of activation barriers for polaron hopping gave fundamental insights about the correlation between electronic carriers and mobile ions. This work established that polaron-ion interactions can alter the local dynamics of electron and ion transport. These types of coupled processes may be common in many materials used for battery electrodes, and new details concerning the influence of polaron-ion interactions on the charge dynamics are relevant to optimizing their electrochemical performance.

X-ray and neutron diffraction studies of crystallinity in hydroxyapatite coatings.

PubMed

Girardin, E; Millet, P; Lodini, A

2000-02-01

To standardize industrial implant production and make comparisons between different experimental results, we have to be able to quantify the crystallinity of hydroxyapatite. Methods of measuring crystallinity ratio were developed for various HA samples before and after plasma spraying. The first series of methods uses X-ray diffraction. The advantage of these methods is that X-ray diffraction equipment is used widely in science and industry. In the second series, a neutron diffraction method is developed and the results recorded are similar to those obtained by the modified X-ray diffraction methods. The advantage of neutron diffraction is the ability to obtain measurements deep inside a component. It is a nondestructive method, owing to the very low absorption of neutrons in most materials. Copyright 2000 John Wiley & Sons, Inc.

X-ray Diffraction Gratings for Astrophysics

NASA Astrophysics Data System (ADS)

Paerels, Frits

2010-12-01

Over the past year, we have celebrated the tenth anniversary of the Chandra and XMM-Newton X-ray observatories. Both carry powerful, novel diffraction grating spectrometers, which have opened true X-ray spectroscopy for astrophysics. I will describe the design and operation of these instruments, as the background to some of the beautiful results they have produced. But these designs do not exhaust the versatility and essential simplicity of diffraction grating spectrometers, and I will discuss applications for the International X-ray Observatory IXO.

Hexafluorobenzene under Extreme Conditions.

PubMed

Pravica, Michael; Sneed, Daniel; Wang, Yonggang; Smith, Quinlan; White, Melanie

2016-03-17

We report the results from three high pressure experiments on hexafluorobenzene (C6F6). In the first experiment, Raman spectra were recorded up to 34.4 GPa. A phase transition from I → II was observed near 2 GPa. Near 8.8 GPa, a phase transition to an unreported phase (III) commenced. Above 20.6 GPa, yet another phase was observed (IV). Pressure cycling was employed to determine that, below 25.6 GPa, all pressure-induced alterations were reversible. However, at pressures above 20 GPa, dramatic spectral changes and broadening were observed at 25.6 and 34.4 GPa. The sample irreversibly changed into a soft solid with waxlike consistency when pressure was reduced to ambient and was recoverable. In the second experiment, IR spectra were collected up to 14.6 GPa. The phase transition (II → III) near 8.8 GPa was confirmed. An angular dispersive X-ray diffraction experiment was conducted to 25.6 GPa. Phase transitions above 1.4 GPa (I → II), above 5.5 GPa (II → III), above 10 GPa (III → IV), and above 15.5 GPa (IV → V) were observed. Near 25.6 GPa, long-range crystalline order was lost as the X-ray diffraction spectrum presented evidence of an amorphous solid.

DOE Office of Scientific and Technical Information (OSTI.GOV)

Chuvashova, Irina, E-mail: irina.chuvashova@gmail.com; Bayerisches Geoinstitut, University of Bayreuth, D-95440 Bayreuth; Bykova, Elena

In the present study single crystals of rhombohedral α-B were investigated under pressure to 60 GPa by means of single-crystal X-ray diffraction. The bulk modulus of α-B was found to be K=224(7) GPa (K′=3.0(3)). Measurements of interatomic distances as a function of pressure revealed that the intericosahedral two-center two-electron (2c–2e) bonds are almost as stiff as some of intraicosahedral ones. The three-center two-electron (3c–2e) intericosahedral bonds show much higher compliance compared to other bonds in α-B. The vibrational properties of α-B under pressure were investigated by Raman spectroscopy at pressures up to 160 GPa and IR spectroscopy at pressures upmore » to 53 GPa. - Graphical abstract: The rhombohedral α-B is highly incompressible and extremely stable: it maintains its crystal structure up to 160 GPa and its intericosahedral 2e2c bonds are almost as stiff as some of intraicosahedral ones. - Highlights: • Structural stability of α-B has been investigated up to 160 GPa on single crystals. • Single-crystal x-ray diffraction reveals that α-B is highly incompressible. • Compressibility of B{sub 12} icosahedra is considerably lower than that of the bulk material. • Intericosahedral 2e2c bonds are almost as stiff as some of intraicosahedral ones.« less

Bond compressibility and bond Grüneisen parameters of CdTe

NASA Astrophysics Data System (ADS)

Fornasini, P.; Grisenti, R.; Irifune, T.; Shinmei, T.; Mathon, O.; Pascarelli, S.; Rosa, A. D.

2018-06-01

Extended x-ray absorption fine structure (EXAFS) at the Cd K edge and diffraction patterns have been measured on CdTe as a function of pressure from 100 kPa (1 bar) to 5 GPa using a cell with nano-polycrystalline diamond anvils and an x-ray focussing scanning spectrometer. Three phases—zincblende (ZB), mixed cinnabar-ZB and rocksalt (RS)—are well distinguished in different pressure intervals. The bond compressibility measured by EXAFS in the ZB phase is slightly smaller than the one measured by diffraction and decreases significantly faster when the pressure increases; the difference is attributed to the effect of relative vibrations perpendicular to the Cd–Te bond. The parallel mean square relative displacement (MSRD) decreases, the perpendicular MSRD increases when the pressure increases, leading to an increasing anisotropy of relative atomic vibrations. A constant-temperature bond Grüneisen parameter (GP) has been evaluated for the ZB phase and compared with the constant-pressure bond GP measured in a previous experiment; an attempt is made to connect the bond GPs measured by EXAFS and the more familiar thermodynamic GP and mode GPs; the comparisons suggest the inadequacy of the quasi-harmonic approximation to deal with the local vibrational properties sampled by EXAFS.

High-pressure high-temperature phase diagram of gadolinium studied using a boron-doped heater anvil

NASA Astrophysics Data System (ADS)

Montgomery, J. M.; Samudrala, G. K.; Velisavljevic, N.; Vohra, Y. K.

2016-04-01

A boron-doped designer heater anvil is used in conjunction with powder x-ray diffraction to collect structural information on a sample of quasi-hydrostatically loaded gadolinium metal up to pressures above 8 GPa and 600 K. The heater anvil consists of a natural diamond anvil that has been surface modified with a homoepitaxially grown chemical-vapor-deposited layer of conducting boron-doped diamond, and is used as a DC heating element. Internally insulating both diamond anvils with sapphire support seats allows for heating and cooling of the high-pressure area on the order of a few tens of seconds. This device is then used to scan the phase diagram of the sample by oscillating the temperature while continuously increasing the externally applied pressure and collecting in situ time-resolved powder diffraction images. In the pressure-temperature range covered in this experiment, the gadolinium sample is observed in its hcp, αSm, and dhcp phases. Under this temperature cycling, the hcp → αSm transition proceeds in discontinuous steps at points along the expected phase boundary. From these measurements (representing only one hour of synchrotron x-ray collection time), a single-experiment equation of state and phase diagram of each phase of gadolinium is presented for the range of 0-10 GPa and 300-650 K.

X-Ray Sum Frequency Diffraction for Direct Imaging of Ultrafast Electron Dynamics

NASA Astrophysics Data System (ADS)

Rouxel, Jérémy R.; Kowalewski, Markus; Bennett, Kochise; Mukamel, Shaul

2018-06-01

X-ray diffraction from molecules in the ground state produces an image of their charge density, and time-resolved x-ray diffraction can thus monitor the motion of the nuclei. However, the density change of excited valence electrons upon optical excitation can barely be monitored with regular diffraction techniques due to the overwhelming background contribution of the core electrons. We present a nonlinear x-ray technique made possible by novel free electron laser sources, which provides a spatial electron density image of valence electron excitations. The technique, sum frequency generation carried out with a visible pump and a broadband x-ray diffraction pulse, yields snapshots of the transition charge densities, which represent the electron density variations upon optical excitation. The technique is illustrated by ab initio simulations of transition charge density imaging for the optically induced electronic dynamics in a donor or acceptor substituted stilbene.

Successive disorder to disorder phase transitions in ionic liquid [HMIM][BF4] under high pressure

NASA Astrophysics Data System (ADS)

Zhu, Xiang; Yuan, Chaosheng; Li, Haining; Zhu, Pinwen; Su, Lei; Yang, Kun; Wu, Jie; Yang, Guoqiang; Liu, Jing

2016-02-01

In situ high-pressure Raman spectroscopy and synchrotron X-ray diffraction have been employed to investigate the phase behavior of ionic liquid, 1-hexyl-3-methylimidazolium tetrafluoroborate ([HMIM][BF4]) under high pressure up to 20 GPa at room temperature. With increasing pressure, some characteristic bands of [HMIM][BF4] disappear, and some characteristic bands of [HMIM][BF4] display non-monotonic pressure-induced frequency shift and non-monotonic variation of full width at half-maximum. Two successive phase transitions at ˜1.7 GPa and 7.3 GPa have been corroborated by the results above. The glass transition pressure (Pg) of [HMIM][BF4] at ˜7.3 GPa has been obtained by ruby R1 line broadening measurements and analysis of synchrotron X-ray diffraction patterns, and its glass transition mechanism is also analyzed in detail. These facts are suggestive of two successive disorder to disorder phase transitions induced by compression, that is, [HMIM][BF4] serves as a superpressurized glass under the pressure above 7.3 GPa, which is similar to the glassy state at low temperature, and a compression-induced liquid to liquid phase transition in [HMIM][BF4] occurs at ˜1.7 GPa. Besides, the conformational equilibrium of the GAAA conformer and AAAA conformer was converted easily in liquid [HMIM][BF4], while it was difficult to be influenced in glassy state.

High-Pressure High-Temperature Phase Diagram of the Organic Crystal Paracetamol

NASA Astrophysics Data System (ADS)

Smith, Spencer; Montgomery, Jeffrey; Vohra, Yogesh

High-pressure high-temperature (HPHT) Raman spectroscopy studies have been performed on the organic crystal paracetamol in a diamond anvil cell utilizing boron-doped diamond as heating anvil. The HPHT data obtained from boron-doped diamond heater is cross-checked with data obtained using a standard block heater diamond anvil cell. Isobaric measurements were conducted at pressures up to 8.5 GPa and temperature up to 520 K in a number of different experiments. Solid state phase transitions from monoclinic Form I --> orthorhombic Form II were observed at various pressures and temperatures as well as transitions from Form II --> unknown Form IV. The melting temperature for paracetamol was observed to increase with increasing pressures to 8.5 GPa. Our previous angle dispersive x-ray diffraction studies at the Advanced Photon Source has confirmed the existence of two unknown crystal structures Form IV and Form V of paracetamol at high pressure and ambient temperature. The phase transformation from Form II to Form IV occurs at ~8.5 GPa and from Form IV to Form V occurs at ~11 GPa at ambient temperature. Our new data is combined with the previous ambient temperature high-pressure Raman and X- ray diffraction data to create the first HPHT phase diagram of paracetamol. Doe-NNSA Carnegie DOE Alliance Center (CDAC) under Grant Number DE-NA0002006.

Pressure effects on magnetic ground states in cobalt doped multiferroic Mn 1-xCo xWO 4

DOE PAGES

Wang, Jinchen; Ye, Feng; Chi, Songxue; ...

2016-04-28

Using x-ray and high pressure neutron diffraction, we studied the pressure effect on structural and magnetic properties of multiferroic Mn 1-xCo xWO 4 single crystals (x = 0, 0.05, 0.135 and 0.17), and compared it with the effects of doping. Both Co doping and pressure stretch the Mn-Mn chain along the c direction. At high doping level (x = 0.135 and 0.17), pressure and Co doping drive the system in a very similar way and induce a spin-flop transition for the x = 0.135 compound. In contrast, magnetic ground states at lower doping level (x = 0 and 0.05) aremore » robust against pressure but experience a pronounced change upon Co substitution. As Co introduces both chemical pressure and magnetic anisotropy into the frustrated magnetic system, our results suggest the magnetic anisotropy is the main driving force for the Co induced phase transitions at low doping level, and chemical pressure plays a more significant role at higher Co concentrations.« less

Neutron powder diffraction and high-pressure synchrotron x-ray diffraction study of tantalum nitrides

NASA Astrophysics Data System (ADS)

Feng, Lei-hao; Hu, Qi-wei; Lei, Li; Fang, Lei-ming; Qi, Lei; Zhang, Lei-lei; Pu, Mei-fang; Kou, Zi-li; Peng, Fang; Chen, Xi-ping; Xia, Yuan-hua; Kojima, Yohei; Ohfuji, Hiroaki; He, Duan-wei; Chen, Bo; Irifune, Tetsuo

2018-02-01

Not Available Project supported by the Research Foundation of Key Laboratory of Neutron Physics (Grant No. 2015BB03), the National Natural Science Foundation of China (Grant Nos. 11774247), the Science Foundation for Excellent Youth Scholars of Sichuan University (Grant No. 2015SCU04A04), and the Joint Usage/Research Center PRIUS (Ehime University, Japan) and Chinese Academy of Sciences (Grant No. 2017-BEPC-PT-000568).

Mechanism of the α -ɛ phase transformation in iron

NASA Astrophysics Data System (ADS)

Dewaele, A.; Denoual, C.; Anzellini, S.; Occelli, F.; Mezouar, M.; Cordier, P.; Merkel, S.; Véron, M.; Rausch, E.

2015-05-01

The α -Fe↔ɛ -Fe pressure-induced transformation under pure hydrostatic static compression has been characterized with in situ x-ray diffraction using α -Fe single crystals as starting samples. The forward transition starts at 14.9 GPa, and the reverse at 12 GPa, with a width of α -ɛ coexistence domain of the order of 2 GPa. The elastic stress in the sample increases in this domain, and partially relaxes after completion of the transformation. Orientation relations between parent α -Fe and child ɛ -Fe have been determined, which definitely validates the Burgers path for the direct transition. On the reverse transition, an unexpected variant selection is observed. X-ray diffraction data, complemented with ex situ microstructural observations, suggest that this selection is caused by defects and stresses accumulated during the direct transition.

Uranium oxidation kinetics monitored by in-situ X-ray diffraction

NASA Astrophysics Data System (ADS)

Zalkind, S.; Rafailov, G.; Halevy, I.; Livneh, T.; Rubin, A.; Maimon, H.; Schweke, D.

2017-03-01

The oxidation kinetics of U-0.1 wt%Cr at oxygen pressures of 150 Torr and the temperature range of 90-150 °C was studied by means of in-situ X-ray diffraction (XRD). A "breakaway" in the oxidation kinetics is found at ∼0.25 μm, turning from a parabolic to a linear rate law. At the initial stage of oxidation the growth plane of UO2(111) is the prominent one. As the oxide thickens, the growth rate of UO2(220) plane increases and both planes grow concurrently. The activation energies obtained for the oxide growth are Qparabolic = 17.5 kcal/mol and Qlinear = 19 kcal/mol. Enhanced oxidation around uranium carbide (UC) inclusions is clearly observed by scanning electron microscopy (SEM).

Three-dimensional coherent x-ray diffraction imaging of molten iron in mantle olivine at nanoscale resolution.

PubMed

Jiang, Huaidong; Xu, Rui; Chen, Chien-Chun; Yang, Wenge; Fan, Jiadong; Tao, Xutang; Song, Changyong; Kohmura, Yoshiki; Xiao, Tiqiao; Wang, Yong; Fei, Yingwei; Ishikawa, Tetsuya; Mao, Wendy L; Miao, Jianwei

2013-05-17

We report quantitative 3D coherent x-ray diffraction imaging of a molten Fe-rich alloy and crystalline olivine sample, synthesized at 6 GPa and 1800 °C, with nanoscale resolution. The 3D mass density map is determined and the 3D distribution of the Fe-rich and Fe-S phases in the olivine-Fe-S sample is observed. Our results indicate that the Fe-rich melt exhibits varied 3D shapes and sizes in the olivine matrix. This work has potential for not only improving our understanding of the complex interactions between Fe-rich core-forming melts and mantle silicate phases but also paves the way for quantitative 3D imaging of materials at nanoscale resolution under extreme pressures and temperatures.

Comparative properties of cellulose nano-crystals from native and mercerized cotton fibers

USDA-ARS?s Scientific Manuscript database

Stable aqueous suspensions of cellulose nano-crystals (CNCs) were fabricated from both native and mercerized cotton fibers by sulfuric acid hydrolysis, followed by high-pressure homogenization. Fourier Transform Infrared Spectrometry and Wide-angle X-Ray Diffraction data showed that the fibers had b...

High pressure Raman and single crystal X-ray diffraction of the alkali/calcium carbonate, shortite

NASA Astrophysics Data System (ADS)

Williams, Q. C.; Vennari, C.; O'Bannon, E. F., III

2015-12-01

Raman and synchrotron-based single crystal x-ray diffraction data have been collected on shortite (Na2Ca2(CO3)3) up to 10 GPa at 300 K. Shortite is of geological importance due to its presence in the ground-mass of kimberlites, and the alkaline-/carbon-rich character of kimberlitic eruptions. This investigation focuses on shortite's high pressure behavior and is relevant to the behavior of alkali-carbonate systems within Earth's upper mantle. X-ray data demonstrate that shortite's symmetry remains stable at high pressures—retaining orthorhombic C crystal system (Amm2) up to 10 GPa; diffraction data show a 12% volume decrease from room pressure, and a bulk modulus of 71.0(3) GPa. These also demonstrate that the c-axis is twice as compressible as the a- and b-axes. This anisotropic compression is likely due to the orientation of the relatively stiff carbonate groups, a third of which are oriented close to the plane of the a- and b-axes, c axis compression primarily involves the compaction of the 9-fold coordinate sodium and calcium polyhedral. The two distinct carbonate sites within the unit cell give rise to two Raman symmetric stretching modes of the symmetric stretch; the carbonate group stretching vibration which is close to in plane with the a- and b-axes shifts at 3.75 cm-1/GPa as opposed to the carbonate groups which is closer to in plane with the b- and c-axes which shift at 4.25 cm-1/GPa. This furthers evidence for anisotropic compression observed using x-ray diffraction--as the carbonate in plane with the a- and b-axes is compressed, the strength of oxygen bonds along the c-axis with the cations increases, thus decreasing the pressure shift of the mode. The out of plane bending vibration shifts at -0.48 cm-1/GPa, indicating an enhanced interaction of the oxygens with the cations. The multiple in plane bending modes all shift positively, as do at the low frequency lattice modes, indicating that major changes in bonding do not occur up to 10 GPa. The data collected indicates that this phase is stable at 300 K to 10 GPa. The anisotropic compaction of this alkali-rich carbonate appears to be governed by the orientation of the sodium sites, thus the behavior of alkali-rich carbonates within the kimberlitic systems is likely dependent on the bonding and local geometry of alkali cations.

Phase development in the Bi 2Sr 2CaCu 2O y system . Effects of oxygen pressure

NASA Astrophysics Data System (ADS)

List, F. A.; Hsu, H.; Cavin, O. B.; Porter, W. D.; Hubbard, C. R.; Kroeger, D. M.

1992-11-01

Studies have been undertaken using thermal analysis, in conjunction with high-temperature and room temperature X-ray diffraction, fraction, to elucidate phase relationships during thermal processing of thick films of initially phase pure Bi 2Sr 2CaCu 2O y (2212) on silver substrates in various oxygen-containing atmospheres (0.001 to 100% O 2). Exothermic events on cooling at 10°C/min from a partially liquid state vary with oxygen partial pressure and can be grouped into three sets (I-III). Set I is prominent for 0.001% and 0.1% O 2 in the range of 740-775°C and is believed to be associated with the crystallization of a Cu-free ∼ Bi 5Sr 3Ca 1 oxide phase. Set II results from the crystallization of 2212; it is observed for p(O 2)≥1.0% in the temperature range 800-870°C. Set III appears for 21% and 100% O 2 in the temperature range 880-910°C, and its origin is not clear from the results of this study. Subsequent room temperature X-ray diffraction from these samples suggests that in general high oxygen partial pressures (100% O 2) tend to favor the formation of Bi 2Sr 2CuO 6 (2201), whereas low oxygen partial pressures (0.001-0.1% O 2) lead to the formation of a Cu-free, Bi-Sr-Ca oxide phase. The 2212 phase forms at this cooling rate predominantly for intermediate oxygen partial pressures (7.6-21% O 2). High-temperature X-ray diffraction during cooling (2°C/h) from the partially liquid state shows a pronounced dependence of the order of evolution of crystalline 2212 and 2201 phases on p(O 2). For an oxygen partial pressure of 1.0% the formation of 2212 precedes that of 2201, whereas for 0.01% O 2 2201 crystallizes at a higher temperature than 2212. The implications of these results pertaining to thermal processing of thick 2212 films are discussed.

Thin Film Research. Volume 1

DTIC Science & Technology

1985-05-30

Order (FECO) ......... 23 3. X -Ray Diffraction ............................... 26 4. Transmission Electron Microscopy (TEM) ............... 26 5...remained amorphous after bombardment, as evidenced by X - ray diffraction, and showed no other changes. 0 (2) For Sb203, the crystallite size was reduced...main effect on MgF2 was the reduction in crystallite size. The films were too thir. for meaningful x - ray diffraction analysis. Durability and

X-Ray Diffraction and the Discovery of the Structure of DNA

ERIC Educational Resources Information Center

Crouse, David T.

2007-01-01

A method is described for teaching the analysis of X-ray diffraction of DNA through a series of steps utilizing the original methods used by James Watson, Francis Crick, Maurice Wilkins and Rosalind Franklin. The X-ray diffraction pattern led to the conclusion of the basic helical structure of DNA and its dimensions while basic chemical principles…

High Resolution X-Ray Diffraction of Macromolecules with Synchrotron Radiation

NASA Technical Reports Server (NTRS)

Stojanoff, Vivian; Boggon, Titus; Helliwell, John R.; Judge, Russell; Olczak, Alex; Snell, Edward H.; Siddons, D. Peter; Rose, M. Franklin (Technical Monitor)

2000-01-01

We recently combined synchrotron-based monochromatic X-ray diffraction topography methods with triple axis diffractometry and rocking curve measurements: high resolution X-ray diffraction imaging techniques, to better understand the quality of protein crystals. We discuss these methods in the light of results obtained on crystals grown under different conditions. These non destructive techniques are powerful tools in the characterization of the protein crystals and ultimately will allow to improve, develop, and understand protein crystal growth. High resolution X-ray diffraction imaging methods will be discussed in detail in light of recent results obtained on Hen Egg White Lysozyme crystals and other proteins.

Hard X-ray polarizer to enable simultaneous three-dimensional nanoscale imaging of magnetic structure and lattice strain

DOE PAGES

Logan, Jonathan; Harder, Ross; Li, Luxi; ...

2016-01-01

Recent progress in the development of dichroic Bragg coherent diffractive imaging, a new technique for simultaneous three-dimensional imaging of strain and magnetization at the nanoscale, is reported. This progress includes the installation of a diamond X-ray phase retarder at beamline 34-ID-C of the Advanced Photon Source. Here, the performance of the phase retarder for tuning X-ray polarization is demonstrated with temperature-dependent X-ray magnetic circular dichroism measurements on a gadolinium foil in transmission and on a Gd 5Si 2Ge 2crystal in diffraction geometry with a partially coherent, focused X-ray beam. Feasibility tests for dichroic Bragg coherent diffractive imaging are presented. Thesemore » tests include (1) using conventional Bragg coherent diffractive imaging to determine whether the phase retarder introduces aberrations using a nonmagnetic gold nanocrystal as a control sample, and (2) collecting coherent diffraction patterns of a magnetic Gd 5Si 2Ge 2nanocrystal with left- and right-circularly polarized X-rays. Future applications of dichroic Bragg coherent diffractive imaging for the correlation of strain and lattice defects with magnetic ordering and inhomogeneities are considered.« less

In-situ high-pressure powder X-ray diffraction study of α-zirconium phosphate.

PubMed

Readman, Jennifer E; Lennie, Alistair; Hriljac, Joseph A

2014-06-01

The high-pressure structural chemistry of α-zirconium phosphate, α-Zr(HPO4)2·H2O, was studied using in-situ high-pressure diffraction and synchrotron radiation. The layered phosphate was studied under both hydrostatic and non-hydrostatic conditions and Rietveld refinement carried out on the resulting diffraction patterns. It was found that under hydrostatic conditions no uptake of additional water molecules from the pressure-transmitting medium occurred, contrary to what had previously been observed with some zeolite materials and a layered titanium phosphate. Under hydrostatic conditions the sample remained crystalline up to 10 GPa, but under non-hydrostatic conditions the sample amorphized between 7.3 and 9.5 GPa. The calculated bulk modulus, K0 = 15.2 GPa, showed the material to be very compressible with the weak linkages in the structure of the type Zr-O-P.

Three Dimensional Variable-Wavelength X-Ray Bragg Coherent Diffraction Imaging

DOE PAGES

Cha, W.; Ulvestad, A.; Allain, M.; ...

2016-11-23

Here, we present and demonstrate a formalism by which three-dimensional (3D) Bragg x-ray coherent diffraction imaging (BCDI) can be implemented without moving the sample by scanning the energy of the incident x-ray beam. This capability is made possible by introducing a 3D Fourier transform that accounts for x-ray wavelength variability. We also demonstrate the approach by inverting coherent Bragg diffraction patterns from a gold nanocrystal measured with an x-ray energy scan. Furthermore, variable-wavelength BCDI will expand the breadth of feasible in situ 3D strain imaging experiments towards more diverse materials environments, especially where sample manipulation is difficult.

Synchrotron X-Ray Diffraction Analysis of Meteorites in Thin Section: Preliminary Results

NASA Technical Reports Server (NTRS)

Treiman, A. H.; Lanzirotti, A.; Xirouchakis, D.

2004-01-01

X-ray diffraction is the pre-eminent technique for mineral identification and structure determination, but is difficult to apply to grains in thin section, the standard meteorite preparation. Bright focused X-ray beams from synchrotrons have been used extensively in mineralogy and have been applied to extraterrestrial particles. The intensity and small spot size achievable in synchrotron X-ray beams makes them useful for study of materials in thin sections. Here, we describe Synchrotron X-ray Diffraction (SXRD) in thin section as done at the National Synchrotron Light Source, and cite examples of its value for studies of meteorites in thin section.

Three Dimensional Variable-Wavelength X-Ray Bragg Coherent Diffraction Imaging

NASA Astrophysics Data System (ADS)

Cha, W.; Ulvestad, A.; Allain, M.; Chamard, V.; Harder, R.; Leake, S. J.; Maser, J.; Fuoss, P. H.; Hruszkewycz, S. O.

2016-11-01

We present and demonstrate a formalism by which three-dimensional (3D) Bragg x-ray coherent diffraction imaging (BCDI) can be implemented without moving the sample by scanning the energy of the incident x-ray beam. This capability is made possible by introducing a 3D Fourier transform that accounts for x-ray wavelength variability. We demonstrate the approach by inverting coherent Bragg diffraction patterns from a gold nanocrystal measured with an x-ray energy scan. Variable-wavelength BCDI will expand the breadth of feasible in situ 3D strain imaging experiments towards more diverse materials environments, especially where sample manipulation is difficult.

Three Dimensional Variable-Wavelength X-Ray Bragg Coherent Diffraction Imaging.

PubMed

Cha, W; Ulvestad, A; Allain, M; Chamard, V; Harder, R; Leake, S J; Maser, J; Fuoss, P H; Hruszkewycz, S O

2016-11-25

We present and demonstrate a formalism by which three-dimensional (3D) Bragg x-ray coherent diffraction imaging (BCDI) can be implemented without moving the sample by scanning the energy of the incident x-ray beam. This capability is made possible by introducing a 3D Fourier transform that accounts for x-ray wavelength variability. We demonstrate the approach by inverting coherent Bragg diffraction patterns from a gold nanocrystal measured with an x-ray energy scan. Variable-wavelength BCDI will expand the breadth of feasible in situ 3D strain imaging experiments towards more diverse materials environments, especially where sample manipulation is difficult.

Fixation of CO 2 by chrysotile in low-pressure dry and moist carbonation: Ex-situ and in-situ characterizations

NASA Astrophysics Data System (ADS)

Larachi, Faïçal; Daldoul, Insaf; Beaudoin, Georges

2010-06-01

A detailed study of low-pressure gas-solid carbonation of chrysotile in dry and humid environments has been carried out. The evolving structure of chrysotile and its reactivity as a function of temperature (300-1200 °C), humidity (0-10 mol %) and CO 2 partial pressure (20-67 mol %), thermal preconditioning, and alkali metal doping (Li, Na, K, Cs) have been monitored through in-situ X-ray photoelectron spectroscopy, isothermal thermogravimetry/mass spectrometry, ex-situ X-ray powder diffraction, and water and nitrogen adsorption/desorption. Based on chrysotile crystalline structure and its nanofibrilar orderliness, a multistep carbonation mechanism was elaborated to explain the role of water during chrysotile partial amorphisation, formation of periclase, brucite, and hydromagnesite crystalline phases, and surface passivation thereof, during humid carbonation. The weak carbonation reactivity was rationalized in terms of incongruent CO 2 van der Waals molecular diameters with the octahedral-tetrahedral lattice constants of chrysotile. This lack of reactivity appeared to be relatively indifferent to the facilitated water crisscrossing during chrysotile core dehydroxylation/pseudo-amorphisation and surface hydroxylation induced product stabilization during humid carbonation. Thermodynamic stability domains of the species observed at low pressure have been thoroughly discussed on the basis of X-ray powder diffraction patterns and X-ray photoelectron spectroscopy evidence. The highest carbon dioxide uptake occurred at 375 °C in moist atmospheres. On the basis of chrysotile fresh N 2 BET area, nearly 15 atoms out of 100 of the surface chrysotile brucitic Mg moiety have been carbonated at this temperature which was tantamount to the carbonation of about 2.5 at. % of the total brucitic Mg moiety in chrysotile. The carbonation of brucite (Mg(OH) 2) impurities coexisting in chrysotile was minor and estimated to contribute by less than 17.6 at. % of the total converted magnesium. The presence of cesium traces (3 Cs atoms per 100 Mg atoms) was found to boost chrysotile carbonation capacity by a factor 2.7.

Probing the Hydrogen Sublattice of FeHx with High-Pressure Neutron Diffraction

NASA Astrophysics Data System (ADS)

Murphy, C. A.; Guthrie, M.; Boehler, R.; Somayazulu, M.; Fei, Y.; Molaison, J.; dos Santos, A. M.

2013-12-01

The combination of seismic, cosmochemical, and mineral physics observations have revealed that Earth's iron-rich core must contain some light elements, such as hydrogen, carbon, oxygen, silicon, and/or sulfur. Therefore, understanding the influence of these light elements on the structural, thermoelastic, and electronic properties of iron is important for constraining the composition of this remote layer of the Earth and, in turn, providing constraints on planetary differentiation and core formation models. The high-pressure structural and magnetic properties of iron hydride (FeHx) have previously been studied using synchrotron x-ray diffraction and Mössbauer spectroscopy. Such experiments revealed that the double hexagonal close-packed (dhcp) structure of FeHx is stable above a pressure of ~5 GPa and up to at least 80 GPa at 300 K [1]. In addition, dhcp-FeHx is ferromagnetic at low-pressures, but undergoes a magnetic collapse around 22 GPa [2]. X-ray experiments provide valuable insight into the properties of FeHx, but such techniques are largely sensitive to the iron component because it is difficult to detect the hydrogen sublattice with x-rays. Therefore, neutron diffraction has been used to investigate metastable FeHx, which is formed by quenching the high-pressure phase to liquid nitrogen temperatures and probing the sample at ambient pressure [3]. However, such neutron experiments have been limited to formation pressures below 10 GPa, and cannot be performed at ambient temperature. Here we present the first in-situ investigation of FeHx at 300 K using high-pressure neutron diffraction experiments performed at the Spallation Neutrons and Pressure Diffractometer (SNAP) instrument at the Spallation Neutron Source, Oak Ridge National Laboratory. In order to achieve pressures of ~50 GPa, we loaded iron samples with a hydrogen gas pressure medium into newly designed large-volume panoramic diamond-anvil cells (DACs) for neutron diffraction experiments [4; 5]. We will present the details of our DAC preparations and results of our in-situ structural refinements of dhcp-FeHx up to ~50 GPa. Together with previous investigations of the thermoelastic and electronic properties of FeHx [2; 6], we will discuss implications for the composition of Earth's iron-rich core. References: 1. N. Hirao et al. (2004), Geophys. Res. Lett., 31, L06616, doi:10.1029/2003GL019380. 2. W.L. Mao et al. (2004), Geophys. Res. Lett., 31, L15618, doi:10.1029/2004GL020541. 3. V.E. Antonov et al. (2002), J. Phys.: Condens. Matter, 14, 6427-6445, doi:10.1088/0953-8984/14/25/311. 4. M. Guthrie et al. (2013), ACA Transactions, 44, in press. 5. R. Boehler et al. (2013), High Press. Res., in press, doi:10.1080/08957959.2013.823197. 6. Y. Shibazaki et al. (2012), Earth Planet. Sci. Lett., 313-314, 79-85, doi:10.1016/j.epsl.2011.11.002.

Experimental study of planetary gases with applications to planetary interior models

NASA Technical Reports Server (NTRS)

Bell, Peter M.; Mao, Ho-Kwang

1988-01-01

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.

In-situ X-ray diffraction system using sources and detectors at fixed angular positions

DOEpatents

Gibson, David M [Voorheesville, NY; Gibson, Walter M [Voorheesville, NY; Huang, Huapeng [Latham, NY

2007-06-26

An x-ray diffraction technique for measuring a known characteristic of a sample of a material in an in-situ state. The technique includes using an x-ray source for emitting substantially divergent x-ray radiation--with a collimating optic disposed with respect to the fixed source for producing a substantially parallel beam of x-ray radiation by receiving and redirecting the divergent paths of the divergent x-ray radiation. A first x-ray detector collects radiation diffracted from the sample; wherein the source and detector are fixed, during operation thereof, in position relative to each other and in at least one dimension relative to the sample according to a-priori knowledge about the known characteristic of the sample. A second x-ray detector may be fixed relative to the first x-ray detector according to the a-priori knowledge about the known characteristic of the sample, especially in a phase monitoring embodiment of the present invention.

Rapid Sintering of Li₂O-Nb₂O₅-TiO₂ Solid Solution by Air Pressure Control and Clarification of Its Mechanism.

PubMed

Nakano, Hiromi; Kamimoto, Konatsu; Yamamoto, Takahisa; Furuta, Yoshio

2018-06-11

We first successfully synthesized Li 1+ x − y Nb 1− x −3 y Ti x +4 y O₃ (LNT) solid solutions (0.13 ≤ x ≤ 0.18, 0 ≤ y ≤ 0.06) rapidly at 1373 K for one hour under 0.35 MPa by the controlling of air pressure using an air-pressure control atmosphere furnace. The composition is a formation area of a superstructure for LNT, in which the periodical intergrowth layer was formed in the matrix, and where it can be controlled by Ti content. Therefore, the sintering time depended on Ti content, and annealing was repeated for over 24 h until a homogeneous structure was formed using a conventional electric furnace. We clarified the mechanism of the rapid sintering using various microscale to nanoscale characterization techniques: X-ray diffraction, a scanning electron microscope, a transmission electron microscope (TEM), a Cs-corrected scanning TEM equipped with electron energy-loss spectroscopy, and X-ray absorption fine structure spectroscopy.

In situ 3D-X-ray diffraction tracking of individual grains of olivine during high-pressure/ high-temperature phase transitions

NASA Astrophysics Data System (ADS)

Rosa, A. D.; Merkel, S.; Ghosh, S.; Hilairet, N.; Perrillat, J.; Mezouar, N.; Vaughan, G.

2013-12-01

The series of phase transitions between olivine, wadsleyite and ringwoodite play an essential role for large scale dynamical processes in the Earth mantle. Detailed knowledge of the microscopic mechanism at the origin of these high-pressure and high-temperature phase transformations is useful to connect global seismic observations and geodynamics. Indeed, the textures of these phases can be induced either during mantle flow or during the phase transformations and they greatly affect the characteristics of seismic wave propagation. Here, we present a new design of diamond anvil cell experiments to collect three-dimensional diffraction images and track individual grains inside a polycristalline sample at high pressure and high temperature. The instrumentation includes a new resistively heated diamond anvil cell developed at beamline ID27 of the ESRF which provided stable and homogenous temperature condition over more than 24 hours. In our experiments, the pressure is first increased up to 12 GPa at a constant temperature of T = 800 K. The temperature is then further increased to 1300 K to reach the stability field of the high-pressure polymorph. Upon further compression the transformation of olivine to its high-pressure polymorph is successfully monitored. At each pressure-temperature step and while the sample is transforming the crystallographic parameters, the orientations and positions of grains within the sample are tracked in situ using three-dimensional X-ray diffraction. This will provide important information on the micromechanical properties of olivine including orientation statistics, orientation relations between parent and daughter phases, and transformation textures at different stages of the phase transition. This in turn will help in interpreting the geophysical observations. Details of the experimental and analytical approach used in this study will be given.

The effect of exit beam phase aberrations on parallel beam coherent x-ray reconstructions

NASA Astrophysics Data System (ADS)

Hruszkewycz, S. O.; Harder, R.; Xiao, X.; Fuoss, P. H.

2010-12-01

Diffraction artifacts from imperfect x-ray windows near the sample are an important consideration in the design of coherent x-ray diffraction measurements. In this study, we used simulated and experimental diffraction patterns in two and three dimensions to explore the effect of phase imperfections in a beryllium window (such as a void or inclusion) on the convergence behavior of phasing algorithms and on the ultimate reconstruction. A predictive relationship between beam wavelength, sample size, and window position was derived to explain the dependence of reconstruction quality on beryllium defect size. Defects corresponding to this prediction cause the most damage to the sample exit wave and induce signature error oscillations during phasing that can be used as a fingerprint of experimental x-ray window artifacts. The relationship between x-ray window imperfection size and coherent x-ray diffractive imaging reconstruction quality explored in this work can play an important role in designing high-resolution in situ coherent imaging instrumentation and will help interpret the phasing behavior of coherent diffraction measured in these in situ environments.

The effect of exit beam phase aberrations on parallel beam coherent x-ray reconstructions.

PubMed

Hruszkewycz, S O; Harder, R; Xiao, X; Fuoss, P H

2010-12-01

Diffraction artifacts from imperfect x-ray windows near the sample are an important consideration in the design of coherent x-ray diffraction measurements. In this study, we used simulated and experimental diffraction patterns in two and three dimensions to explore the effect of phase imperfections in a beryllium window (such as a void or inclusion) on the convergence behavior of phasing algorithms and on the ultimate reconstruction. A predictive relationship between beam wavelength, sample size, and window position was derived to explain the dependence of reconstruction quality on beryllium defect size. Defects corresponding to this prediction cause the most damage to the sample exit wave and induce signature error oscillations during phasing that can be used as a fingerprint of experimental x-ray window artifacts. The relationship between x-ray window imperfection size and coherent x-ray diffractive imaging reconstruction quality explored in this work can play an important role in designing high-resolution in situ coherent imaging instrumentation and will help interpret the phasing behavior of coherent diffraction measured in these in situ environments.

Femtosecond X-ray Diffraction From Two-Dimensional Protein Crystals

DOE Office of Scientific and Technical Information (OSTI.GOV)

Frank, Matthias; Carlson, David B.; Hunter, Mark

2014-02-28

Here we present femtosecond x-ray diffraction patterns from two-dimensional (2-D) protein crystals using an x-ray free electron laser (XFEL). To date it has not been possible to acquire x-ray diffraction from individual 2-D protein crystals due to radiation damage. However, the intense and ultrafast pulses generated by an XFEL permits a new method of collecting diffraction data before the sample is destroyed. Utilizing a diffract-before-destroy methodology at the Linac Coherent Light Source, we observed Bragg diffraction to better than 8.5 Å resolution for two different 2-D protein crystal samples that were maintained at room temperature. These proof-of-principle results show promisemore » for structural analysis of both soluble and membrane proteins arranged as 2-D crystals without requiring cryogenic conditions or the formation of three-dimensional crystals.« less

Influence of gamma ray irradiation on stoichiometry of hydrothermally synthesized bismuth telluride nanoparticles

NASA Astrophysics Data System (ADS)

Abishek, N. S.; Naik, K. Gopalakrishna

2018-05-01

Bismuth telluride (Bi2Te3) nanoparticles were synthesized by the hydrothermal method at 200 °C for 24 h. The synthesized Bi2Te3 nanoparticles were irradiated with gamma rays at doses of 50 kGy and 100 kGy. The structural characterization of the pre-irradiated and post-irradiated samples was carried out by X-ray diffraction technique and was found to have rhombohedral phase having R3 ¯m (166) space group. The X-ray diffraction peaks were found to shift towards lower diffraction angle with gamma ray irradiation. The morphologies and compositions of the grown Bi2Te3 nanoparticles were studied using Field Emission Scanning Electron Microscope and X-ray energy dispersive analysis, respectively. The possible cause for the shift in the X-ray diffraction peaks with gamma ray irradiation has been discussed in the present work.

High Power Optical Coatings by Atomic Layer Deposition and Signatures of Laser-Induced Damage

DTIC Science & Technology

2012-08-28

diffraction angle 0 into crystal lattice spacing d by the Bragg condition, mX = 2d sin 0. Here X is the x - ray wavelength... angle x - ray diffraction (GAXRD) measurements, which were made at a fixed shallow incidence angle of 0.5°. Detector scans were done to measure the...was finished with 200 hafnia cycles m the fmal half period rather than 400. Crystallinity was measured by x - ray diffraction (XRD) with

Materials identification using a small-scale pixellated x-ray diffraction system

NASA Astrophysics Data System (ADS)

O'Flynn, D.; Crews, C.; Drakos, I.; Christodoulou, C.; Wilson, M. D.; Veale, M. C.; Seller, P.; Speller, R. D.

2016-05-01

A transmission x-ray diffraction system has been developed using a pixellated, energy-resolving detector (HEXITEC) and a small-scale, mains operated x-ray source (Amptek Mini-X). HEXITEC enables diffraction to be measured without the requirement of incident spectrum filtration, or collimation of the scatter from the sample, preserving a large proportion of the useful signal compared with other diffraction techniques. Due to this efficiency, sufficient molecular information for material identification can be obtained within 5 s despite the relatively low x-ray source power. Diffraction data are presented from caffeine, hexamine, paracetamol, plastic explosives and narcotics. The capability to determine molecular information from aspirin tablets inside their packaging is demonstrated. Material selectivity and the potential for a sample classification model is shown with principal component analysis, through which each different material can be clearly resolved.

Dynamic X-ray diffraction sampling for protein crystal positioning

DOE Office of Scientific and Technical Information (OSTI.GOV)

Scarborough, Nicole M.; Godaliyadda, G. M. Dilshan P.; Ye, Dong Hye

A sparse supervised learning approach for dynamic sampling (SLADS) is described for dose reduction in diffraction-based protein crystal positioning. Crystal centering is typically a prerequisite for macromolecular diffraction at synchrotron facilities, with X-ray diffraction mapping growing in popularity as a mechanism for localization. In X-ray raster scanning, diffraction is used to identify the crystal positions based on the detection of Bragg-like peaks in the scattering patterns; however, this additional X-ray exposure may result in detectable damage to the crystal prior to data collection. Dynamic sampling, in which preceding measurements inform the next most information-rich location to probe for image reconstruction,more » significantly reduced the X-ray dose experienced by protein crystals during positioning by diffraction raster scanning. The SLADS algorithm implemented herein is designed for single-pixel measurements and can select a new location to measure. In each step of SLADS, the algorithm selects the pixel, which, when measured, maximizes the expected reduction in distortion given previous measurements. Ground-truth diffraction data were obtained for a 5 µm-diameter beam and SLADS reconstructed the image sampling 31% of the total volume and only 9% of the interior of the crystal greatly reducing the X-ray dosage on the crystal. Furthermore, by usingin situtwo-photon-excited fluorescence microscopy measurements as a surrogate for diffraction imaging with a 1 µm-diameter beam, the SLADS algorithm enabled image reconstruction from a 7% sampling of the total volume and 12% sampling of the interior of the crystal. When implemented into the beamline at Argonne National Laboratory, without ground-truth images, an acceptable reconstruction was obtained with 3% of the image sampled and approximately 5% of the crystal. The incorporation of SLADS into X-ray diffraction acquisitions has the potential to significantly minimize the impact of X-ray exposure on the crystal by limiting the dose and area exposed for image reconstruction and crystal positioning using data collection hardware present in most macromolecular crystallography end-stations.« less

Dynamic X-ray diffraction sampling for protein crystal positioning

DOE PAGES

Scarborough, Nicole M.; Godaliyadda, G. M. Dilshan P.; Ye, Dong Hye; ...

2017-01-01

A sparse supervised learning approach for dynamic sampling (SLADS) is described for dose reduction in diffraction-based protein crystal positioning. Crystal centering is typically a prerequisite for macromolecular diffraction at synchrotron facilities, with X-ray diffraction mapping growing in popularity as a mechanism for localization. In X-ray raster scanning, diffraction is used to identify the crystal positions based on the detection of Bragg-like peaks in the scattering patterns; however, this additional X-ray exposure may result in detectable damage to the crystal prior to data collection. Dynamic sampling, in which preceding measurements inform the next most information-rich location to probe for image reconstruction,more » significantly reduced the X-ray dose experienced by protein crystals during positioning by diffraction raster scanning. The SLADS algorithm implemented herein is designed for single-pixel measurements and can select a new location to measure. In each step of SLADS, the algorithm selects the pixel, which, when measured, maximizes the expected reduction in distortion given previous measurements. Ground-truth diffraction data were obtained for a 5 µm-diameter beam and SLADS reconstructed the image sampling 31% of the total volume and only 9% of the interior of the crystal greatly reducing the X-ray dosage on the crystal. Furthermore, by usingin situtwo-photon-excited fluorescence microscopy measurements as a surrogate for diffraction imaging with a 1 µm-diameter beam, the SLADS algorithm enabled image reconstruction from a 7% sampling of the total volume and 12% sampling of the interior of the crystal. When implemented into the beamline at Argonne National Laboratory, without ground-truth images, an acceptable reconstruction was obtained with 3% of the image sampled and approximately 5% of the crystal. The incorporation of SLADS into X-ray diffraction acquisitions has the potential to significantly minimize the impact of X-ray exposure on the crystal by limiting the dose and area exposed for image reconstruction and crystal positioning using data collection hardware present in most macromolecular crystallography end-stations.« less

Dynamic X-ray diffraction sampling for protein crystal positioning

PubMed Central

Scarborough, Nicole M.; Godaliyadda, G. M. Dilshan P.; Ye, Dong Hye; Kissick, David J.; Zhang, Shijie; Newman, Justin A.; Sheedlo, Michael J.; Chowdhury, Azhad U.; Fischetti, Robert F.; Das, Chittaranjan; Buzzard, Gregery T.; Bouman, Charles A.; Simpson, Garth J.

2017-01-01

A sparse supervised learning approach for dynamic sampling (SLADS) is described for dose reduction in diffraction-based protein crystal positioning. Crystal centering is typically a prerequisite for macromolecular diffraction at synchrotron facilities, with X-ray diffraction mapping growing in popularity as a mechanism for localization. In X-ray raster scanning, diffraction is used to identify the crystal positions based on the detection of Bragg-like peaks in the scattering patterns; however, this additional X-ray exposure may result in detectable damage to the crystal prior to data collection. Dynamic sampling, in which preceding measurements inform the next most information-rich location to probe for image reconstruction, significantly reduced the X-ray dose experienced by protein crystals during positioning by diffraction raster scanning. The SLADS algorithm implemented herein is designed for single-pixel measurements and can select a new location to measure. In each step of SLADS, the algorithm selects the pixel, which, when measured, maximizes the expected reduction in distortion given previous measurements. Ground-truth diffraction data were obtained for a 5 µm-diameter beam and SLADS reconstructed the image sampling 31% of the total volume and only 9% of the interior of the crystal greatly reducing the X-ray dosage on the crystal. Using in situ two-photon-excited fluorescence microscopy measurements as a surrogate for diffraction imaging with a 1 µm-diameter beam, the SLADS algorithm enabled image reconstruction from a 7% sampling of the total volume and 12% sampling of the interior of the crystal. When implemented into the beamline at Argonne National Laboratory, without ground-truth images, an acceptable reconstruction was obtained with 3% of the image sampled and approximately 5% of the crystal. The incorporation of SLADS into X-ray diffraction acquisitions has the potential to significantly minimize the impact of X-ray exposure on the crystal by limiting the dose and area exposed for image reconstruction and crystal positioning using data collection hardware present in most macromolecular crystallography end-stations. PMID:28009558

Dynamic X-ray diffraction sampling for protein crystal positioning.

PubMed

Scarborough, Nicole M; Godaliyadda, G M Dilshan P; Ye, Dong Hye; Kissick, David J; Zhang, Shijie; Newman, Justin A; Sheedlo, Michael J; Chowdhury, Azhad U; Fischetti, Robert F; Das, Chittaranjan; Buzzard, Gregery T; Bouman, Charles A; Simpson, Garth J

2017-01-01

A sparse supervised learning approach for dynamic sampling (SLADS) is described for dose reduction in diffraction-based protein crystal positioning. Crystal centering is typically a prerequisite for macromolecular diffraction at synchrotron facilities, with X-ray diffraction mapping growing in popularity as a mechanism for localization. In X-ray raster scanning, diffraction is used to identify the crystal positions based on the detection of Bragg-like peaks in the scattering patterns; however, this additional X-ray exposure may result in detectable damage to the crystal prior to data collection. Dynamic sampling, in which preceding measurements inform the next most information-rich location to probe for image reconstruction, significantly reduced the X-ray dose experienced by protein crystals during positioning by diffraction raster scanning. The SLADS algorithm implemented herein is designed for single-pixel measurements and can select a new location to measure. In each step of SLADS, the algorithm selects the pixel, which, when measured, maximizes the expected reduction in distortion given previous measurements. Ground-truth diffraction data were obtained for a 5 µm-diameter beam and SLADS reconstructed the image sampling 31% of the total volume and only 9% of the interior of the crystal greatly reducing the X-ray dosage on the crystal. Using in situ two-photon-excited fluorescence microscopy measurements as a surrogate for diffraction imaging with a 1 µm-diameter beam, the SLADS algorithm enabled image reconstruction from a 7% sampling of the total volume and 12% sampling of the interior of the crystal. When implemented into the beamline at Argonne National Laboratory, without ground-truth images, an acceptable reconstruction was obtained with 3% of the image sampled and approximately 5% of the crystal. The incorporation of SLADS into X-ray diffraction acquisitions has the potential to significantly minimize the impact of X-ray exposure on the crystal by limiting the dose and area exposed for image reconstruction and crystal positioning using data collection hardware present in most macromolecular crystallography end-stations.

Pressure and temperature dependence of the Ce valence and c -f hybridization gap in Ce T2In5(T =Co ,Rh ,Ir ) heavy-fermion superconductors

NASA Astrophysics Data System (ADS)

Yamaoka, H.; Yamamoto, Y.; Schwier, E. F.; Honda, F.; Zekko, Y.; Ohta, Y.; Lin, J.-F.; Nakatake, M.; Iwasawa, H.; Arita, M.; Shimada, K.; Hiraoka, N.; Ishii, H.; Tsuei, K.-D.; Mizuki, J.

2015-12-01

Pressure- and temperature-induced changes in the Ce valence and c -f hybridization of the Ce115 superconductors have been studied systematically. Resonant x-ray-emission spectroscopy indicated that the increase of the Ce valence with pressure was significant for CeCoIn5, and moderate for CeIr (In0.925Cd0.075)5 . We found no abrupt change of the Ce valence in the Kondo regime for CeIr (In0.925Cd0.075)5 , which suggests that valence fluctuations are unlikely to mediate the superconductivity in this material. X-ray-diffraction results were consistent with the pressure-induced change in the Ce valence. High-resolution photoelectron spectroscopy revealed a temperature-dependent reduction of the spectral intensity at the Fermi level, indicating enhanced c -f hybridization on cooling.

High pressure X-ray diffraction studies on Bi2-xSbxTe3 (x=0,1,2) materials

NASA Astrophysics Data System (ADS)

Jacobsen, Matthew; Kumar, Ravhi; Cornelius, Andrew

2007-06-01

Recently Bi2Te3 based thermoelectric materials have gained importance due to their high thermoelectric figure of merit in thin films [3]. Pressure tuning of the thermoelectric figure of merit has been reported for several materials [1],[2]. In order to investigate the bulk properties of Bi2Te3, Sb2Te3, and their solid solution in detail, we have performed structural studies up to 20 GPa. Our diffraction results show that all three compounds transform from the ambient pressure structure to a high pressure phase between 5 and 7 GPa. Details of the results will be discussed in this presentation. [1]Chen, G., Dresselhaus, M.S., Dresselhaus, G., Fleurial, J.-P., and Caillat, T. Recent developments in themoelectric materials. International Materials Reviews, 48, 45-66 (2003). [2]Rowe, D.M. CRC Handbook of Thermoelectric Materials. CRC Press, 1995. [3]Venkatasubramanian, R., Silvola, E., Colpitts, T., and O'Quinn, B. Thin-film thermoelectric devices with high room-temperature figures of merit. Nature, 413, 597-602, 2001.

In situ X-ray diffraction measurement of shock-wave-driven twinning and lattice dynamics

NASA Astrophysics Data System (ADS)

Wehrenberg, C. E.; McGonegle, D.; Bolme, C.; Higginbotham, A.; Lazicki, A.; Lee, H. J.; Nagler, B.; Park, H.-S.; Remington, B. A.; Rudd, R. E.; Sliwa, M.; Suggit, M.; Swift, D.; Tavella, F.; Zepeda-Ruiz, L.; Wark, J. S.

2017-10-01

Pressure-driven shock waves in solid materials can cause extreme damage and deformation. Understanding this deformation and the associated defects that are created in the material is crucial in the study of a wide range of phenomena, including planetary formation and asteroid impact sites, the formation of interstellar dust clouds, ballistic penetrators, spacecraft shielding and ductility in high-performance ceramics. At the lattice level, the basic mechanisms of plastic deformation are twinning (whereby crystallites with a mirror-image lattice form) and slip (whereby lattice dislocations are generated and move), but determining which of these mechanisms is active during deformation is challenging. Experiments that characterized lattice defects have typically examined the microstructure of samples after deformation, and so are complicated by post-shock annealing and reverberations. In addition, measurements have been limited to relatively modest pressures (less than 100 gigapascals). In situ X-ray diffraction experiments can provide insights into the dynamic behaviour of materials, but have only recently been applied to plasticity during shock compression and have yet to provide detailed insight into competing deformation mechanisms. Here we present X-ray diffraction experiments with femtosecond resolution that capture in situ, lattice-level information on the microstructural processes that drive shock-wave-driven deformation. To demonstrate this method we shock-compress the body-centred-cubic material tantalum—an important material for high-energy-density physics owing to its high shock impedance and high X-ray opacity. Tantalum is also a material for which previous shock compression simulations and experiments have provided conflicting information about the dominant deformation mechanism. Our experiments reveal twinning and related lattice rotation occurring on the timescale of tens of picoseconds. In addition, despite the common association between twinning and strong shocks, we find a transition from twinning to dislocation-slip-dominated plasticity at high pressure (more than 150 gigapascals), a regime that recovery experiments cannot accurately access. The techniques demonstrated here will be useful for studying shock waves and other high-strain-rate phenomena, as well as a broad range of processes induced by plasticity.

In situ X-ray diffraction measurement of shock-wave-driven twinning and lattice dynamics

DOE Office of Scientific and Technical Information (OSTI.GOV)

Wehrenberg, C. E.; McGonegle, D.; Bolme, C.

We report that pressure-driven shock waves in solid materials can cause extreme damage and deformation. Understanding this deformation and the associated defects that are created in the material is crucial in the study of a wide range of phenomena, including planetary formation and asteroid impact sites, the formation of interstellar dust clouds, ballistic penetrators, spacecraft shielding and ductility in high-performance ceramics. At the lattice level, the basic mechanisms of plastic deformation are twinning (whereby crystallites with a mirror-image lattice form) and slip (whereby lattice dislocations are generated and move), but determining which of these mechanisms is active during deformation ismore » challenging. Experiments that characterized lattice defects have typically examined the microstructure of samples after deformation, and so are complicated by post-shock annealing and reverberations. In addition, measurements have been limited to relatively modest pressures (less than 100 gigapascals). In situ X-ray diffraction experiments can provide insights into the dynamic behaviour of materials, but have only recently been applied to plasticity during shock compression and have yet to provide detailed insight into competing deformation mechanisms. Here we present X-ray diffraction experiments with femtosecond resolution that capture in situ, lattice-level information on the microstructural processes that drive shock-wave-driven deformation. To demonstrate this method we shock-compress the body-centred-cubic material tantalum—an important material for high-energy-density physics owing to its high shock impedance and high X-ray opacity. Tantalum is also a material for which previous shock compression simulations and experiments have provided conflicting information about the dominant deformation mechanism. Our experiments reveal twinning and related lattice rotation occurring on the timescale of tens of picoseconds. In addition, despite the common association between twinning and strong shocks, we find a transition from twinning to dislocation-slip-dominated plasticity at high pressure (more than 150 gigapascals), a regime that recovery experiments cannot accurately access. Lastly, the techniques demonstrated here will be useful for studying shock waves and other high-strain-rate phenomena, as well as a broad range of processes induced by plasticity.« less

In situ X-ray diffraction measurement of shock-wave-driven twinning and lattice dynamics

DOE PAGES

Wehrenberg, C. E.; McGonegle, D.; Bolme, C.; ...

2017-10-25

We report that pressure-driven shock waves in solid materials can cause extreme damage and deformation. Understanding this deformation and the associated defects that are created in the material is crucial in the study of a wide range of phenomena, including planetary formation and asteroid impact sites, the formation of interstellar dust clouds, ballistic penetrators, spacecraft shielding and ductility in high-performance ceramics. At the lattice level, the basic mechanisms of plastic deformation are twinning (whereby crystallites with a mirror-image lattice form) and slip (whereby lattice dislocations are generated and move), but determining which of these mechanisms is active during deformation ismore » challenging. Experiments that characterized lattice defects have typically examined the microstructure of samples after deformation, and so are complicated by post-shock annealing and reverberations. In addition, measurements have been limited to relatively modest pressures (less than 100 gigapascals). In situ X-ray diffraction experiments can provide insights into the dynamic behaviour of materials, but have only recently been applied to plasticity during shock compression and have yet to provide detailed insight into competing deformation mechanisms. Here we present X-ray diffraction experiments with femtosecond resolution that capture in situ, lattice-level information on the microstructural processes that drive shock-wave-driven deformation. To demonstrate this method we shock-compress the body-centred-cubic material tantalum—an important material for high-energy-density physics owing to its high shock impedance and high X-ray opacity. Tantalum is also a material for which previous shock compression simulations and experiments have provided conflicting information about the dominant deformation mechanism. Our experiments reveal twinning and related lattice rotation occurring on the timescale of tens of picoseconds. In addition, despite the common association between twinning and strong shocks, we find a transition from twinning to dislocation-slip-dominated plasticity at high pressure (more than 150 gigapascals), a regime that recovery experiments cannot accurately access. Lastly, the techniques demonstrated here will be useful for studying shock waves and other high-strain-rate phenomena, as well as a broad range of processes induced by plasticity.« less

Fixture for supporting and aligning a sample to be analyzed in an x-ray diffraction apparatus

DOEpatents

Green, L.A.; Heck, J.L. Jr.

1985-04-23

A fixture is provided for supporting and aligning small samples of material on a goniometer for x-ray diffraction analysis. A sample-containing capillary is accurately positioned for rotation in the x-ray beam by selectively adjusting the fixture to position the capillary relative to the x and y axes thereof to prevent wobble and position the sample along the z axis or the axis of rotation. By employing the subject fixture relatively small samples of materials can be analyzed in an x-ray diffraction apparatus previously limited to the analysis of much larger samples.

Fixture for supporting and aligning a sample to be analyzed in an X-ray diffraction apparatus

DOEpatents

Green, Lanny A.; Heck, Jr., Joaquim L.

1987-01-01

A fixture is provided for supporting and aligning small samples of material on a goniometer for X-ray diffraction analysis. A sample-containing capillary is accurately positioned for rotation in the X-ray beam by selectively adjusting the fixture to position the capillary relative to the x and y axes thereof to prevent wobble and position the sample along the z axis or the axis of rotation. By employing the subject fixture relatively small samples of materials can be analyzed in an X-ray diffraction apparatus previously limited to the analysis of much larger samples.

Pressure-induced kinetics of the α to ω transition in zirconium

DOE Office of Scientific and Technical Information (OSTI.GOV)

Jacobsen, M. K.; Velisavljevic, N., E-mail: nenad@lanl.gov; Sinogeikin, S. V.

Diamond anvil cells (DAC) coupled with x-ray diffraction (XRD) measurements are one of the primary techniques for investigating structural stability of materials at high pressure-temperature (P-T) conditions. DAC-XRD has been predominantly used to resolve structural information at set P-T conditions and, consequently, provides P-T phase diagram information on a broad range of materials. With advances in large scale synchrotron x-ray facilities and corresponding x-ray diagnostic capabilities, it is now becoming possible to perform sub-second time resolved measurements on micron sized DAC samples. As a result, there is an opportunity to gain valuable information about the kinetics of structural phase transformationsmore » and extend our understanding of material behavior at high P-T conditions. Using DAC-XRD time resolved measurements, we have investigated the kinetics of the α to ω transformation in zirconium. We observe a clear time and pressure dependence in the martensitic α-ω transition as a function of pressure-jump, i.e., drive pressure. The resulting data are fit using available kinetics models, which can provide further insight into transformation mechanism that influence transformation kinetics. Our results help shed light on the discrepancies observed in previous measurements of the α-ω transition pressure in zirconium.« less

Pressure-induced kinetics of the α to ω transition in zirconium

DOE PAGES

Jacobsen, M. K.; Velisavljevic, N.; Sinogeikin, S. V.

2015-07-13

Diamond anvil cells (DAC) coupled with x-ray diffraction (XRD) measurements are one of the primary techniques for investigating structural stability of materials at high pressure-temperature (P-T) conditions. DAC-XRD has been predominantly used to resolve structural information at set P-T conditions and, consequently, provides P-T phase diagram information on a broad range of materials. With advances in large scale synchrotron x-ray facilities and corresponding x-ray diagnostic capabilities, it is now becoming possible to perform sub-second time resolved measurements on micron sized DAC samples. As a result, there is an opportunity to gain valuable information about the kinetics of structural phase transformationsmore » and extend our understanding of material behavior at high P-T conditions. Using DAC-XRD time resolved measurements, we have investigated the kinetics of the α to ω transformation in zirconium. We observe a clear time and pressure dependence in the martensitic α-ω transition as a function of pressure-jump, i.e., drive pressure. The resulting data are fit using available kinetics models, which can provide further insight into transformation mechanism that influence transformation kinetics. Our results help shed light on the discrepancies observed in previous measurements of the α-ω transition pressure in zirconium.« less

Effect of chemical pressure on competition and cooperation between polar and antiferrodistortive distortions in sodium niobate

NASA Astrophysics Data System (ADS)

Jauhari, Mrinal; Mishra, S. K.; Mittal, R.; Sastry, P. U.; Chaplot, S. L.

2017-12-01

We present results obtained from a combination of dielectric and x-ray diffraction measurements for compositional design of (1 -x )NaNb O3-x BaTi O3(NNBT x ) , which can induce interferroelectric phase transitions. Anomalies are observed in dielectric measurements performed for various compositions at 300 K, as well as at different temperatures for NNBT03. We observed the appearance(disappearance) of the superlattice reflections along with change in the intensities of the main perovskite peaks in the powder x-ray diffraction data, which provide clear evidences for structural phase transitions with composition and temperature. We found that increasing the concentration of BaTi O3 leads to the suppression of out-of-phase rotation of octahedra and an increment in tetragonality (c /a ratio), which promotes the polar mode at room temperature. The temperature-dependent powder diffraction study shows that the ferroelectric rhombohedral phase of pure sodium niobate gets suppressed for the composition x =0.03 , and the monoclinic phase C c gets stabilized at low temperature. The monoclinic phase is believed to provide for a flexible polarization rotation and is considered to be directly linked to the high-performance piezoelectricity in materials due to presence of more easy axes for spontaneous polarizations than the rhombohedral phase.

Density Determination of Metallic Melts from Diffuse X-Ray Scattering

NASA Astrophysics Data System (ADS)

Brauser, N.; Davis, A.; Greenberg, E.; Prakapenka, V. B.; Campbell, A.

2017-12-01

Liquids comprise several important structural components of the deep Earth, for example, the present outer core and a hypothesized magma ocean early in Earth history. However, the physical properties of the constituent materials of these structures at high pressures and temperatures are less well constrained than their crystalline counterparts. Determination of the physical properties of these liquids can inform geophysical models of the composition and structure of the Earth, but methods for studying the physical properties of liquids at high pressure and temperatures are underdeveloped. One proposed method for direct determination of density of a melt requires analysis of the diffuse scattered X-ray signal of the liquid. Among the challenges to applying this technique to high-pressure melts within a laser heated diamond anvil cell are the low signal-to-noise ratio and overlapping diffraction peaks from the crystalline components of the sample assembly interfering with the diffuse scattering from the liquid. Recent advances in instrumentation at synchrotron X-ray sources have made this method more accessible for determination of density of melted material. In this work we present the technique and report the densities of three high-pressure melts of the FCC metals iron, nickel, and gold derived from diffuse scattered X-ray spectra collected from in situ laser-heated diamond anvil cell synchrotron experiments. The results are compared to densities derived from shock wave experiments.

JMFA2—a graphically interactive Java program that fits microfibril angle X-ray diffraction data

Treesearch

Steve P. Verrill; David E. Kretschmann; Victoria L. Herian

2006-01-01

X-ray diffraction techniques have the potential to decrease the time required to determine microfibril angles dramatically. In this paper, we discuss the latest version of a curve-fitting toll that permits us to reduce the time required to evaluate MFA X-ray diffraction patterns. Further, because this tool reflects the underlying physics more accurately than existing...

Carbon nanohorns under cold compression to 40 GPa: Raman scattering and X-ray diffraction experiments

NASA Astrophysics Data System (ADS)

Li, Bo; Nan, Yanli; Zhao, Xiang; Song, Xiaolong; Li, Haining; Wu, Jie; Su, Lei

2017-11-01

We report a high-pressure behavior of carbon nanohorns (CNHs) to 40 GPa at ambient temperature by in situ Raman spectroscopy and synchrotron radiation x-ray diffraction (XRD) in a diamond anvil cell. In Raman measurement, multiple structural transitions are observed. In particular, an additional band at ˜1540 cm-1 indicative of sp3 bonding is shown above 35 GPa, but it reverses upon releasing pressure, implying the formation of a metastable carbon phase having both sp2 and sp3 bonds. Raman frequencies of all bands (G, 2D, D + G, and 2D') are dependent upon pressure with respective pressure coefficients, among which the value for the G band is as small as ˜2.65 cm-1 GPa-1 above 10 GPa, showing a superior high-pressure structural stability. Analysis based on mode Grüneisen parameter demonstrates the similarity of high-pressure behavior between CNHs and single-walled carbon nanotubes. Furthermore, the bulk modulus and Grüneisen parameter for the G band of CNHs are calculated to be ˜33.3 GPa and 0.1, respectively. In addition, XRD data demonstrate that the structure of post-graphite phase derives from surface nanohorns. Based on topological defects within conical graphene lattice, a reasonable transformation route from nanohorns to the post-graphite phase is proposed.

High-pressure X-ray diffraction, Raman, and computational studies of MgCl2 up to 1 Mbar: Extensive pressure stability of the β-MgCl2 layered structure.

PubMed

Stavrou, Elissaios; Yao, Yansun; Zaug, Joseph M; Bastea, Sorin; Kalkan, Bora; Konôpková, Zuzana; Kunz, Martin

2016-08-12

Magnesium chloride (MgCl2) with the rhombohedral layered CdCl2-type structure (α-MgCl2) has been studied experimentally using synchrotron angle-dispersive powder x-ray diffraction and Raman spectroscopy using a diamond-anvil cell up to 100 GPa at room temperature and theoretically using first-principles density functional calculations. The results reveal a pressure-induced second-order structural phase transition to a hexagonal layered CdI2-type structure (β-MgCl2) at 0.7 GPa: the stacking sequence of the Cl anions are altered resulting in a reduction of the c-axis length. Theoretical calculations confirm this phase transition sequence and the calculated transition pressure is in excellent agreement with the experiment. Lattice dynamics calculations also reproduce the experimental Raman spectra measured for the ambient and high-pressure phase. According to our experimental results MgCl2 remains in a 2D layered phase up to 100 GPa and further, the 6-fold coordination of Mg cations is retained. Theoretical calculations of relative enthalpy suggest that this extensive pressure stability is due to a low enthalpy of the layered structure ruling out kinetic barrier effects. This observation is unusual, as it contradicts with the general structural behavior of highly compressed AB2 compounds.

High-pressure X-ray diffraction, Raman, and computational studies of MgCl 2 up to 1 Mbar: Extensive pressure stability of the β-MgCl 2 layered structure

DOE PAGES

Stavrou, Elissaios; Yao, Yansun; Zaug, Joseph M.; ...

2016-08-12

We studied magnesium chloride (MgCl 2) with the rhombohedral layered CdCl 2-type structure (α-MgCl 2), experimentally, using synchrotron angle-dispersive powder x-ray diffraction and Raman spectroscopy using a diamond-anvil cell up to 100 GPa at room temperature and theoretically using first-principles density functional calculations. Our results reveal a pressure-induced second-order structural phase transition to a hexagonal layered CdI 2-type structure (β-MgCl 2) at 0.7 GPa: the stacking sequence of the Cl anions are altered resulting in a reduction of the c-axis length. Theoretical calculations confirm this phase transition sequence and the calculated transition pressure is in excellent agreement with the experiment.more » Lattice dynamics calculations also reproduce the experimental Raman spectra measured for the ambient and high-pressure phase. According to our experimental results MgCl 2 remains in a 2D layered phase up to 100 GPa and further, the 6-fold coordination of Mg cations is retained. Theoretical calculations of relative enthalpy suggest that this extensive pressure stability is due to a low enthalpy of the layered structure ruling out kinetic barrier effects. Our observation is unusual, as it contradicts with the general structural behavior of highly compressed AB 2 compounds.« less

Structural Transitions in Nanosized Zn0.97Al0.03O Powders under High Pressure Analyzed by in Situ Angle-Dispersive X-ray Diffraction

PubMed Central

Lin, Chih-Ming; Liu, Hsin-Tzu; Zhong, Shi-Yao; Hsu, Chia-Hung; Chiu, Yi-Te; Tai, Ming-Fong; Juang, Jenh-Yih; Chuang, Yu-Chun; Liao, Yen-Fa

2016-01-01

Nanosized aluminum-doped zinc oxide Zn1−xAlxO (AZO) powders (AZO-NPs) with x = 0.01, 0.03, 0.06, 0.09 and 0.11 were synthesized by chemical precipitation method. The thermogravimetric analysis (TGA) indicated that the precursors were converted to oxides from hydroxides near 250 °C, which were then heated to 500 °C for subsequent thermal processes to obtain preliminary powders. The obtained preliminary powders were then calcined at 500 °C for three hours. The structure and morphology of the products were measured and characterized by angle-dispersive X-ray diffraction (ADXRD) and scanning electron microscopy (SEM). ADXRD results showed that AZO-NPs with Al content less than 11% exhibited würtzite zinc oxide structure and there was no other impurity phase in the AZO-NPs, suggesting substitutional doping of Al on Zn sites. The Zn0.97Al0.03O powders (A3ZO-NPs) with grain size of about 21.4 nm were used for high-pressure measurements. The in situ ADXRD measurements revealed that, for loading run, the pressure-induced würtzite (B4)-to-rocksalt (B1) structural phase transition began at 9.0(1) GPa. Compared to the predicted phase-transition pressure of ~12.7 GPa for pristine ZnO nanocrystals of similar grain size (~21.4 nm), the transition pressure for the present A3ZO-NPs exhibited a reduction of ~3.7 GPa. The significant reduction in phase-transition pressure is attributed to the effects of highly selective site occupation, namely Zn2+ and Al3+, were mainly found in tetrahedral and octahedral sites, respectively. PMID:28773683

A high-transparency, micro-patternable chip for X-ray diffraction analysis of microcrystals under native growth conditions

DOE PAGES

Murray, Thomas D.; Lyubimov, Artem Y.; Ogata, Craig M.; ...

2015-08-11

Microcrystals present a significant impediment to the determination of macromolecular structures by X-ray diffraction methods. Although microfocus synchrotron beamlines and X-ray free-electron lasers (XFELs) can enable the collection of interpretable diffraction data from microcrystals, there is a need for efficient methods of harvesting small volumes (<2 µl) of microcrystals grown under common laboratory formats and delivering them to an X-ray beam source under native growth conditions. One approach that shows promise in overcoming the challenges intrinsic to microcrystal analysis is to pair so-called `fixed-target' sample-delivery devices with microbeam-based X-ray diffraction methods. However, to record weak diffraction patterns it is necessarymore » to fabricate devices from X-ray-transparent materials that minimize background scattering. Presented here is the design of a new micro-diffraction device consisting of three layers fabricated from silicon nitride, photoresist and polyimide film. The chip features low X-ray scattering and X-ray absorption properties, and uses a customizable blend of hydrophobic and hydrophilic surface patterns to help localize microcrystals to defined regions. Microcrystals in their native growth conditions can be loaded into the chips with a standard pipette, allowing data collection at room temperature. Diffraction data collected from hen egg-white lysozyme microcrystals (10–15 µm) loaded into the chips yielded a complete, high-resolution (<1.6 Å) data set sufficient to determine a high-quality structure by molecular replacement. In addition, the features of the chip allow the rapid and user-friendly analysis of microcrystals grown under virtually any laboratory format at microfocus synchrotron beamlines and XFELs.« less

A high-transparency, micro-patternable chip for X-ray diffraction analysis of microcrystals under native growth conditions

DOE Office of Scientific and Technical Information (OSTI.GOV)

Murray, Thomas D.; Lyubimov, Artem Y.; Ogata, Craig M.

Microcrystals present a significant impediment to the determination of macromolecular structures by X-ray diffraction methods. Although microfocus synchrotron beamlines and X-ray free-electron lasers (XFELs) can enable the collection of interpretable diffraction data from microcrystals, there is a need for efficient methods of harvesting small volumes (<2 µl) of microcrystals grown under common laboratory formats and delivering them to an X-ray beam source under native growth conditions. One approach that shows promise in overcoming the challenges intrinsic to microcrystal analysis is to pair so-called `fixed-target' sample-delivery devices with microbeam-based X-ray diffraction methods. However, to record weak diffraction patterns it is necessarymore » to fabricate devices from X-ray-transparent materials that minimize background scattering. Presented here is the design of a new micro-diffraction device consisting of three layers fabricated from silicon nitride, photoresist and polyimide film. The chip features low X-ray scattering and X-ray absorption properties, and uses a customizable blend of hydrophobic and hydrophilic surface patterns to help localize microcrystals to defined regions. Microcrystals in their native growth conditions can be loaded into the chips with a standard pipette, allowing data collection at room temperature. Diffraction data collected from hen egg-white lysozyme microcrystals (10–15 µm) loaded into the chips yielded a complete, high-resolution (<1.6 Å) data set sufficient to determine a high-quality structure by molecular replacement. In addition, the features of the chip allow the rapid and user-friendly analysis of microcrystals grown under virtually any laboratory format at microfocus synchrotron beamlines and XFELs.« less

A high-transparency, micro-patternable chip for X-ray diffraction analysis of microcrystals under native growth conditions

DOE Office of Scientific and Technical Information (OSTI.GOV)

Murray, Thomas D.; Lyubimov, Artem Y.; Ogata, Craig M.

Microcrystals present a significant impediment to the determination of macromolecular structures by X-ray diffraction methods. Although microfocus synchrotron beamlines and X-ray free-electron lasers (XFELs) can enable the collection of interpretable diffraction data from microcrystals, there is a need for efficient methods of harvesting small volumes (<2µl) of microcrystals grown under common laboratory formats and delivering them to an X-ray beam source under native growth conditions. One approach that shows promise in overcoming the challenges intrinsic to microcrystal analysis is to pair so-called `fixed-target' sample-delivery devices with microbeam-based X-ray diffraction methods. However, to record weak diffraction patterns it is necessary tomore » fabricate devices from X-ray-transparent materials that minimize background scattering. Presented here is the design of a new micro-diffraction device consisting of three layers fabricated from silicon nitride, photoresist and polyimide film. The chip features low X-ray scattering and X-ray absorption properties, and uses a customizable blend of hydrophobic and hydrophilic surface patterns to help localize microcrystals to defined regions. Microcrystals in their native growth conditions can be loaded into the chips with a standard pipette, allowing data collection at room temperature. Diffraction data collected from hen egg-white lysozyme microcrystals (10–15µm) loaded into the chips yielded a complete, high-resolution (<1.6Å) data set sufficient to determine a high-quality structure by molecular replacement. The features of the chip allow the rapid and user-friendly analysis of microcrystals grown under virtually any laboratory format at microfocus synchrotron beamlines and XFELs.« less

A high-transparency, micro-patternable chip for X-ray diffraction analysis of microcrystals under native growth conditions

PubMed Central

Murray, Thomas D.; Lyubimov, Artem Y.; Ogata, Craig M.; Vo, Huy; Uervirojnangkoorn, Monarin; Brunger, Axel T.; Berger, James M.

2015-01-01

Microcrystals present a significant impediment to the determination of macromolecular structures by X-ray diffraction methods. Although microfocus synchrotron beamlines and X-ray free-electron lasers (XFELs) can enable the collection of interpretable diffraction data from microcrystals, there is a need for efficient methods of harvesting small volumes (<2 µl) of microcrystals grown under common laboratory formats and delivering them to an X-ray beam source under native growth conditions. One approach that shows promise in overcoming the challenges intrinsic to microcrystal analysis is to pair so-called ‘fixed-target’ sample-delivery devices with microbeam-based X-ray diffraction methods. However, to record weak diffraction patterns it is necessary to fabricate devices from X-ray-transparent materials that minimize background scattering. Presented here is the design of a new micro-diffraction device consisting of three layers fabricated from silicon nitride, photoresist and polyimide film. The chip features low X-ray scattering and X-ray absorption properties, and uses a customizable blend of hydrophobic and hydrophilic surface patterns to help localize microcrystals to defined regions. Microcrystals in their native growth conditions can be loaded into the chips with a standard pipette, allowing data collection at room temperature. Diffraction data collected from hen egg-white lysozyme microcrystals (10–15 µm) loaded into the chips yielded a complete, high-resolution (<1.6 Å) data set sufficient to determine a high-quality structure by molecular replacement. The features of the chip allow the rapid and user-friendly analysis of microcrystals grown under virtually any laboratory format at microfocus synchrotron beamlines and XFELs. PMID:26457423

Shear Deformation of Fe Polycrystals in the Rotational Diamond Anvil Cell

NASA Astrophysics Data System (ADS)

Merkel, S.; Lincot, A.; Nisr, C.; Hanfland, M.; Zerr, A.

2014-12-01

For many years, experiments are being developed for performing deformation experiments under lower mantle conditions. They include methods such as the Deformation-DIA (Wang et al, 2003) or radial x-ray diffraction in the diamond anvil cell (Merkel et al, 2002). However, the strain applied to the sample is typically limited to about 40%. This can be an issue for studying effects of large deformation or, for the case of diamond anvil cells, applying actual plastic strain at megabar pressures. The issue can be solved using apparatus such as the Rotational-Drickamer (RDA) (e.g. Yamazaki and Karato, 2001). However, the RDA offers limited diffraction access to the sample and operating pressures do not reach those of the lower mantle.In this abstract, we investigate the potential applications of the rotational diamond anvil cell (Rot-DAC) for such studies. 300 K experiments in the Rot-DAC have been performed up to pressures exceeding 50 GPa (e.g. Serebryanaya et al, 1995) with studies focusing on the effect of shear on solid-solid phase transformation pressures. The authors did not investigate the possibility of using the Rot-DAC for studying rheological properties.Here, a sample of polycrystalline Fe is submitted to shear deformation in the Rot-DAC at pressures up to 20 GPa. Synchrotron X-ray diffraction and Rietveld refinements are then used to study the texture and stress state at multiple locations in the sample. The study shows that the Rot-DAC is efficient at producing deformation textures in a polycrystalline aggregate but that care should be taken in ensuring that the sample is actually undergoing plastic deformation and not solid rotation. Stresses, on the other hand, are difficult to extract from the x-ray diffraction data because of lack of understanding of stress distributions in the deforming aggregate.S. Merkel, H. R. Wenk, J. Shu, G. Shen, P. Gillet, H. K. Mao and R. J. Hemley, J. Geophys. Res., 107, 2271 (2002)N. Serebryanaya, V. Blank and V. Ivdenko, Phys. Lett. A, 197, 63-66 (1995)Y. Wang, W. B. Duhram, I. C. Getting and D. J. Weidner, Rev. Sci. Instrum., 74, 3002-3011 (2003)D. Yamazaki and S.-I. Karato, Rev. Sci. Instrum., 72, 4207-4211 (2001)

An electrochemical cell with sapphire windows for operando synchrotron X-ray powder diffraction and spectroscopy studies of high-power and high-voltage electrodes for metal-ion batteries.

PubMed

Drozhzhin, Oleg A; Tereshchenko, Ivan V; Emerich, Hermann; Antipov, Evgeny V; Abakumov, Artem M; Chernyshov, Dmitry

2018-03-01

A new multi-purpose operando electrochemical cell was designed, constructed and tested on the Swiss-Norwegian Beamlines BM01 and BM31 at the European Synchrotron Radiation Facility. Single-crystal sapphire X-ray windows provide a good signal-to-noise ratio, excellent electrochemical contact because of the constant pressure between the electrodes, and perfect electrochemical stability at high potentials due to the inert and non-conductive nature of sapphire. Examination of the phase transformations in the Li 1-x Fe 0.5 Mn 0.5 PO 4 positive electrode (cathode) material at C/2 and 10C charge and discharge rates, and a study of the valence state of the Ni cations in the Li 1-x Ni 0.5 Mn 1.5 O 4 cathode material for Li-ion batteries, revealed the applicability of this novel cell design to diffraction and spectroscopic investigations of high-power/high-voltage electrodes for metal-ion batteries.

DOE Office of Scientific and Technical Information (OSTI.GOV)

Veiga, L. S. I.; Etter, M.; Glazyrin, K.

Here, we explore the response of Ir 5d orbitals to pressure in β-Li 2IrO 3, a hyperhoneycomb iridate in proximity to a Kitaev quantum spin-liquid (QSL) ground state. X-ray absorption spectroscopy reveals a reconstruction of the electronic ground state below 2 GPa, the same pressure range where x-ray magnetic circular dichroism shows an apparent collapse of magnetic order. The electronic reconstruction, which manifests a reduction in the effective spin-orbit interaction in 5d orbitals, pushes β-Li 2IrO 3 further away from the pure J eff = 1/2 limit. Although lattice symmetry is preserved across the electronic transition, x-ray diffraction shows amore » highly anisotropic compression of the hyperhoneycomb lattice which affects the balance of bond-directional Ir-Ir exchange interactions driven by spin-orbit coupling at Ir sites. An enhancement of symmetric anisotropic exchange over Kitaev and Heisenberg exchange interactions seen in theoretical calculations that use precisely this anisotropic Ir-Ir bond compression provides one possible route to the realization of a QSL state in this hyperhoneycomb iridate at high pressures.« less

Determination of a Two-Phase Structure of Nanocrystals: GaN and SiC

NASA Technical Reports Server (NTRS)

Palosz, W.; Grzanka, E.; Gierlotka, S.; Stelmakh, S.; Pielaszek, R.; Lojkowski, W.; Bismayer, U.; Neuefeind, J.; Weber, H.-P.; Janik, J. F.;

High-resolution x-ray diffraction microscopy of specifically labeled yeast cells

PubMed Central

Nelson, Johanna; Huang, Xiaojing; Steinbrener, Jan; Shapiro, David; Kirz, Janos; Marchesini, Stefano; Neiman, Aaron M.; Turner, Joshua J.; Jacobsen, Chris

2010-01-01

X-ray diffraction microscopy complements other x-ray microscopy methods by being free of lens-imposed radiation dose and resolution limits, and it allows for high-resolution imaging of biological specimens too thick to be viewed by electron microscopy. We report here the highest resolution (11–13 nm) x-ray diffraction micrograph of biological specimens, and a demonstration of molecular-specific gold labeling at different depths within cells via through-focus propagation of the reconstructed wavefield. The lectin concanavalin A conjugated to colloidal gold particles was used to label the α-mannan sugar in the cell wall of the yeast Saccharomyces cerevisiae. Cells were plunge-frozen in liquid ethane and freeze-dried, after which they were imaged whole using x-ray diffraction microscopy at 750 eV photon energy. PMID:20368463

High-resolution x-ray diffraction microscopy of specifically labeled yeast cells

DOE PAGES

Nelson, Johanna; Huang, Xiaojing; Steinbrener, Jan; ...

2010-04-20

X-ray diffraction microscopy complements other x-ray microscopy methods by being free of lens-imposed radiation dose and resolution limits, and it allows for high-resolution imaging of biological specimens too thick to be viewed by electron microscopy. We report here the highest resolution (11-13 nm) x-ray diffraction micrograph of biological specimens, and a demonstration of molecular-specific gold labeling at different depths within cells via through-focus propagation of the reconstructed wavefield. The lectin concanavalin A conjugated to colloidal gold particles was used to label the α-mannan sugar in the cell wall of the yeast Saccharomyces cerevisiae. Cells were plunge-frozen in liquid ethane andmore » freeze-dried, after which they were imaged whole using x-ray diffraction microscopy at 750 eV photon energy.« less

A High-Pressure Study of Manganese Metal and its Reactions with CO2 at 6, 23, and 44 GPa

NASA Astrophysics Data System (ADS)

Sawchuk, K. L. S.; McGuire, C. P.; Greenburg, A.; Makhluf, A.; Kavner, A.

2017-12-01

The free energies of formation of oxides and carbonates at the extreme pressures and temperatures of Earth's interior provides some of the thermodynamic constrains for models of mantle/core formation and subsequent chemical evolution. The broad goal of our research program is to measure the pressure- and temperature-dependence of free energies of formation of transition metal oxides and carbonates. This requires measurements of the phase stability, density, and thermoelastic properties of metals, oxides, and carbonates at deep-Earth and planetary conditions. Manganese is of interest because it is one of the most abundant transition metal geochemical tracers, it readily forms a carbonate at ambient pressure, and its high-pressure carbonate and oxide densities and equation of state parameters are relatively unknown. Here we report new data on the pressure/volume equation of state and structure of manganese metal as well as its reactions with CO2. These measurements were made using a laser heated diamond anvil cell in conjunction with synchrotron-based X-ray diffraction at beamline 12.2.2 at the Advanced Light Source. Three samples of manganese metal were gas-loaded in a CO2 pressure medium and pressurized to 6, 23, and 44 GPa. Upon laser heating, the CO2 reacted with the Mn metal generating new phases. To analyze the diffraction patterns, we we use a python-based program developed in-house for extracting high resolution 2-dimensional diffraction peak position and intensity information from two-dimensional X-ray diffraction patterns. At each pressure step, the structure and density of the quenched Mn metal phase was determined. At 6 GPa, Mn metal adopts a BCC structure, and at 23 GPa a tetragonal distortion is observed in the lattice. The measured equation of state is in good agreement with an existing meaurement by Fujihisa and Takemura (1995). MnCO3 rhodochrosite is observed in the sample quenched after heating at 6 GPa. Additional high pressure phases are evident in the diffraction patterns from the samples at 23 GPa and 44 GPa. The density and equation of state parameters for our observed oxide, carbonate, and metal manganese structures are used in conjunction with existing thermodynamic information to predict how the free energies of formation of Mn- oxide and Mn-carbonate change as a function of pressure.

Coherent x-ray zoom condenser lens for diffractive and scanning microscopy.

PubMed

Kimura, Takashi; Matsuyama, Satoshi; Yamauchi, Kazuto; Nishino, Yoshinori

2013-04-22

We propose a coherent x-ray zoom condenser lens composed of two-stage deformable Kirkpatrick-Baez mirrors. The lens delivers coherent x-rays with a controllable beam size, from one micrometer to a few tens of nanometers, at a fixed focal position. The lens is suitable for diffractive and scanning microscopy. We also propose non-scanning coherent diffraction microscopy for extended objects by using an apodized focused beam produced by the lens with a spatial filter. The proposed apodized-illumination method will be useful in highly efficient imaging with ultimate storage ring sources, and will also open the way to single-shot coherent diffraction microscopy of extended objects with x-ray free-electron lasers.

Scanning force microscope for in situ nanofocused X-ray diffraction studies

PubMed Central

Ren, Zhe; Mastropietro, Francesca; Davydok, Anton; Langlais, Simon; Richard, Marie-Ingrid; Furter, Jean-Jacques; Thomas, Olivier; Dupraz, Maxime; Verdier, Marc; Beutier, Guillaume; Boesecke, Peter; Cornelius, Thomas W.

2014-01-01

A compact scanning force microscope has been developed for in situ combination with nanofocused X-ray diffraction techniques at third-generation synchrotron beamlines. Its capabilities are demonstrated on Au nano-islands grown on a sapphire substrate. The new in situ device allows for in situ imaging the sample topography and the crystallinity by recording simultaneously an atomic force microscope (AFM) image and a scanning X-ray diffraction map of the same area. Moreover, a selected Au island can be mechanically deformed using the AFM tip while monitoring the deformation of the atomic lattice by nanofocused X-ray diffraction. This in situ approach gives access to the mechanical behavior of nanomaterials. PMID:25178002

An ultrahigh pressure homogenization technique for easily exfoliating few-layer phosphorene from bulk black phosphorus

NASA Astrophysics Data System (ADS)

Guan, Qing-Qing; Zhou, Hua-Jing; Ning, Ping; Lian, Pei-Chao; Wang, Bo; He, Liang; Chai, Xin-Sheng

2018-05-01

We have developed an easy and efficient method for exfoliating few-layer sheets of black phosphorus (BP) in N-methyl-2-pyrrolidone, using ultra-high pressure homogenization (UPH). The BP was first exfoliated into sheets that were a few atomic layers thick, using a homogenizer for only 30 min. Next, a double centrifugation procedure was used to separate the material into few-layer nanosheets that were examined by X-ray diffraction, atomic force microscopy (AFM), transmission electron microscopy (TEM), high-angle annular dark field scanning transmission electron microscopy (HAADF-STEM), and energy-dispersive X-ray (EDX) spectroscopy. The results show that the products are specimens of phosphorene that are only a few-layer thick.

Effect of nitrogen-containing plasma on adherence, friction, and wear of radiofrequency-sputtered titanium carbide coatings

NASA Technical Reports Server (NTRS)

Brainard, W. A.; Wheeler, D. R.

1979-01-01

Friction and wear experiments on 440C steel surfaces that were rf sputtered with titanium carbide when a small percentage of nitrogen was added to the plasma were conducted. Both X-ray photoelectron spectroscopy and X-ray diffraction were used to analyze the resultant coatings. Results indicate that the small partial pressure of nitrogen (approximately 0.5 percent) markedly improves the adherence, friction, and wear properties when compared with coatings applied to sputter-etched surfaces, oxidized surfaces, or in the presence of a small oxygen partial pressure. The improvements are related to the formation of an interface containing a mixture of the nitrides of titanium and iron, which are harder than their corresponding oxides.

Pressure-tuning of bond-directional exchange interactions and magnetic frustration in hyperhoneycomb iridate β-Li 2IrO 3

DOE PAGES

Veiga, L. S. I.; Etter, M.; Glazyrin, K.; ...

2017-10-10

Here, we explore the response of Ir 5d orbitals to pressure in β-Li 2IrO 3, a hyperhoneycomb iridate in proximity to a Kitaev quantum spin-liquid (QSL) ground state. X-ray absorption spectroscopy reveals a reconstruction of the electronic ground state below 2 GPa, the same pressure range where x-ray magnetic circular dichroism shows an apparent collapse of magnetic order. The electronic reconstruction, which manifests a reduction in the effective spin-orbit interaction in 5d orbitals, pushes β-Li 2IrO 3 further away from the pure J eff = 1/2 limit. Although lattice symmetry is preserved across the electronic transition, x-ray diffraction shows amore » highly anisotropic compression of the hyperhoneycomb lattice which affects the balance of bond-directional Ir-Ir exchange interactions driven by spin-orbit coupling at Ir sites. An enhancement of symmetric anisotropic exchange over Kitaev and Heisenberg exchange interactions seen in theoretical calculations that use precisely this anisotropic Ir-Ir bond compression provides one possible route to the realization of a QSL state in this hyperhoneycomb iridate at high pressures.« less

Pressure tuning of bond-directional exchange interactions and magnetic frustration in the hyperhoneycomb iridate β -Li2IrO3

NASA Astrophysics Data System (ADS)

Veiga, L. S. I.; Etter, M.; Glazyrin, K.; Sun, F.; Escanhoela, C. A.; Fabbris, G.; Mardegan, J. R. L.; Malavi, P. S.; Deng, Y.; Stavropoulos, P. P.; Kee, H.-Y.; Yang, W. G.; van Veenendaal, M.; Schilling, J. S.; Takayama, T.; Takagi, H.; Haskel, D.

2017-10-01

We explore the response of Ir 5 d orbitals to pressure in β -Li2IrO3 , a hyperhoneycomb iridate in proximity to a Kitaev quantum spin-liquid (QSL) ground state. X-ray absorption spectroscopy reveals a reconstruction of the electronic ground state below 2 GPa, the same pressure range where x-ray magnetic circular dichroism shows an apparent collapse of magnetic order. The electronic reconstruction, which manifests a reduction in the effective spin-orbit interaction in 5 d orbitals, pushes β -Li2IrO3 further away from the pure Jeff=1 /2 limit. Although lattice symmetry is preserved across the electronic transition, x-ray diffraction shows a highly anisotropic compression of the hyperhoneycomb lattice which affects the balance of bond-directional Ir-Ir exchange interactions driven by spin-orbit coupling at Ir sites. An enhancement of symmetric anisotropic exchange over Kitaev and Heisenberg exchange interactions seen in theoretical calculations that use precisely this anisotropic Ir-Ir bond compression provides one possible route to the realization of a QSL state in this hyperhoneycomb iridate at high pressures.

X-ray topography using the forward transmitted beam under multiple-beam diffraction conditions

DOE Office of Scientific and Technical Information (OSTI.GOV)

Tsusaka, Y., E-mail: tsusaka@sci.u-hyogo.ac.jp; Takano, H.; Takeda, S.

2016-02-15

X-ray topographs are taken for a sapphire wafer with the [0001] surface normal, as an example, by forward transmitted synchrotron x-ray beams combined with two-dimensional electronic arrays in the x-ray detector having a spatial resolution of 1 μm. They exhibit no shape deformation and no position shift of the dislocation lines on the topographs. Since the topography is performed under multiple-beam diffraction conditions, the topographic images of a single diffraction (two-wave approximation condition) or plural diffractions (six-wave approximation condition) can be recorded without large specimen position changes. As usual Lang topographs, it is possible to determine the Burgers vector ofmore » each dislocation line. Because of high parallelism of the incoming x-rays and linear sensitivity of the electronic arrays to the incident x-rays, the present technique can be used to visualize individual dislocations in single crystals of the dislocation density as high as 1 × 10{sup 5} cm{sup −2}.« less

Thermal equation of state of MgSiO4H2 phase H determined by in situ X-ray diffraction and a multianvil apparatus

NASA Astrophysics Data System (ADS)

Nishi, Masayuki; Tsuchiya, Jun; Arimoto, Takeshi; Kakizawa, Sho; Kunimoto, Takehiro; Tange, Yoshinori; Higo, Yuji; Irifune, Tetsuo

2018-06-01

Phase H (MgSiO4H2) is the high-pressure form of dense hydrous silicate that could deliver surface water into the lower mantle. In this study, we determined the thermal equations of the state of phase H using in situ X-ray diffraction measurements, under conditions ranging from 34 to 62 GPa and 300 and 1300 K, using a multianvil apparatus. Analysis of the data, based on the Mie-Grüneisen-Debye model using third-order Burch-Murnaghan equations at a reference pressure of 35 GPa, yielded the following results V ref = 49.61 ± 0.01 Å3, K ref = 344.6±4.1 GPa, K_{{{ref}}}^' } = 3.05 ± 0.32, θ ref = 974 ± 146 K, γ ref = 1.8 ± 0.1, and q = 1.79 ± 0.55. The compressibility of phase H observed in this study agrees well with that derived from theoretical calculations in pressure regions where hydrogen bond symmetrization is predicted. It was also found that the volume and compressibility of phase H and δ-AlOOH were similar.

Persistence of Mixed and Non-intermediate Valence in the High-Pressure Structure of Silver(I,III) Oxide, AgO: A Combined Raman, X-ray Diffraction (XRD), and Density Functional Theory (DFT) Study.

PubMed

Grzelak, Adam; Gawraczyński, Jakub; Jaroń, Tomasz; Somayazulu, Maddury; Derzsi, Mariana; Struzhkin, Viktor; Grochala, Wojciech

2017-05-15

The X-ray diffraction data collected up to ca. 56 GPa and the Raman spectra measured up to 74.8 GPa for AgO, or Ag I Ag III O 2 , which is a prototypical mixed valence (disproportionated) oxide, indicate that two consecutive phase transitions occur: the first-order phase transition occurs between 16.1 GPa and 19.7 GPa, and a second-order phase transition occurs at ca. 40 GPa. All polymorphic forms host the square planar [Ag III O 4 ] units typical of low-spin Ag III . The disproportionated Imma form persists at least up to 74.8 GPa, as indicated by Raman spectra. Theoretical hybrid density functional theory (DFT) calculations show that the first-order transition is phonon-driven. AgO stubbornly remains disproportionated up to at least 100 GPa-in striking contrast to its copper analogue-and the fundamental band gap of AgO is ∼0.3 eV at this pressure and is weakly pressure-dependent. Metallization of AgO is yet to be achieved.

Membrane lateral compressibility determined by NMR and x-ray diffraction: effect of acyl chain polyunsaturation.

PubMed Central

Koenig, B W; Strey, H H; Gawrisch, K

1997-01-01

The elastic area compressibility modulus, Ka, of lamellar liquid crystalline bilayers was determined by a new experimental approach using 2H-NMR order parameters of lipid hydrocarbon chains together with lamellar repeat spacings measured by x-ray diffraction. The combination of NMR and x-ray techniques yields accurate determination of lateral area per lipid molecule. Samples of saturated, monounsaturated, and polyunsaturated phospholipids were equilibrated with polyethylene glycol (PEG) 20,000 solutions in water at concentrations from 0 to 55 wt % PEG at 30 degrees C. This procedure is equivalent to applying 0 to 8 dyn/cm lateral pressure to the bilayers. The resulting reductions in area per lipid were measured with a resolution of +/-0.2 A2 and the fractional area decrease was proportional to applied lateral pressure. For 1,2-dimyristoyl(d54)-sn-glycero-3-phosphocholine, 1-stearoyl(d35)-2-oleoyl-sn-glycero-3-phosphocholine (SOPC-d35), and 1-stearoyl(d35)-2-docosahexaenoyl-sn-glycero-3-phosphocholine (SDPC-d35) cross-sectional areas per molecule in excess water of 59.5, 61.4, and 69.2 A2 and bilayer elastic area compressibility moduli of 141, 221, and 121 dyn/cm were determined, respectively. Combining NMR and x-ray results enables the determination of compressibility differences between saturated and unsaturated hydrocarbon chains. In mixed-chain SOPC-d35 both chains have similar compressibility moduli; however, in mixed-chain polyunsaturated SDPC-d35, the saturated stearic acid chain appears to be far less compressible than the polyunsaturated docosahexaenoic acid chain. Images FIGURE 3 FIGURE 5 PMID:9336191

Multiple defocused coherent diffraction imaging: method for simultaneously reconstructing objects and probe using X-ray free-electron lasers.

PubMed

Hirose, Makoto; Shimomura, Kei; Suzuki, Akihiro; Burdet, Nicolas; Takahashi, Yukio

2016-05-30

The sample size must be less than the diffraction-limited focal spot size of the incident beam in single-shot coherent X-ray diffraction imaging (CXDI) based on a diffract-before-destruction scheme using X-ray free electron lasers (XFELs). This is currently a major limitation preventing its wider applications. We here propose multiple defocused CXDI, in which isolated objects are sequentially illuminated with a divergent beam larger than the objects and the coherent diffraction pattern of each object is recorded. This method can simultaneously reconstruct both objects and a probe from the coherent X-ray diffraction patterns without any a priori knowledge. We performed a computer simulation of the prposed method and then successfully demonstrated it in a proof-of-principle experiment at SPring-8. The prposed method allows us to not only observe broad samples but also characterize focused XFEL beams.

Multiple image x-radiography for functional lung imaging

NASA Astrophysics Data System (ADS)

Aulakh, G. K.; Mann, A.; Belev, G.; Wiebe, S.; Kuebler, W. M.; Singh, B.; Chapman, D.

2018-01-01

Detection and visualization of lung tissue structures is impaired by predominance of air. However, by using synchrotron x-rays, refraction of x-rays at the interface of tissue and air can be utilized to generate contrast which may in turn enable quantification of lung optical properties. We utilized multiple image radiography, a variant of diffraction enhanced imaging, at the Canadian light source to quantify changes in unique x-ray optical properties of lungs, namely attenuation, refraction and ultra small-angle scatter (USAXS or width) contrast ratios as a function of lung orientation in free-breathing or respiratory-gated mice before and after intra-nasal bacterial endotoxin (lipopolysaccharide) instillation. The lung ultra small-angle scatter and attenuation contrast ratios were significantly higher 9 h post lipopolysaccharide instillation compared to saline treatment whereas the refraction contrast decreased in magnitude. In ventilated mice, end-expiratory pressures result in an increase in ultra small-angle scatter contrast ratio when compared to end-inspiratory pressures. There were no detectable changes in lung attenuation or refraction contrast ratio with change in lung pressure alone. In effect, multiple image radiography can be applied towards following optical properties of lung air-tissue barrier over time during pathologies such as acute lung injury.

Angular rheology study of colloidal nanocrystals using Coherent X-ray Diffraction

NASA Astrophysics Data System (ADS)

Liang, Mengning; Harder, Ross; Robinson, Ian

2007-03-01

A new method using coherent x-ray diffraction provides a way to investigate the rotational motion of a colloidal suspension of crystals in real time. Coherent x-ray diffraction uses the long coherence lengths of synchrotron sources to illuminate a nanoscale particle coherently over its spatial dimensions. The penetration of high energy x-rays into various media allows for in-situ measurements making it ideal for suspensions. This technique has been used to image the structure of nanocrystals for some time but also has the capability of providing information about the orientation and dynamics of crystals. The particles are imaged in a specific diffraction condition allowing us to determine their orientation and observe how they rotate in real time with exceptional resolution. Such sensitivity allows for the study of rotational Brownian motion of nanocrystals in various suspensions and conditions. We present a study of the angular rheology of alumina and TiO2 colloidal nanocrystals in media using coherent x-ray diffraction.

Characterization of polycrystalline materials using synchrotron X-ray imaging and diffraction techniques

NASA Astrophysics Data System (ADS)

Ludwig, W.; King, A.; Herbig, M.; Reischig, P.; Marrow, J.; Babout, L.; Lauridsen, E. M.; Proudhon, H.; Buffière, J. Y.

2010-12-01

The combination of synchrotron radiation x-ray imaging and diffraction techniques offers new possibilities for in-situ observation of deformation and damage mechanisms in the bulk of polycrystalline materials. Minute changes in electron density (i.e., cracks, porosities) can be detected using propagation based phase contrast imaging, a 3-D imaging mode exploiting the coherence properties of third generation synchrotron beams. Furthermore, for some classes of polycrystalline materials, one may use a 3-D variant of x-ray diffraction imaging, termed x-ray diffraction contrast tomography. X-ray diffraction contrast tomography provides access to the 3-D shape, orientation, and elastic strain state of the individual grains from polycrystalline sample volumes containing up to thousand grains. Combining both imaging modalities, one obtains a comprehensive description of the materials microstructure at the micrometer length scale. Repeated observation during (interrupted) mechanical tests provide unprecedented insight into crystallographic and grain microstructure related aspects of polycrystalline deformation and degradation mechanisms.

Quantitative analysis of thoria phase in Th-U alloys using diffraction studies

NASA Astrophysics Data System (ADS)

Thakur, Shital; Krishna, P. S. R.; Shinde, A. B.; Kumar, Raj; Roy, S. B.

2017-05-01

In the present study the quantitative phase analysis of Th-U alloys in bulk form namely Th-52 wt% U and Th-3wt%U has been performed over the data obtained from both X ray diffraction and neutron diffraction technique using Rietveld method of FULLPROF software. Quantifying thoria (ThO2) phase present in bulk of the sample is limited due to surface oxidation and low penetration of x rays in high Z material. Neutron diffraction study probing bulk of the samples has been presented in comparison with x-ray diffraction study.

Selenium single-wavelength anomalous diffraction de novo phasing using an X-ray-free electron laser

DOE PAGES

Hunter, Mark S.; Yoon, Chun Hong; DeMirci, Hasan; ...

2016-11-04

Structural information about biological macromolecules near the atomic scale provides important insight into the functions of these molecules. To date, X-ray crystallography has been the predominant method used for macromolecular structure determination. However, challenges exist when solving structures with X-rays, including the phase problem and radiation damage. X-ray-free electron lasers (X-ray FELs) have enabled collection of diffraction information before the onset of radiation damage, yet the majority of structures solved at X-ray FELs have been phased using external information via molecular replacement. De novo phasing at X-ray FELs has proven challenging due in part to per-pulse variations in intensity andmore » wavelength. Here we report the solution of a selenobiotinyl-streptavidin structure using phases obtained by the anomalous diffraction of selenium measured at a single wavelength (Se-SAD) at the Linac Coherent Light Source. Finally, our results demonstrate Se-SAD, routinely employed at synchrotrons for novel structure determination, is now possible at X-ray FELs.« less

Macromolecular structures probed by combining single-shot free-electron laser diffraction with synchrotron coherent X-ray imaging.

PubMed

Gallagher-Jones, Marcus; Bessho, Yoshitaka; Kim, Sunam; Park, Jaehyun; Kim, Sangsoo; Nam, Daewoong; Kim, Chan; Kim, Yoonhee; Noh, Do Young; Miyashita, Osamu; Tama, Florence; Joti, Yasumasa; Kameshima, Takashi; Hatsui, Takaki; Tono, Kensuke; Kohmura, Yoshiki; Yabashi, Makina; Hasnain, S Samar; Ishikawa, Tetsuya; Song, Changyong

2014-05-02

Nanostructures formed from biological macromolecular complexes utilizing the self-assembly properties of smaller building blocks such as DNA and RNA hold promise for many applications, including sensing and drug delivery. New tools are required for their structural characterization. Intense, femtosecond X-ray pulses from X-ray free-electron lasers enable single-shot imaging allowing for instantaneous views of nanostructures at ambient temperatures. When combined judiciously with synchrotron X-rays of a complimentary nature, suitable for observing steady-state features, it is possible to perform ab initio structural investigation. Here we demonstrate a successful combination of femtosecond X-ray single-shot diffraction with an X-ray free-electron laser and coherent diffraction imaging with synchrotron X-rays to provide an insight into the nanostructure formation of a biological macromolecular complex: RNA interference microsponges. This newly introduced multimodal analysis with coherent X-rays can be applied to unveil nano-scale structural motifs from functional nanomaterials or biological nanocomplexes, without requiring a priori knowledge.

Anomalous behavior of cristobalite in helium under high pressure

NASA Astrophysics Data System (ADS)

Sato, Tomoko; Takada, Hiroto; Yagi, Takehiko; Gotou, Hirotada; Okada, Taku; Wakabayashi, Daisuke; Funamori, Nobumasa

2013-01-01

We have investigated the high-pressure behavior of cristobalite in helium by powder X-ray diffraction. Cristobalite transformed to a new phase at about 8 GPa. This phase is supposed to have a molar volume of about 30 % larger than cristobalite, suggesting the dissolution of helium atoms in its interstitial voids. On further compression, the new phase transformed to a different phase which showed an X-ray diffraction pattern similar to cristobalite X-I at about 21 GPa. On the other hand, when the new phase was decompressed, it transformed to another new phase at about 7 GPa, which is also supposed to have a molar volume of about 25 % larger than cristobalite. On further decompression, the second new phase transformed to cristobalite II at about 2 GPa. In contrast to cristobalite, quartz did not show anomalous behavior in helium. The behavior of cristobalite in helium was also consistent with that in other mediums up to about 8 GPa, where the volume of cristobalite became close to that of quartz. These results suggest that dissolution of helium may be controlled not only by the density (amount of voids) but also by the network structure of SiO4 tetrahedra (topology of voids).

Exploration of New Principles in Spintronics Based on Topological Insulators (Option 1)

DTIC Science & Technology

2012-05-14

on the surface and found that our crystals are exceedingly homogeneous (Supplementary Information). The persistently narrow X - ray diffraction peaks...modified Bridgman method (see Supplementary Information for details). X - ray diffraction measurements indicated the monotonic shrinkage of a and c axis...and annealing at that temperature for 4 days. X - ray diffraction analyses confirmed that all the samples have the same crystal structure (R 3m

Structural, magnetic and transport properties of Pb{sub 2}Cr{sub 1+x}Mo{sub 1−x}O{sub 6} (−1≤x≤1/3)

DOE Office of Scientific and Technical Information (OSTI.GOV)

Zhao, H.F.; School of Mathematics and Physics, University of Science and Technology, Beijing 100083; Cao, L.P.

Pb{sub 2}Cr{sub 1+x}Mo{sub 1-x}O{sub 6} (−1≤x≤1/3) samples were synthesized via a high pressure and high temperature route. X-ray diffraction results suggest the samples crystallize in a disordered double perovskite structure (Pm-3m). X-ray photoemission spectroscopy results confirm the presence of Mo{sup 4+} for x=−1 and Mo{sup 6+} for x=1/3. The measured magnetic and electrical properties exhibit systematic change with increasing x. - Highlights: • A series of Pb{sub 2}Cr{sub 1+x}Mo{sub 1−x}O{sub 6} samples were synthesized under high pressure. • Magnetic and electrical properties of the series samples were investigated. • Valence states of Cr and Mo were determined through the analysesmore » of XRD and XPS results. • Ground state of PbMoO{sub 3} were determined through the transport study and first-principles calculations.« less

Efficient modeling of Bragg coherent x-ray nanobeam diffraction

DOE PAGES

Hruszkewycz, S. O.; Holt, M. V.; Allain, M.; ...

2015-07-02

X-ray Bragg diffraction experiments that utilize tightly focused coherent beams produce complicated Bragg diffraction patterns that depend on scattering geometry, characteristics of the sample, and properties of the x-ray focusing optic. In this paper, we use a Fourier-transform-based method of modeling the 2D intensity distribution of a Bragg peak and apply it to the case of thin films illuminated with a Fresnel zone plate in three different Bragg scattering geometries. Finally, the calculations agree well with experimental coherent diffraction patterns, demonstrating that nanodiffraction patterns can be modeled at nonsymmetric Bragg conditions with this approach—a capability critical for advancing nanofocused x-raymore » diffraction microscopy.« less

High-pressure phases of cordierite from single-crystal X-ray diffraction to 15 GPa

DOE PAGES

Finkelstein, Gregory J.; Dera, Przemyslaw K.; Duffy, Thomas S.

2015-08-14

High-pressure single-crystal X-ray diffraction experiments were conducted on natural cordierite crystals with composition Mg1.907(18)Fe0.127(6)Al4.01(2)Si4.96(3)Na0.026(3)O18.12(9) using a synchrotron X-ray source. The samples were compressed at 300 K in a diamond anvil cell to a maximum pressure of 15.22(15) GPa with a neon pressure-transmitting medium and a gold pressure calibrant. We observed a recently described orthorhombic to triclinic transition, as well as a further transition to a second triclinic phase. We solved and refined both new triclinic hases in space group P1, and designate them cordierite II and III. The structures of cordierite II and III were refined at 7.52(3) GPa atmore » 15.22(15) GPa, respectively. The lattice parameters at these pressures are a = 15.567(3) Å, b = 9.6235(4) Å, c = 9.0658(6) Å, α = 89.963(5)°, β = 86.252(10)°, and γ = 90.974(8)° for cordierite II, and a = 8.5191(19) Å, b = 8.2448(3) Å, c = 9.1627(4) Å, α = 85.672(4)°, β = 85.986(7)°, and γ = 70.839(10)° for cordierite III. Across the phase transitions there is a significant reduction in the length of the a-axis (~2 Å per phase transition), whereas both the b- and c-axis remain largely unchanged. Cordierite II has four- and five-coordinated Si and Al, while cordierite III has four-, five-, and six-coordinated Si, four- and five-coordinated Al, and five- and six-coordinated Mg. The sequence of high-pressure phases shows increasing polymerization of coordination polyhedra. These results, together with other recent studies, suggest that mixed 4-, 5-, and 6-fold coordination states may occur more commonly in silicate structures compressed at 300 K than previously recognized.« less

Using acoustic levitation in synchrotron based laser pump hard x-ray probe experiments

NASA Astrophysics Data System (ADS)

Hu, Bin; Lerch, Jason; Suthar, Kamlesh; Dichiara, Anthony

Acoustic levitation provides a platform to trap and hold a small amount of material by using standing pressure waves without a container. The technique has a potential to be used for laser pump x-ray probe experiments; x-ray scattering and laser distortion from the container can be avoided, sample consumption can be minimized, and unwanted chemistry that may occur at the container interface can be avoided. The method has been used at synchrotron sources for studying protein and pharmaceutical solutions using x-ray diffraction (XRD) and small angle x-ray scattering (SAXS). However, pump-probe experiments require homogeneously excited samples, smaller than the absorption depth of the material that must be held stably at the intersection of both the laser and x-ray beams. We discuss 1) the role of oscillations in acoustic levitation and the optimal acoustic trapping conditions for x-ray/laser experiments, 2) opportunities to automate acoustic levitation for fast sample loading and manipulation, and 3) our experimental results using SAXS to monitor laser induced thermal expansion in gold nanoparticles solution. We also performed Finite Element Analysis to optimize the trapping performance and stability of droplets ranging from 0.4 mm to 2 mm. Our early x-ray/laser demonstrated the potential of the technique for time-resolved X-ray science.

HiSPoD: a program for high-speed polychromatic X-ray diffraction experiments and data analysis on polycrystalline samples

DOE PAGES

Sun, Tao; Fezzaa, Kamel

2016-06-17

Here, a high-speed X-ray diffraction technique was recently developed at the 32-ID-B beamline of the Advanced Photon Source for studying highly dynamic, yet non-repeatable and irreversible, materials processes. In experiments, the microstructure evolution in a single material event is probed by recording a series of diffraction patterns with extremely short exposure time and high frame rate. Owing to the limited flux in a short pulse and the polychromatic nature of the incident X-rays, analysis of the diffraction data is challenging. Here, HiSPoD, a stand-alone Matlab-based software for analyzing the polychromatic X-ray diffraction data from polycrystalline samples, is described. With HiSPoD,more » researchers are able to perform diffraction peak indexing, extraction of one-dimensional intensity profiles by integrating a two-dimensional diffraction pattern, and, more importantly, quantitative numerical simulations to obtain precise sample structure information.« less

Structural properties of pressure-induced structural phase transition of Si-doped GaAs by angular-dispersive X-ray diffraction

NASA Astrophysics Data System (ADS)

Lin, Kung-Liang; Lin, Chih-Ming; Lin, Yu-Sheng; Jian, Sheng-Rui; Liao, Yen-Fa; Chuang, Yu-Chun; Wang, Chuan-Sheng; Juang, Jenh-Yih

2016-02-01

Pressure-induced phase transitions in n-type silicon-doped gallium arsenide (GaAs:Si ) at ambient temperature were investigated by using angular-dispersive X-ray diffraction (ADXRD) under high pressure up to around 18.6 (1) GPa, with a 4:1 (in volume ratio) methanol-ethanol mixture as the pressure-transmitting medium. In situ ADXRD measurements revealed that n-type GaAs:Si starts to transform from zinc- blende structure to an orthorhombic structure [GaAs-II phase], space group Pmm2, at 16.4 (1) GPa. In contrast to previous studies of pure GaAs under pressure, our results show no evidence of structural transition to Fmmm or Cmcm phase. The fitting of volume compression data to the third-order Birch-Murnaghan equation of state yielded that the zero-pressure isothermal bulk moduli and the first-pressure derivatives were 75 (3) GPa and 6.4 (9) for the B3 phase, respectively. After decompressing to the ambient pressure, the GaAs:Si appears to revert to the B3 phase completely. By fitting to the empirical relations, the Knoop microhardness numbers are between H PK = 6.21 and H A = 5.85, respectively, which are substantially smaller than the values of 7-7.5 for pure GaAs reported previously. A discontinuous drop in the pressure-dependent lattice parameter, N- N distances, and V/ V 0 was observed at a pressure of 11.5 (1) GPa, which was tentatively attributed to the pressure-induced dislocation activities in the crystal grown by vertical gradient freeze method.

Advanced Photon Source Activity Report 2003: Report of Work Conducted at the APS, January 2003-December 2003, Synchrotron x-ray diffraction at the APS, Sector 16 (HPCAT)

DOE Office of Scientific and Technical Information (OSTI.GOV)

Goncharov, A F; Zaug, J M; Crowhurst, J C

2005-01-27

We present here the summary of the results of our studies using the APS synchrotron beamline IDB Sector 16 (HPCAT). Optical calibration of pressure sensors for high pressures and temperatures: The high-pressure ruby scale for static measurements is well established to at least 100 GPa (about 5% accuracy), however common use of this and other pressure scales at high temperature is clearly based upon unconfirmed assumptions. Namely that high temperature does not affect observed room temperature pressure derivatives. The establishment of a rigorous pressure scale along with the identification of appropriate pressure gauges (i.e. stable in the high P-T environmentmore » and easy to use) is important for securing the absolute accuracy of fundamental experimental science where results guide the development of our understanding of planetary sciences, geophysics, chemistry at extreme conditions, etc. X-ray diffraction in formic acid under high pressure: Formic acid (HCOOH) is common in the solar system; it is a potential component of the Galilean satellites. Despite this, formic acid has not been well-studied at high temperatures and pressures. A phase diagram of formic acid at planetary interior pressures and temperatures will add to the understanding of planetary formation and the potential for life on Europa. Formic acid (unlike most simple organic acids) forms low-temperature crystal structures characterized by infinite hydrogen-bonded chains of molecules. The behavior of these hydrogen bonds at high pressure is of great interest. Our current research fills this need.« less

Identification of a Catalytically Highly Active Surface Phase for CO Oxidation over PtRh Nanoparticles under Operando Reaction Conditions

NASA Astrophysics Data System (ADS)

Hejral, U.; Franz, D.; Volkov, S.; Francoual, S.; Strempfer, J.; Stierle, A.

2018-03-01

Pt-Rh alloy nanoparticles on oxide supports are widely employed in heterogeneous catalysis with applications ranging from automotive exhaust control to energy conversion. To improve catalyst performance, an atomic-scale correlation of the nanoparticle surface structure with its catalytic activity under industrially relevant operando conditions is essential. Here, we present x-ray diffraction data sensitive to the nanoparticle surface structure combined with in situ mass spectrometry during near ambient pressure CO oxidation. We identify the formation of ultrathin surface oxides by detecting x-ray diffraction signals from particular nanoparticle facets and correlate their evolution with the sample's enhanced catalytic activity. Our approach opens the door for an in-depth characterization of well-defined, oxide-supported nanoparticle based catalysts under operando conditions with unprecedented atomic-scale resolution.

In Situ Probes of Capture and Decomposition of Chemical Warfare Agent Simulants by Zr-Based Metal Organic Frameworks

DOE Office of Scientific and Technical Information (OSTI.GOV)

Plonka, Anna M.; Wang, Qi; Gordon, Wesley O.

Recently, Zr-based metal organic frameworks (MOFs) were shown to be among the fastest catalysts of nerve-agent hydrolysis in solution. Here, we report a detailed study of the adsorption and decomposition of a nerve-agent simulant, dimethyl methylphosphonate (DMMP), on UiO-66, UiO-67, MOF-808, and NU-1000 using synchrotron-based X-ray powder diffraction, X-ray absorption, and infrared spectroscopy, which reveals key aspects of the reaction mechanism. The diffraction measurements indicate that all four MOFs adsorb DMMP (introduced at atmospheric pressures through a flow of helium or air) within the pore space. In addition, the combination of X-ray absorption and infrared spectra suggests direct coordination ofmore » DMMP to the Zr6 cores of all MOFs, which ultimately leads to decomposition to phosphonate products. Our experimental probes into the mechanism of adsorption and decomposition of chemical warfare agent simulants on Zr-based MOFs open new opportunities in rational design of new and superior decontamination materials.« less

In Situ Probes of Capture and Decomposition of Chemical Warfare Agent Simulants by Zr-Based Metal Organic Frameworks

DOE Office of Scientific and Technical Information (OSTI.GOV)

Plonka, Anna M.; Wang, Qi; Gordon, Wesley O.

Zr-based metal organic frameworks (MOFs) have been recently shown to be among the fastest catalysts of nerve-agent hydrolysis in solution. We report a detailed study of the adsorption and decomposition of a nerve-agent simulant, dimethyl methylphosphonate (DMMP), on UiO-66, UiO-67, MOF-808, and NU-1000 using synchrotron-based X-ray powder diffraction, X-ray absorption, and infrared spectroscopy, which reveals key aspects of the reaction mechanism. The diffraction measurements indicate that all four MOFs adsorb DMMP (introduced at atmospheric pressures through a flow of helium or air) within the pore space. In addition, the combination of X-ray absorption and infrared spectra suggests direct coordination ofmore » DMMP to the Zr6 cores of all MOFs, which ultimately leads to decomposition to phosphonate products. These experimental probes into the mechanism of adsorption and decomposition of chemical warfare agent simulants on Zr-based MOFs open new opportunities in rational design of new and superior decontamination materials.« less

In Situ Probes of Capture and Decomposition of Chemical Warfare Agent Simulants by Zr-Based Metal Organic Frameworks

DOE PAGES

Plonka, Anna M.; Wang, Qi; Gordon, Wesley O.; ...

2016-12-30

Recently, Zr-based metal organic frameworks (MOFs) were shown to be among the fastest catalysts of nerve-agent hydrolysis in solution. Here, we report a detailed study of the adsorption and decomposition of a nerve-agent simulant, dimethyl methylphosphonate (DMMP), on UiO-66, UiO-67, MOF-808, and NU-1000 using synchrotron-based X-ray powder diffraction, X-ray absorption, and infrared spectroscopy, which reveals key aspects of the reaction mechanism. The diffraction measurements indicate that all four MOFs adsorb DMMP (introduced at atmospheric pressures through a flow of helium or air) within the pore space. In addition, the combination of X-ray absorption and infrared spectra suggests direct coordination ofmore » DMMP to the Zr6 cores of all MOFs, which ultimately leads to decomposition to phosphonate products. Our experimental probes into the mechanism of adsorption and decomposition of chemical warfare agent simulants on Zr-based MOFs open new opportunities in rational design of new and superior decontamination materials.« less

X-ray diffraction and X-ray standing-wave study of the lead stearate film structure

DOE Office of Scientific and Technical Information (OSTI.GOV)

Blagov, A. E.; Dyakova, Yu. A.; Kovalchuk, M. V.

2016-05-15

A new approach to the study of the structural quality of crystals is proposed. It is based on the use of X-ray standing-wave method without measuring secondary processes and considers the multiwave interaction of diffraction reflections corresponding to different harmonics of the same crystallographic reflection. A theory of multiwave X-ray diffraction is developed to calculate the rocking curves in the X-ray diffraction scheme under consideration for a long-period quasi-one-dimensional crystal. This phase-sensitive method is used to study the structure of a multilayer lead stearate film on a silicon substrate. Some specific structural features are revealed for the surface layer ofmore » the thin film, which are most likely due to the tilt of the upper layer molecules with respect to the external normal to the film surface.« less

High-resolution ab initio three-dimensional x-ray diffraction microscopy

DOE PAGES

Chapman, Henry N.; Barty, Anton; Marchesini, Stefano; ...

2006-01-01

Coherent x-ray diffraction microscopy is a method of imaging nonperiodic isolated objects at resolutions limited, in principle, by only the wavelength and largest scattering angles recorded. We demonstrate x-ray diffraction imaging with high resolution in all three dimensions, as determined by a quantitative analysis of the reconstructed volume images. These images are retrieved from the three-dimensional diffraction data using no a priori knowledge about the shape or composition of the object, which has never before been demonstrated on a nonperiodic object. We also construct two-dimensional images of thick objects with greatly increased depth of focus (without loss of transverse spatialmore » resolution). These methods can be used to image biological and materials science samples at high resolution with x-ray undulator radiation and establishes the techniques to be used in atomic-resolution ultrafast imaging at x-ray free-electron laser sources.« less

Enhancing resolution in coherent x-ray diffraction imaging.

PubMed

Noh, Do Young; Kim, Chan; Kim, Yoonhee; Song, Changyong

2016-12-14

Achieving a resolution near 1 nm is a critical issue in coherent x-ray diffraction imaging (CDI) for applications in materials and biology. Albeit with various advantages of CDI based on synchrotrons and newly developed x-ray free electron lasers, its applications would be limited without improving resolution well below 10 nm. Here, we review the issues and efforts in improving CDI resolution including various methods for resolution determination. Enhancing diffraction signal at large diffraction angles, with the aid of interference between neighboring strong scatterers or templates, is reviewed and discussed in terms of increasing signal-to-noise ratio. In addition, we discuss errors in image reconstruction algorithms-caused by the discreteness of the Fourier transformations involved-which degrade the spatial resolution, and suggest ways to correct them. We expect this review to be useful for applications of CDI in imaging weakly scattering soft matters using coherent x-ray sources including x-ray free electron lasers.

A portable X-ray diffraction apparatus for in situ analyses of masters' paintings

NASA Astrophysics Data System (ADS)

Eveno, Myriam; Duran, Adrian; Castaing, Jacques

2010-09-01

It is rare that the analyses of materials in paintings can be carried out by taking micro-samples. Valuable works of art are best studied in situ by non-invasive techniques. For that purpose, a portable X-ray diffraction and fluorescence apparatus has been designed and constructed at the C2RMF. This apparatus has been used for paintings of Rembrandt, Leonardo da Vinci, Van Gogh, Mantegna, etc. Results are given to illustrate the performance of X-ray diffraction, especially when X-ray fluorescence does not bring sufficient information to conclude.

X-ray fractography on fatigue fractured surface of austenitic stainless steel

DOE Office of Scientific and Technical Information (OSTI.GOV)

Yajima, Zenjiro; Tokuyama, Hideki; Kibayashi, Yasuo

1995-12-31

X-ray diffraction observation of the material internal structure beneath fracture surfaces provide fracture analysis with useful information to investigate the conditions and mechanisms of fracture. X-ray fractography is a generic name given to this technique. In the present study, X-ray fractography was applied to fatigue fracture surfaces of austenitic stainless steel (AISI 304) which consisted of solution treatment. The fatigue tests were carried out on compact tension (CT) specimens. The plastic strain on the fracture surface was estimated from measuring the line broadening of X-ray diffraction profiles. The line broadening of X-ray diffraction profiles was measured on and beneath fatiguemore » fracture surfaces. The depth of the plastic zone left on fracture surfaces was evaluated from the line broadening. The results are discussed on the basis of fracture mechanics.« less

Toward in situ x-ray diffraction imaging at the nanometer scale

NASA Astrophysics Data System (ADS)

Zatsepin, Nadia A.; Dilanian, Ruben A.; Nikulin, Andrei Y.; Gable, Brian M.; Muddle, Barry C.; Sakata, Osami

2008-08-01

We present the results of preliminary investigations determining the sensitivity and applicability of a novel x-ray diffraction based nanoscale imaging technique, including simulations and experiments. The ultimate aim of this nascent technique is non-destructive, bulk-material characterization on the nanometer scale, involving three dimensional image reconstructions of embedded nanoparticles and in situ sample characterization. The approach is insensitive to x-ray coherence, making it applicable to synchrotron and laboratory hard x-ray sources, opening the possibility of unprecedented nanometer resolution with the latter. The technique is being developed with a focus on analyzing a technologically important light metal alloy, Al-xCu (where x is 2.0-5.0 %wt). The mono- and polycrystalline samples contain crystallographically oriented, weakly diffracting Al2Cu nanoprecipitates in a sparse, spatially random dispersion within the Al matrix. By employing a triple-axis diffractometer in the non-dispersive setup we collected two-dimensional reciprocal space maps of synchrotron x-rays diffracted from the Al2Cu nanoparticles. The intensity profiles of the diffraction peaks confirmed the sensitivity of the technique to the presence and orientation of the nanoparticles. This is a fundamental step towards in situ observation of such extremely sparse, weakly diffracting nanoprecipitates embedded in light metal alloys at early stages of their growth.

Diffraction and Imaging Study of Imperfections of Protein Crystals with Coherent X-rays

NASA Technical Reports Server (NTRS)

Hu, Z. W.; Thomas, B. R.; Chernov, A. A.; Chu, Y. S.; Lai, B.

2004-01-01

High angular-resolution x-ray diffraction and phase contrast x-ray imaging were combined to study defects and perfection of protein crystals. Imperfections including line defects, inclusions and other microdefects were observed in the diffraction images of a uniformly grown lysozyme crystal. The observed line defects carry distinct dislocation features running approximately along the <110> growth front and have been found to originate mostly in a central growth area and occasionally in outer growth regions. Slow dehydration led to the broadening of a fairly symmetric 4 4 0 rocking curve by a factor of approximately 2.6, which was primarily attributed to the dehydration-induced microscopic effects that are clearly shown in diffraction images. X-ray imaging and diffraction characterization of the quality of apoferritin crystals will also be discussed in the presentation.

Structure and bulk modulus of Ln-doped UO 2 (Ln = La, Nd) at high pressure

DOE PAGES

Rittman, Dylan R.; Park, Sulgiye; Tracy, Cameron L.; ...

2017-04-10

The structure of lanthanide-doped uranium dioxide, Ln xU 1-xO 2-0.5x+y (Ln = La, Nd), was investigated at pressures up to ~50–55 GPa. Samples were synthesized with different lanthanides at different concentrations (x ~ 0.2 and 0.5), and all were slightly hyperstoichiometric (y ~ 0.25–0.4). In situ high-pressure synchrotron X-ray diffraction was used to investigate their high-pressure phase behavior and determine their bulk moduli. All samples underwent a fluorite-to-cotunnite phase transformation with increasing pressure. The pressure of the phase transformation increased with increasing hyperstoichiometry, which is consistent with results from previous computational simulations. Bulk moduli are inversely proportional to both themore » ionic radius of the lanthanide and its concentration, as quantified using a weighted cationic radius ratio. As a result, this trend was found to be consistent with the behavior of other elastic properties measured for Ln-doped UO 2, such as Young's modulus.« less

THE EFFECT OF SATELLITE LINES FROM THE X-RAY SOURCE ON X-RAY DIFFRACTION PEAKS

EPA Science Inventory

The article discusses the development of a method for relating reactivity to crystallite size and strain parameters obtained by the Warren-Averbach technique. EPA has been using crystallite size and strain data obtained from x-ray diffraction (XRD) peak profile analysis to predic...

History and Solution of the Phase Problem in theTheory of Structure Determination of Crystals from X-ray Diffraction Experiments

ScienceCinema

Wolf, Emil [University of Rochester, Rochester, New York, United States

2017-12-09

Since the pioneering work of Max von Laue on interference and diffraction of x-rays, carried out almost 100 years ago, numerous attempts have been made to determine structures of crystalline media from x-ray diffraction experiments. The usefulness of all of them has been limited by the inability of measuring phases of the diffracted beams. In this talk, the most important research carried out in this field will be reviewed and a recently obtained solution of the phase problem will be presented.

Stable low-pressure hydrogen clusters stored in a binary clathrate hydrate.

PubMed

Florusse, Louw J; Peters, Cor J; Schoonman, Joop; Hester, Keith C; Koh, Carolyn A; Dec, Steven F; Marsh, Kenneth N; Sloan, E Dendy

2004-10-15

Thermodynamic, x-ray diffraction, and Raman and nuclear magnetic resonance spectroscopy measurements show that clusters of H2 can be stabilized and stored at low pressures in a sII binary clathrate hydrate. Clusters of H2 molecules occupy small water cages, whereas large water cages are singly occupied by tetrahydrofuran. The presence of this second guest component stabilizes the clathrate at pressures of 5 megapascals at 279.6 kelvin, versus 300 megapascals at 280 kelvin for pure H2 hydrate.

Crystal structure of new AsS{sub 2} compound

DOE Office of Scientific and Technical Information (OSTI.GOV)

Bolotina, N. B., E-mail: bolotina@ns.crys.ras.ru; Brazhkin, V. V.; Dyuzheva, T. I.

2013-01-15

AsS{sub 2} single crystals have been obtained for the first time from an As{sub 2}S{sub 3} melt at pressures above 6 GPa and temperatures above 800 K in the As{sub 2}S{sub 3} {yields} AsS + AsS{sub 2} reaction. The monoclinic structure of the new high-pressure phase is solved by X-ray diffraction analysis and compared to the structure of high-pressure AsS phase, which was studied previously.

Simultaneous measurement of pressure evolution of crystal structure and superconductivity in FeSe[subscript 0.92] using designer diamonds

DOE Office of Scientific and Technical Information (OSTI.GOV)

Uhoya, Walter; Tsoi, Georgiy; Vohra, Yogesh

Simultaneous high-pressure X-ray diffraction and electrical resistance measurements have been carried out on a PbO-type {alpha}-FeSe{sub 0.92} compound to a pressure of 44 GPa and temperatures down to 4 K using designer diamond anvils at synchrotron source. A ambient temperature, a structural phase transition from a tetragonal (P4/nmm) phase to an orthorhombic (Pbnm) phase is observed at 11 GPa and the Pbnm phase persists up to 74 GPa. The superconducting transition temperature (T{sub c}) increases rapidly with pressure reaching a maximum of {approx}28 K at {approx}6 GPa and decreases at higher pressures, disappearing completely at 14.6 GPa. Simultaneous pressure-dependent X-raymore » diffraction and resistance measurements at low temperatures show superconductivity only in a low-pressure orthorhombic (Cmma) phase of the {alpha}-FeSe{sub 0.92}. Upon increasing pressure at 10 K near T{sub c}, crystalline phases change from a mixture of orthorhombic (Cmma) and hexagonal (P63/mmc) phases to a high-pressure orthorhombic (Pbnm) phase near 6.4 GPa where T{sub c} is maximum.« less

XRayView: a teaching aid for X-ray crystallography.

PubMed

Phillips, G N

1995-10-01

A software package, XRayView, has been developed that uses interactive computer graphics to introduce basic concepts of x-ray diffraction by crystals, including the reciprocal lattice, the Ewald sphere construction, Laue cones, the wavelength dependence of the reciprocal lattice, primitive and centered lattices and systematic extinctions, rotation photography. Laue photography, space group determination and Laue group symmetry, and the alignment of crystals by examination of reciprocal space. XRayView is designed with "user-friendliness" in mind, using pull-down menus to control the program. Many of the experiences of using real x-ray diffraction equipment to examine crystalline diffraction can be simulated. Exercises are available on-line to guide the users through many typical x-ray diffraction experiments.

Electronic and structural ground state of heavy alkali metals at high pressure

NASA Astrophysics Data System (ADS)

Fabbris, G.; Lim, J.; Veiga, L. S. I.; Haskel, D.; Schilling, J. S.

2015-02-01

Alkali metals display unexpected properties at high pressure, including emergence of low-symmetry crystal structures, which appear to occur due to enhanced electronic correlations among the otherwise nearly free conduction electrons. We investigate the high-pressure electronic and structural ground state of K, Rb, and Cs using x-ray absorption spectroscopy and x-ray diffraction measurements together with a b i n i t i o theoretical calculations. The sequence of phase transitions under pressure observed at low temperature is similar in all three heavy alkalis except for the absence of the o C 84 phase in Cs. Both the experimental and theoretical results point to pressure-enhanced localization of the valence electrons characterized by pseudogap formation near the Fermi level and strong s p d hybridization. Although the crystal structures predicted to host magnetic order in K are not observed, the localization process appears to drive these alkalis closer to a strongly correlated electron state.

Experimental and first-principles calculation study of the pressure-induced transitions to a metastable phase in GaP O4 and in the solid solution AlP O4-GaP O4

NASA Astrophysics Data System (ADS)

Angot, E.; Huang, B.; Levelut, C.; Le Parc, R.; Hermet, P.; Pereira, A. S.; Aquilanti, G.; Frapper, G.; Cambon, O.; Haines, J.

2017-08-01

α -Quartz-type gallium phosphate and representative compositions in the AlP O4-GaP O4 solid solution were studied by x-ray powder diffraction and absorption spectroscopy, Raman scattering, and by first-principles calculations up to pressures of close to 30 GPa. A phase transition to a metastable orthorhombic high-pressure phase along with some of the stable orthorhombic C m c m CrV O4 -type material is found to occur beginning at 9 GPa at 320 ∘C in GaP O4 . In the case of the AlP O4-GaP O4 solid solution at room temperature, only the metastable orthorhombic phase was obtained above 10 GPa. The possible crystal structures of the high-pressure forms of GaP O4 were predicted from first-principles calculations and the evolutionary algorithm USPEX. A predicted orthorhombic structure with a P m n 21 space group with the gallium in sixfold and phosphorus in fourfold coordination was found to be in the best agreement with the combined experimental data from x-ray diffraction and absorption and Raman spectroscopy. This method is found to very powerful to better understand competition between different phase transition pathways at high pressure.

High-pressure high-temperature phase diagram of gadolinium studied using a boron-doped heater anvil

DOE Office of Scientific and Technical Information (OSTI.GOV)

Montgomery, J. M.; Samudrala, G. K.; Vohra, Y. K.

A boron-doped designer heater anvil is used in conjunction with powder x-ray diffraction to collect structural information on a sample of quasi-hydrostatically loaded gadolinium metal up to pressures above 8 GPa and 600 K. The heater anvil consists of a natural diamond anvil that has been surface modified with a homoepitaxially grown chemical-vapor-deposited layer of conducting boron-doped diamond, and is used as a DC heating element. Internally insulating both diamond anvils with sapphire support seats allows for heating and cooling of the high-pressure area on the order of a few tens of seconds. This device is then used to scan the phasemore » diagram of the sample by oscillating the temperature while continuously increasing the externally applied pressure and collecting in situ time-resolved powder diffraction images. In the pressure-temperature range covered in this experiment, the gadolinium sample is observed in its hcp, αSm, and dhcp phases. Under this temperature cycling, the hcp → αSm transition proceeds in discontinuous steps at points along the expected phase boundary. From these measurements (representing only one hour of synchrotron x-ray collection time), a single-experiment equation of state and phase diagram of each phase of gadolinium is presented for the range of 0–10 GPa and 300–650 K.« less

Structural and vibrational properties of single crystals of Scandia, Sc{sub 2}O{sub 3} under high pressure

DOE Office of Scientific and Technical Information (OSTI.GOV)

Ovsyannikov, Sergey V., E-mail: sergey.ovsyannikov@uni-bayreuth.de, E-mail: sergey2503@gmail.com; Wenz, Michelle D.; Pakhomova, Anna S.

2015-10-28

We report the results of single-crystal X-ray diffraction and Raman spectroscopy studies of scandium oxide, Sc{sub 2}O{sub 3}, at ambient temperature under high pressure up to 55 and 28 GPa, respectively. Both X-ray diffraction and Raman studies indicated a phase transition from the cubic bixbyite phase (so-called C-Res phase) to a monoclinic C2/m phase (so-called B-Res phase) at pressures around 25–28 GPa. The transition was accompanied by a significant volumetric drop by ∼6.7%. In addition, the Raman spectroscopy detected a minor crossover around 10–12 GPa, which manifested in the appearance of new and disappearance of some Raman modes, as well as in softeningmore » of one Raman mode. We found the bulk modulus values of the both C-Res and B-Res phases as B{sub 0} = 198.2(3) and 171.2(1) GPa (for fixed B′ = 4), respectively. Thus, the denser high-pressure lattice of Sc{sub 2}O{sub 3} is much softer than the original lattice. We discuss possible mechanisms that might be responsible for the pronounced elastic softening in the monoclinic high-pressure phase in this “simple” oxide with an ultra-wide band gap.« less

Application of MEMS-based x-ray optics as tuneable nanosecond choppers

NASA Astrophysics Data System (ADS)

Chen, Pice; Walko, Donald A.; Jung, Il Woong; Li, Zhilong; Gao, Ya; Shenoy, Gopal K.; Lopez, Daniel; Wang, Jin

2017-08-01

Time-resolved synchrotron x-ray measurements often rely on using a mechanical chopper to isolate a set of x-ray pulses. We have started the development of micro electromechanical systems (MEMS)-based x-ray optics, as an alternate method to manipulate x-ray beams. In the application of x-ray pulse isolation, we recently achieved a pulse-picking time window of half a nanosecond, which is more than 100 times faster than mechanical choppers can achieve. The MEMS device consists of a comb-drive silicon micromirror, designed for efficiently diffracting an x-ray beam during oscillation. The MEMS devices were operated in Bragg geometry and their oscillation was synchronized to x-ray pulses, with a frequency matching subharmonics of the cycling frequency of x-ray pulses. The microscale structure of the silicon mirror in terms of the curvature and the quality of crystallinity ensures a narrow angular spread of the Bragg reflection. With the discussion of factors determining the diffractive time window, this report showed our approaches to narrow down the time window to half a nanosecond. The short diffractive time window will allow us to select single x-ray pulse out of a train of pulses from synchrotron radiation facilities.

Fabrication of high-resolution x-ray diffractive optics at King's College London

NASA Astrophysics Data System (ADS)

Charalambous, Pambos S.; Anastasi, Peter A. F.; Burge, Ronald E.; Popova, Katia

1995-09-01

The fabrication of high resolution x-ray diffractive optics, and Fresnel zone plates (ZPs) in particular, is a very demanding multifaceted technological task. The commissioning of more (and brighter) synchrotron radiation sources, has increased the number of x-ray imaging beam lines world wide. The availability of cheaper and more effective laboratory x-ray sources, has further increased the number of laboratories involved in x-ray imaging. The result is an ever increasing demand for x-ray optics with a very wide range of specifications, reflecting the particular type of x-ray imaging performed at different laboratories. We have been involved in all aspects of high resolution nanofabrication for a number of years, and we have explored many different methods of lithography, which, although unorthodox, open up possibilities, and increase our flexibility for the fabrication of different diffractive optical elements, as well as other types of nanostructures. The availability of brighter x-ray sources, means that the diffraction efficiency of the ZPs is becoming of secondary importance, a trend which will continue in the future. Resolution, however, is important and will always remain so. Resolution is directly related to the accuracy af pattern generation, as well as the ability to draw fine lines. This is the area towards which we have directed most of our efforts so far.

Phase degradation in BxGa1-xN films grown at low temperature by metalorganic vapor phase epitaxy

NASA Astrophysics Data System (ADS)

Gunning, Brendan P.; Moseley, Michael W.; Koleske, Daniel D.; Allerman, Andrew A.; Lee, Stephen R.

2017-04-01

Using metalorganic vapor phase epitaxy, a comprehensive study of BxGa1-xN growth on GaN and AlN templates is described. BGaN growth at high-temperature and high-pressure results in rough surfaces and poor boron incorporation efficiency, while growth at low-temperature and low-pressure (750-900 °C and 20 Torr) using nitrogen carrier gas results in improved surface morphology and boron incorporation up to 7.4% as determined by nuclear reaction analysis. However, further structural analysis by transmission electron microscopy and x-ray pole figures points to severe degradation of the high boron composition films, into a twinned cubic structure with a high density of stacking faults and little or no room temperature photoluminescence emission. Films with <1% triethylboron (TEB) flow show more intense, narrower x-ray diffraction peaks, near-band-edge photoluminescence emission at 362 nm, and primarily wurtzite-phase structure in the x-ray pole figures. For films with >1% TEB flow, the crystal structure becomes dominated by the cubic phase. Only when the TEB flow is zero (pure GaN), does the cubic phase entirely disappear from the x-ray pole figure, suggesting that under these growth conditions even very low boron compositions lead to mixed crystalline phases.

Whisker growth of l-menthol in coexistence with various excipients.

PubMed

Yuasa, H; Ooi, M; Takashima, Y; Kanaya, Y

2000-08-10

The purpose of the present study was to clarify the mechanism for l-menthol whisker growth. l-Menthol was mixed with an excipient, and the interaction was examined by IR measurement, thermal analysis and powder X-ray diffraction. Then we examined the involvement of the capillary condensation using the pore size distribution measurement. By mixing l-menthol with an excipient with whisker growth, the hydroxyl group stretching band of l-menthol was shifted to the higher wavenumber in the IR spectrum, the melting point and heat of fusion of l-menthol became lower in the thermal analysis, and the diffraction intensity of l-menthol became lower in the powder X-ray diffraction. The excipients with whisker growth showed the tendency to have the meso-pore involved in the capillary condensation in the pore size distribution measurement. From the above results, the whisker growth mechanism is considered as follows. When l-menthol was mixed with an excipient with whisker growth, the crystallinity of l-menthol was lowered and the vapor pressure was increased by the interaction mainly consisting of the hydrogen bond. The generated l-menthol vapor entered meso-pore, the saturated vapor pressure was lowered by the capillary condensation, and the nucleation occurred. The vapor was further supplied, generating the growth of whisker.

Investigation of solid phase composition on tablet surfaces by grazing incidence X-ray diffraction.

PubMed

Koradia, Vishal; Tenho, Mikko; Lopez de Diego, Heidi; Ringkjøbing-Elema, Michiel; Møller-Sonnergaard, Jørn; Salonen, Jarno; Lehto, Vesa-Pekka; Rantanen, Jukka

2012-01-01

To investigate solid state transformations of drug substances during compaction using grazing incidence X-ray diffraction (GIXD). The solid forms of three model drugs-theophylline (TP), nitrofurantoin (NF) and amlodipine besylate (AMB)-were compacted at different pressures (from 100 to 1000 MPa); prepared tablets were measured using GIXD. After the initial measurements of freshly compacted tablets, tablets were subjected to suitable recrystallization treatment, and analogous measurements were performed. Solid forms of TP, NF and AMB showed partial amorphization as well as crystal disordering during compaction; the extent of these effects generally increased as a function of pressure. The changes were most pronounced at the outer surface region. The different solid forms showed difference in the formation of amorphicity/crystal disordering. Dehydration due to compaction was observed for the TP monohydrate, whereas hydrates of NF and AMB were stable towards dehydration. With GIXD measurements, it was possible to probe the solid form composition at the different depths of the tablet surfaces and to obtain depth-dependent information on the compaction-induced amorphization, crystal disordering and dehydration.

High-pressure structural behavior of hydrogarnet, katoite Ca3Al2(O4H4)3

NASA Astrophysics Data System (ADS)

Kyono, A.; Kato, M.; Sano-Furukawa, A.; Machida, S. I.; Hattori, T.

2016-12-01

High-pressure structural behavior of hydrogarnet, katoite Ca3Al2(O4H4)3, was investigated using single-crystal synchrotron x-ray diffraction, Raman spectroscopic, and neutron diffraction analyses. The high-pressure single-crystal synchrotron x-ray diffraction was performed at BL10A, Photon Factory, KEK, Japan. With compression, the a lattice parameter decreased continuously from 12.565 (1) Å to 12.226 (3) Å up to 7.1 GPa. A fit to the Birch-Murnaghan equation of state (EoS) based on the P-V data gives K0 = 56.0 (6) GPa, K' = 4.3 (1), and V0 = 1984.2 (5) Å3, which were consistent with the previous study by Lager et al. (2002). Weak reflections forbidden by the systematic absence of hk0 with k, l = 2n were observed at 5.5 GPa and their intensities became stronger as increasing pressure. The pattern change of systematic absence implies phase transformation from space group Ia-3d to its non-centrosymmetric space group I-43d. High-pressure Raman spectroscopic study was performed up to 8.3 GPa at room temperature. The pressure dependence of lattice modes showed a positive pressure shifts, whereas that of OH stretching vibration mode was changed negative above 5.1 GPa. The change indicates that the strength of hydrogen bonding turns to increase above 5.1 GPa. High-pressure and high-temperature neutron diffraction study was performed with six-axis large volume press, ATSUHIME, at BL11 (PLANET), J-PARC, Japan. At a pressure of approximately 8 GPa, the a lattice parameter increased with temperature, but neither thermal decomposition nor dehydroxylation process occurred up to 1123 K. The crystal structure of katoite was determined by Rietveld method using neutron diffraction data with the space group I-43d. The volume of dodecahedral site containing Ca cations and that of octahedral site occupied by Al cations remained almost constant with temperature, but two crystallographically inequivalent tetrahedral sites which were caused by phase transformation behaved differently from each other. The volume of T2 site was continuously increased, but that of T1 site was constantly decreased, resulting from anisotropic expansion of the dodecahedral site. Consequently, these anisotropic modifications of coordination polyhedra seem to induce the thermal decomposition of katoite at 1123 K and 8 GPa.

Microstructural characteristics of Hadfield steel solidified under high pressure

NASA Astrophysics Data System (ADS)

Zhang, Yuzi; Li, Yanguo; Han, Bo; Zhang, Fucheng; Qian, Lihe

2011-12-01

Samples of Hadfield steel, high manganese austenite steel with 13 wt% manganese and 1.2 wt% carbon, were solidified under a pressure of 6 GPa. The microstructures of the samples were analyzed by metallography and X-ray diffraction. The results indicate that the solidification microstructure of the Hadfield steel was remarkably refined under high pressure. Additionally, the carbide of M23C6 was obtained in the Hadfield steel solidified under high pressure was different from the carbide of M3C obtained by solidification under normal pressure. Furthermore, high pressure promoted the formation of orientational solidified microstructure of the Hadfield steel.

Two-photon x-ray diffraction

DOE Office of Scientific and Technical Information (OSTI.GOV)

Stohr, J.

The interference pattern of a circular photon source has long been used to define the optical diffraction limit. Here we show the breakdown of conventional x-ray diffraction theory for the fundamental case of a “source”, consisting of a back-illuminated thin film in a circular aperture. When the conventional spontaneous x-ray scattering by atoms in the film is replaced at high incident intensity by stimulated resonant scattering, the film becomes the source of cloned photon twins and the diffraction pattern becomes self-focused beyond the diffraction limit. Furthermore, the case of cloned photon pairs is compared to and distinguished from entangled photonmore » pairs or biphotons.« less

Two-photon x-ray diffraction

DOE PAGES

Stohr, J.

2017-01-11

The interference pattern of a circular photon source has long been used to define the optical diffraction limit. Here we show the breakdown of conventional x-ray diffraction theory for the fundamental case of a “source”, consisting of a back-illuminated thin film in a circular aperture. When the conventional spontaneous x-ray scattering by atoms in the film is replaced at high incident intensity by stimulated resonant scattering, the film becomes the source of cloned photon twins and the diffraction pattern becomes self-focused beyond the diffraction limit. Furthermore, the case of cloned photon pairs is compared to and distinguished from entangled photonmore » pairs or biphotons.« less

Characterization of X80 and X100 Microalloyed Pipeline Steel Using Quantitative X-ray Diffraction

NASA Astrophysics Data System (ADS)

Wiskel, J. B.; Li, X.; Ivey, D. G.; Henein, H.

2018-06-01

Quantitative X-ray diffraction characterization of four (4) X80 and three (3) X100 microalloyed steels was undertaken. The effect of through-thickness position, processing parameters, and composition on the measured crystallite size, microstrain, and J index (relative magnitude of crystallographic texture) was determined. Microstructure analysis using optical microscopy, scanning electron microscopy, transmission electron microscopy, and electron-backscattered diffraction was also undertaken. The measured value of microstrain increased with increasing alloy content and decreasing cooling interrupt temperature. Microstructural features corresponding to crystallite size in the X80 steels were both above and below the detection limit for quantitative X-ray diffraction. The X100 steels consistently exhibited microstructure features below the crystallite size detection limit. The yield stress of each steel increased with increasing microstrain. The increase in microstrain from X80 to X100 is also associated with a change in microstructure from predominantly polygonal ferrite to bainitic ferrite.

Diffractive-refractive optics: (+,-,-,+) X-ray crystal monochromator with harmonics separation.

PubMed

Hrdý, Jaromír; Mikulík, Petr; Oberta, Peter

2011-03-01

A new kind of two channel-cut crystals X-ray monochromator in dispersive (+,-,-,+) position which spatially separates harmonics is proposed. The diffracting surfaces are oriented so that the diffraction is inclined. Owing to refraction the diffracted beam is sagittally deviated. The deviation depends on wavelength and is much higher for the first harmonics than for higher harmonics. This leads to spatial harmonics separation. The idea is supported by ray-tracing simulation.

Hydrothermal Diamond Anvil Cell (HDAC): From Visual Observation to X-ray Absorption Spectroscopy

NASA Astrophysics Data System (ADS)

Bassett, W. A.; Mibe, K.

2006-05-01

A fluid sample contained in a Re gasket between two diamond anvils can be subjected to pressures up to 2.5 GPa and temperatures up to 1200°C in a resistively heated hydrothermal diamond anvil cell (HDAC). Thermocouples are used to measure temperature. The constant-volume sample chamber permits isochoric measurements that can be used to determine pressure from the equation of state of H2O and to map phases and properties in P-T space. A movie of reactions between K-feldspar and water up to 2.5 GPa and 880°C illustrates the use of visual observations for mapping coexisting solution, melt, and solid phases. X-ray absorption spectroscopy of ZnBr2 in solution up to 500°C and 500 MPa shows hydrogen bond breaking in the hydration shells of the ZnBr42- and Br- ions with increasing temperature. In other studies the stability field of ikaite (CaCO3·6H2O) has been mapped by visual observation and Raman spectroscopy; the phases of montmorillonite have been mapped by X-ray diffraction; and the leaching of Pb from zircon has been measured by X-ray microprobe.

Changes in the chemical composition and spectroscopy of loblolly pine medium density fiberboard furnish as a function of age and refining pressure

Treesearch

Stephen S. Kelley; Thomas Elder; Leslie H. Groom

2005-01-01

Loblolly pine wood between the ages of 5-35 was refined into medium density fiberboard furnish at steam pressures from 2 to 18 bar, The effect of age and processing conditions on the properties of the fibers was assessed by wet chemical analyses, Near Infared Spectroscopy (NIR) and powder X-ray diffraction (XRD).In general ,the percentages of extractives and glucose...

Structure of Al-Fe alloys prepared by different methods after severe plastic deformation under pressure

NASA Astrophysics Data System (ADS)

Dobromyslov, A. V.; Taluts, N. I.

2017-06-01

Al-Fe alloys prepared by casting, rapid quenching from the melt, and mechanical alloying from elemental powders have been studied using X-ray diffraction analysis, optical metallography, transmission electron microscopy, and microhardness measurements in the initial state and after severe plastic deformation by high-pressure torsion using Bridgman anvils. The relationship between the phase composition, microstructure, and the microhardness of the investigated alloys has been established.

Structural and electronic evolution of Cr[subscript 2]O[subscript 3] on compression to 55 GPa

DOE Office of Scientific and Technical Information (OSTI.GOV)

Dera, Przemyslaw; Lavina, Barbara; Meng, Yue

2016-08-15

Synchrotron single-crystal x-ray diffraction experiments have been performed on corundum-type Cr{sub 2}O{sub 3} up to a pressure of 55 GPa in Ne and He pressure transmitting media. Diffraction experiments were complemented by measurements of optical absorption spectra with single crystal samples up to 60 GPa. Results of the diffraction data analysis rule out the earlier reported monoclinic distortion at 15-30 GPa, but indicate evidence of two discontinuous transitions of electronic or magnetic nature, most likely associated with a change in magnetic ordering and charge transfer. The compression mechanism established from single crystal refinements indicates much smaller distortion of the Cr{supmore » 3+} coordination environment than was previously assumed.« less

Room Temperature Elastic Moduli and Vickers Hardness of Hot-Pressed LLZO Cubic Garnet

DTIC Science & Technology

2012-01-01

polishing compounds, Leco, St. Joseph, MI). X - ray diffraction and scanning electron microscopy (SEM) The microstructure of the hot-pressed specimens...was examined on uncoated fracture surfaces by SEM with an accelerating voltage of 1 and 3 kV. Phase purity was evaluated from X - ray diffraction data...the micro- structure appeared to be homogenous for the two hot- pressed LLZO specimens included in this study (Fig. 1). X - ray diffraction confirmed that

Method for improve x-ray diffraction determinations of residual stress in nickel-base alloys

DOEpatents

Berman, Robert M.; Cohen, Isadore

1990-01-01

A process for improving the technique of measuring residual stress by x-ray diffraction in pieces of nickel-base alloys which comprises covering part of a predetermined area of the surface of a nickel-base alloy with a dispersion, exposing the covered and uncovered portions of the surface of the alloy to x-rays by way of an x-ray diffractometry apparatus, making x-ray diffraction determinations of the exposed surface, and measuring the residual stress in the alloy based on these determinations. The dispersion is opaque to x-rays and serves a dual purpose since it masks off unsatisfactory signals such that only a small portion of the surface is measured, and it supplies an internal standard by providing diffractogram peaks comparable to the peaks of the nickel alloy so that the alloy peaks can be very accurately located regardless of any sources of error external to the sample.

Revisiting pressure-induced phase transition in silicon clathrates using Ge substitution

DOE PAGES

Blancon, Jean-Christophe Robert; Machon, Denis; Pischedda, Vittoria; ...

2016-04-11

Ba 8Si 39Ge 7 and Ba 8Si 29Ge 17 have been studied at high pressure using x-ray diffraction and x-ray absorption spectroscopy (XAS) at the Ge K edge. In Ba 8Si 39Ge 7, a transition is observed similar to the one in Ba 8Si 46, apparently isostructural. However, the XAS data analysis shows that the transformation is related to the off-centering of the Ba atoms. A theoretical model based on a Landau potential suggests that this transition is second order, with a symmetry-breaking mechanism related to the Ba displacement probably initiated by the vacancy creation or local distortion predicted theoretically.more » Lastly, this analysis gives a coherent picture of the phase transition mechanism. In the case of Ba 8Si 29Ge 17, such phase transition is not observed as the Ba atoms appear already off-center at ambient pressure.« less

Shock driven melting and resolidification upon release in cerium

NASA Astrophysics Data System (ADS)

Bolme, Cindy; Bronkhorst, Curt; Brown, Don; Cherne, Frank; Cooley, Jason; Furlanetto, Michael; Gleason, Arianna; Jensen, Brian; Owens, Charles; Ali, Suzanne; Fratanduono, Dayne; Galtier, Eric; Granados, Eduardo; Lee, Hae Ja; Nagler, Bob

2017-06-01

The temperature rise due to increasing entropy during shock compression and the corresponding temperature decrease due to isentropic expansion upon release cause the physics of melting and solidification under dynamic pressure changes to differ fundamentally from the more common liquid-solid transitions governed by thermal diffusion. We investigated laser shock driven melting and resolidification during release in cerium to examine the dynamics of these processes. Cerium was selected as the material of study due to the low pressure at which γ-cerium melts along the principle Hugoniot and due to cerium's anomalous melt boundary at low pressure, which facilitates its transition from liquid to solid during isentropic release. The structural phase of cerium was probed with X-ray diffraction using the LCLS X-ray free electron laser, which provided in situ measurements of the transition dynamics. The experimental results will be presented showing the resolidification occurring over 10s of ns.

Combined single crystal polarized XAFS and XRD at high pressure: probing the interplay between lattice distortions and electronic order at multiple length scales in high T c cuprates

DOE PAGES

Fabbris, G.; Hücker, M.; Gu, G. D.; ...

2016-07-14

Some of the most exotic material properties derive from electronic states with short correlation length (~10-500 Å), suggesting that the local structural symmetry may play a relevant role in their behavior. In this study, we discuss the combined use of polarized x-ray absorption fine structure and x-ray diffraction at high pressure as a powerful method to tune and probe structural and electronic orders at multiple length scales. Besides addressing some of the technical challenges associated with such experiments, we illustrate this approach with results obtained in the cuprate La 1.875Ba 0.125CuO 4, in which the response of electronic order tomore » pressure can only be understood by probing the structure at the relevant length scales.« less

Revisiting pressure-induced phase transition in silicon clathrates using Ge substitution

DOE Office of Scientific and Technical Information (OSTI.GOV)

Blancon, Jean-Christophe Robert; Machon, Denis; Pischedda, Vittoria

Ba 8Si 39Ge 7 and Ba 8Si 29Ge 17 have been studied at high pressure using x-ray diffraction and x-ray absorption spectroscopy (XAS) at the Ge K edge. In Ba 8Si 39Ge 7, a transition is observed similar to the one in Ba 8Si 46, apparently isostructural. However, the XAS data analysis shows that the transformation is related to the off-centering of the Ba atoms. A theoretical model based on a Landau potential suggests that this transition is second order, with a symmetry-breaking mechanism related to the Ba displacement probably initiated by the vacancy creation or local distortion predicted theoretically.more » Lastly, this analysis gives a coherent picture of the phase transition mechanism. In the case of Ba 8Si 29Ge 17, such phase transition is not observed as the Ba atoms appear already off-center at ambient pressure.« less

Shock-absorbing and failure mechanisms of WS2 and MoS2 nanoparticles with fullerene-like structures under shock wave pressure.

PubMed

Zhu, Yan Qiu; Sekine, Toshimori; Li, Yan Hui; Fay, Michael W; Zhao, Yi Min; Patrick Poa, C H; Wang, Wen Xin; Roe, Martin J; Brown, Paul D; Fleischer, Niles; Tenne, Reshef

2005-11-23

The excellent shock-absorbing performance of WS2 and MoS2 nanoparticles with inorganic fullerene-like structures (IFs) under very high shock wave pressures of 25 GPa is described. The combined techniques of X-ray diffraction, Raman spectroscopy, X-ray photoelectron spectroscopy, thermal analysis, and transmission electron microscopy have been used to evaluate the diverse, intriguing features of shock recovered IFs, of interest for their tribological applications, thereby allowing improved understanding of their antishock behavior and structure-property relationships. Two possible failure mechanisms are proposed and discussed. The supershock-absorbing ability of the IF-WS2 enables them to survive pressures up to 25 GPa accompanied with concurrent temperatures of up to 1000 degrees C without any significant structural degradation or phase change making them probably the strongest cage molecules now known.

Geometry of α-Cr2O3(0001) as a Function of H2O Partial Pressure

PubMed Central

2015-01-01

Surface X-ray diffraction has been employed to elucidate the surface structure of α-Cr2O3(0001) as a function of water partial pressure at room temperature. In ultra high vacuum, following exposure to ∼2000 Langmuir of H2O, the surface is found to be terminated by a partially occupied double layer of chromium atoms. No evidence of adsorbed OH/H2O is found, which is likely due to either adsorption at minority sites, or X-ray induced desorption. At a water partial pressure of ∼30 mbar, a single OH/H2O species is found to be bound atop each surface Cr atom. This adsorption geometry does not agree with that predicted by ab initio calculations, which may be a result of some differences between the experimental conditions and those modeled. PMID:26877825

Raman and X-Ray Investigation of High-Temperature Methane in the Diamond Anvil Cell

NASA Astrophysics Data System (ADS)

Spaulding, D.; Weck, G.; Loubeyre, P.; Mezouar, M.

2016-12-01

The chemistry and equations of state of simple molecular systems are of extreme importance to planetary astrophysics and for accurate characterization of reaction products and pathways at high pressures and temperatures. Simple molecules such as H2O, CO2 and CH4 are model systems for understanding the effects of pressure on chemical bonding. Here we present recent work to conduct fine-scale studies of the vibrational, chemical and structural properties of CH4 at pressures and temperatures up to 12 GPa and 1000K, with particular attention to behavior in the vicinity of the melting curve. We present results from resistive and laser-heating experiments, coupled with Raman spectroscopy. In addition, high P/T synchrotron powder x-ray diffraction provides tight constraints on melting and solid structure. Our results favor a somewhat higher melting curve and lower dissociative stability limit for the CH4 molecule than other recent work.

Optical and mechanical properties of nanocrystalline ZrC thin films grown by pulsed laser deposition.

DOE PAGES

Craciun, D.; Socol, G.; Lambers, E.; ...

2015-01-17

Thin ZrC films (<500 nm) were grown on (100) Si substrates at a substrate temperature of 500 °C by the pulsed laser deposition (PLD) technique using a KrF excimer laser under different CH 4 pressures. Glancing incidence X-ray diffraction showed that films were nanocrystalline, while X-ray reflectivity studies found out films were very dense and exhibited a smooth surface morphology. Optical spectroscopy data shows that the films have high reflectivity (>90%) in the infrared region, characteristic of metallic behavior. Nanoindentation results indicated that films deposited under lower CH 4 pressures exhibited slightly higher nanohardness and Young modulus values than filmsmore » deposited under higher pressures. As a result, tribological characterization revealed that these films exhibited relatively high wear resistance and steady-state friction coefficients on the order of μ = 0.4.« less

First in-situ monitoring of CO2 delivery to the mantle followed by compression melting, using synchrotron generated X-ray diffraction.

NASA Astrophysics Data System (ADS)

Hammouda, Tahar; Chantel, Julien; Manthilake, Geeth; Guignard, Jérémy; Crichton, Wilson; Gaillard, Fabrice

2014-05-01

Melting of peridotite + CO2 upon compression has been directly monitored in situ, for the first time. We have combined high pressure experiments in the multianvil apparatus with synchrotron-generated X-ray diffraction, in order to monitor sample decarbonation upon heating, followed by melting upon compression. Experiments were performed in the model system CaO-MgO-SiO2+CO2, using dolomite and silicates contained in graphite capsules as starting material. Save Al, starting composition was aimed at reproducing peridotitic system. The sample was first compressed at room temperature, then heated. Decarbonation was observed at 2.2 GPa and 1100°C. After further heating to 1300°C, pressure was increased. Melting was observed at 2.7 GPa, while temperature was kept at 1300°C. All transformations were followed using X-ray diffraction. Starting with silicate + carbonate mixtures, we were thus able to keep CO2 fluid in the experimental sample at high P and T, up to the solidus. Concerning carbon recycling at subduction zones, it is known that CO2 is a non-wetting fluid in silicate aggregates. Therefore, any CO2 resulting from carbonate breakdown likely remains trapped at grain corners either in the subducted lithosphere or in the mantle wedge before eventually being trapped in mantle minerals as fluid inclusions, due to dynamic recrystallization. In this way, CO2 released from the slab may be spread laterally due to mantle convection. Entrainment to further depths by deep subduction or in convection cells induces CO2 introduction to depth wherein the solidus can be crossed, due to pressure increase. The solidus corresponds to the so-called carbonate ledge, beyond which carbonatitic melts are produced. Therefore, compression melting of CO2-bearing lithologies is a way to produce carbonatitic melts at depths corresponding to about 80 km. This mechanism is a viable explanation for the observed geophysical anomalies, such as those revealed by electrical conductivity measurements.

Phase degradation in B xGa 1–xN films grown at low temperature by metalorganic vapor phase epitaxy

DOE PAGES

Gunning, Brendan P.; Moseley, Michael W.; Koleske, Daniel D.; ...

2016-11-01

Using metalorganic vapor phase epitaxy, a comprehensive study of B xGa 1-xN growth on GaN and AlN templates is described. BGaN growth at high-temperature and high-pressure results in rough surfaces and poor boron incorporation efficiency, while growth at low-temperature and low-pressure (750–900 °C and 20 Torr) using nitrogen carrier gas results in improved surface morphology and boron incorporation up to ~7.4% as determined by nuclear reaction analysis. However, further structural analysis by transmission electron microscopy and x-ray pole figures points to severe degradation of the high boron composition films, into a twinned cubic structure with a high density of stackingmore » faults and little or no room temperature photoluminescence emission. Films with <1% triethylboron (TEB) flow show more intense, narrower x-ray diffraction peaks, near-band-edge photoluminescence emission at ~362 nm, and primarily wurtzite-phase structure in the x-ray pole figures. For films with >1% TEB flow, the crystal structure becomes dominated by the cubic phase. As a result, only when the TEB flow is zero (pure GaN), does the cubic phase entirely disappear from the x-ray pole figure, suggesting that under these growth conditions even very low boron compositions lead to mixed crystalline phases.« less

Phase degradation in B xGa 1–xN films grown at low temperature by metalorganic vapor phase epitaxy

DOE Office of Scientific and Technical Information (OSTI.GOV)

Gunning, Brendan P.; Moseley, Michael W.; Koleske, Daniel D.

Using metalorganic vapor phase epitaxy, a comprehensive study of B xGa 1-xN growth on GaN and AlN templates is described. BGaN growth at high-temperature and high-pressure results in rough surfaces and poor boron incorporation efficiency, while growth at low-temperature and low-pressure (750–900 °C and 20 Torr) using nitrogen carrier gas results in improved surface morphology and boron incorporation up to ~7.4% as determined by nuclear reaction analysis. However, further structural analysis by transmission electron microscopy and x-ray pole figures points to severe degradation of the high boron composition films, into a twinned cubic structure with a high density of stackingmore » faults and little or no room temperature photoluminescence emission. Films with <1% triethylboron (TEB) flow show more intense, narrower x-ray diffraction peaks, near-band-edge photoluminescence emission at ~362 nm, and primarily wurtzite-phase structure in the x-ray pole figures. For films with >1% TEB flow, the crystal structure becomes dominated by the cubic phase. As a result, only when the TEB flow is zero (pure GaN), does the cubic phase entirely disappear from the x-ray pole figure, suggesting that under these growth conditions even very low boron compositions lead to mixed crystalline phases.« less

Structural investigation of porcine stomach mucin by X-ray fiber diffraction and homology modeling

DOE Office of Scientific and Technical Information (OSTI.GOV)

Veluraja, K., E-mail: veluraja@msuniv.ac.in; Vennila, K.N.; Umamakeshvari, K.

Research highlights: {yields} Techniques to get oriented mucin fibre. {yields} X-ray fibre diffraction pattern for mucin. {yields} Molecular modeling of mucin based on X-ray fibre diffraction pattern. -- Abstract: The basic understanding of the three dimensional structure of mucin is essential to understand its physiological function. Technology has been developed to achieve orientated porcine stomach mucin molecules. X-ray fiber diffraction of partially orientated porcine stomach mucin molecules show d-spacing signals at 2.99, 4.06, 4.22, 4.7, 5.37 and 6.5 A. The high intense d-spacing signal at 4.22 A is attributed to the antiparallel {beta}-sheet structure identified in the fraction of themore » homology modeled mucin molecule (amino acid residues 800-980) using Nidogen-Laminin complex structure as a template. The X-ray fiber diffraction signal at 6.5 A reveals partial organization of oligosaccharides in porcine stomach mucin. This partial structure of mucin will be helpful in establishing a three dimensional structure for the whole mucin molecule.« less

A nearly on-axis spectroscopic system for simultaneously measuring UV-visible absorption and X-ray diffraction in the SPring-8 structural genomics beamline.

PubMed

Sakaguchi, Miyuki; Kimura, Tetsunari; Nishida, Takuma; Tosha, Takehiko; Sugimoto, Hiroshi; Yamaguchi, Yoshihiro; Yanagisawa, Sachiko; Ueno, Go; Murakami, Hironori; Ago, Hideo; Yamamoto, Masaki; Ogura, Takashi; Shiro, Yoshitsugu; Kubo, Minoru

2016-01-01

UV-visible absorption spectroscopy is useful for probing the electronic and structural changes of protein active sites, and thus the on-line combination of X-ray diffraction and spectroscopic analysis is increasingly being applied. Herein, a novel absorption spectrometer was developed at SPring-8 BL26B2 with a nearly on-axis geometry between the X-ray and optical axes. A small prism mirror was placed near the X-ray beamstop to pass the light only 2° off the X-ray beam, enabling spectroscopic analysis of the X-ray-exposed volume of a crystal during X-ray diffraction data collection. The spectrometer was applied to NO reductase, a heme enzyme that catalyzes NO reduction to N2O. Radiation damage to the heme was monitored in real time during X-ray irradiation by evaluating the absorption spectral changes. Moreover, NO binding to the heme was probed via caged NO photolysis with UV light, demonstrating the extended capability of the spectrometer for intermediate analysis.

Investigating the Effects of Low Temperature Annealing of Amorphous Corrosion Resistant Alloys.

DTIC Science & Technology

1980-11-01

Ray Diffraction.................................................... 6 Differential Scanning Calorimetry....................................... 9...17 LIST OF FIGURES Figure 1. X- Ray Diffraction Results From Fe32Ni 36Cr 4P 2 B Annealed for One Hour at...Various Temperatures (Cr Ka Radiation) ................................. 7 Figure 2. X- Ray Diffraction Results From FeU2NiaeCr14SieB Annealed for One

Mild Hydroprocessing with Dispersed Catalyst of Highly Asphaltenic Pitch

NASA Astrophysics Data System (ADS)

Isquierdo, Fernanda

Asphaltene are known to have diverse negative impacts on heavy oil extraction and hydroprocessing. This research then, explores the optimal conditions to convert asphaltenes into lighter material using mild conditions of pressure and temperature, and investigates changes in asphaltene structure during hydroprocessing. Feedstock and products were characterized by Simulated Distillation, Microdeasphalting, Sulfur content, X-ray diffraction, X-ray photoelectron spectroscopy, and Nuclear magnetic resonance spectroscopy. Solid catalysts were analyzed by Themogravimetric analysis, X-ray diffraction, and Dynamic light scattering. Based on the results obtained from X-ray diffraction and Nuclear magnetic resonance spectroscopy analysis a mechanism for the asphaltene hydroprocessing at mild conditions is proposed in which the alky peripheric portion from the original asphaltenes is partially removed during the reaction. The consequence of that process being an increase in the stacking of the aromatics sheets in the remaining asphaltenes. Also, this study investigates different for ultradispersed catalyst compositions, where CoWS, CoMoS, NiWS, FeWS, NiMo/NaHFeSi 2O6 and NaHFeSi2O6 showed a high asphaltene conversion as determined by asphaltene microdeasphalting, FeMoS and NaHFeSi 2O6 presented a high Vacuum Residue as determined by distillation (SIMDIST) analysis conversion, and in terms of sulfur removal CoMoS gave the higher conversion. In addition, all the catalyst tested showed a coke production lower than 1%. Finally, a kinetic study for the pitch hydroprocessing using CoMoS as catalysts gave a global activation energy of 97.3 kJ/mol.

Ultrafast studies of shock-induced melting and phase transitions at LCLS

NASA Astrophysics Data System (ADS)

McMahon, Malcolm

The study of shock-induced phase transitions, which is vital to the understanding of material response to rapid pressure changes, dates back to the 1950s, when Bankcroft et al reported a transition in iron. Since then, many transitions have been reported in a wide range of materials, but, due to the lack of sufficiently bright x-ray sources, the structural details of these new phases has been notably lacking. While the development of nanosecond in situ x-ray diffraction has meant that lattice-level studies of such phenomena have become possible, including studies of the phase transition reported 60 years ago in iron, the quality of the diffraction data from such studies is noticeably poorer than that obtained from statically-compressed samples on synchrotrons. The advent of x-ray free electron lasers (XFELs), such as the LCLS, has resulted in an unprecedented improvement in the quality of diffraction data that can be obtained from shock-compressed matter. Here I describe the results from three recent experiment at the LCLS that looked at the solid-solid and solid-liquid phase transitions in Sb, Bi and Sc using single 50 fs x-ray exposures. The results provide new insight into the structural changes and melting induced by shock compression. This work is supported by EPSRC under Grant No. EP/J017051/1. Use of the LCLS, SLAC National Accelerator Laboratory, is supported by the U.S. Department of Energy, Office of Science, Office of Basic Energy Sciences under Contract No. DE-AC02-76SF00515.

Evidence from x-ray and neutron powder diffraction patterns that the so-called icosahedral and decagonal quasicrystals of MnAl(6) and other alloys are twinned cubic crystals.

PubMed

Pauling, L

1987-06-01

It is shown that the x-ray powder diffraction patterns of rapidly quenched MnAl(6) and Mg(32)(Al,Zn)(49) and the neutron powder diffraction pattern of MnAl(6) are compatible with the proposed 820-atom primitive cubic structure [Pauling, L. (1987) Phys. Rev. Lett. 58, 365-368]. The values found for the edge of the unit cube are 23.365 A (x-ray) and 23.416 A (neutron) for MnAl(6) and 24.313 A (x-ray) for Mg(32)(Al,Zn)(49).

Evidence from x-ray and neutron powder diffraction patterns that the so-called icosahedral and decagonal quasicrystals of MnAl6 and other alloys are twinned cubic crystals

PubMed Central

Pauling, Linus

1987-01-01

It is shown that the x-ray powder diffraction patterns of rapidly quenched MnAl6 and Mg32(Al,Zn)49 and the neutron powder diffraction pattern of MnAl6 are compatible with the proposed 820-atom primitive cubic structure [Pauling, L. (1987) Phys. Rev. Lett. 58, 365-368]. The values found for the edge of the unit cube are 23.365 Å (x-ray) and 23.416 Å (neutron) for MnAl6 and 24.313 Å (x-ray) for Mg32(Al,Zn)49. PMID:16593841

Charge disproportionation and the pressure-induced insulator–metal transition in cubic perovskite PbCrO3

PubMed Central

Cheng, Jinguang; Kweon, K. E.; Larregola, S. A.; Ding, Yang; Shirako, Y.; Marshall, L. G.; Li, Z.-Y.; Li, X.; dos Santos, António M.; Suchomel, M. R.; Matsubayashi, K.; Uwatoko, Y.; Hwang, G. S.; Goodenough, John B.; Zhou, J.-S.

2015-01-01

The perovskite PbCrO3 is an antiferromagnetic insulator. However, the fundamental interactions leading to the insulating state in this single-valent perovskite are unclear. Moreover, the origin of the unprecedented volume drop observed at a modest pressure of P = 1.6 GPa remains an outstanding problem. We report a variety of in situ pressure measurements including electron transport properties, X-ray absorption spectrum, and crystal structure study by X-ray and neutron diffraction. These studies reveal key information leading to the elucidation of the physics behind the insulating state and the pressure-induced transition. We argue that a charge disproportionation 3Cr4+ → 2Cr3+ + Cr6+ in association with the 6s-p hybridization on the Pb2+ is responsible for the insulating ground state of PbCrO3 at ambient pressure and the charge disproportionation phase is suppressed under pressure to give rise to a metallic phase at high pressure. The model is well supported by density function theory plus the correlation energy U (DFT+U) calculations. PMID:25624483

Charge disproportionation and the pressure-induced insulator–metal transition in cubic perovskite PbCrO 3

DOE PAGES

Cheng, Jinguang; Kweon, K. E.; Larregola, S. A.; ...

2015-01-26

The perovskite PbCrO 3 is an antiferromagnetic insulator. But, the fundamental interactions leading to the insulating state in this single-valent perovskite are unclear. Moreover, the origin of the unprecedented volume drop observed at a modest pressure of P = 1.6 GPa remains an outstanding problem. Our report shows a variety of in situ pressure measurements including electron transport properties, X-ray absorption spectrum, and crystal structure study by X-ray and neutron diffraction. These studies reveal key information leading to the elucidation of the physics behind the insulating state and the pressure-induced transition. Furthermore, we argue that a charge disproportionation 3Cr 4+more » → 2Cr 3+ + Cr 6+ in association with the 6s-p hybridization on the Pb 2+ is responsible for the insulating ground state of PbCrO 3 at ambient pressure and the charge disproportionation phase is suppressed under pressure to give rise to a metallic phase at high pressure. The model is well supported by density function theory plus the correlation energy U (DFT + U) calculations.« less

High-energy X-ray diffraction using the Pixium 4700 flat-panel detector.

PubMed

Daniels, J E; Drakopoulos, M

2009-07-01

The Pixium 4700 detector represents a significant step forward in detector technology for high-energy X-ray diffraction. The detector design is based on digital flat-panel technology, combining an amorphous Si panel with a CsI scintillator. The detector has a useful pixel array of 1910 x 2480 pixels with a pixel size of 154 microm x 154 microm, and thus it covers an effective area of 294 mm x 379 mm. Designed for medical imaging, the detector has good efficiency at high X-ray energies. Furthermore, it is capable of acquiring sequences of images at 7.5 frames per second in full image mode, and up to 60 frames per second in binned region of interest modes. Here, the basic properties of this detector applied to high-energy X-ray diffraction are presented. Quantitative comparisons with a widespread high-energy detector, the MAR345 image plate scanner, are shown. Other properties of the Pixium 4700 detector, including a narrow point-spread function and distortion-free image, allows for the acquisition of high-quality diffraction data at high X-ray energies. In addition, high frame rates and shutterless operation open new experimental possibilities. Also provided are the necessary data for the correction of images collected using the Pixium 4700 for diffraction purposes.

Development of synchrotron X-ray micro-tomography under extreme conditions of pressure and temperature.

PubMed

Álvarez-Murga, M; Perrillat, J P; Le Godec, Y; Bergame, F; Philippe, J; King, A; Guignot, N; Mezouar, M; Hodeau, J L

2017-01-01

X-ray tomography is a non-destructive three-dimensional imaging/microanalysis technique selective to a wide range of properties such as density, chemical composition, chemical states and crystallographic structure with extremely high sensitivity and spatial resolution. Here the development of in situ high-pressure high-temperature micro-tomography using a rotating module for the Paris-Edinburgh cell combined with synchrotron radiation is described. By rotating the sample chamber by 360°, the limited angular aperture of ordinary high-pressure cells is surmounted. Such a non-destructive high-resolution probe provides three-dimensional insight on the morphological and structural evolution of crystalline as well as amorphous phases during high pressure and temperature treatment. To demonstrate the potentials of this new experimental technique the compression behavior of a basalt glass is investigated by X-ray absorption tomography, and diffraction/scattering tomography imaging of the structural changes during the polymerization of C 60 molecules under pressure is performed. Small size and weight of the loading frame and rotating module means that this apparatus is portable, and can be readily installed on most synchrotron facilities to take advantage of the diversity of three-dimensional imaging techniques available at beamlines. This experimental breakthrough should open new ways for in situ imaging of materials under extreme pressure-temperature-stress conditions, impacting diverse areas in physics, chemistry, geology or materials sciences.

Crystallization and preliminary X-ray diffraction analysis of a chitin-binding domain of hyperthermophilic chitinase from Pyrococcus furiosus

DOE Office of Scientific and Technical Information (OSTI.GOV)

Nakamura, Tsutomu; Ishikawa, Kazuhiko; Hagihara, Yoshihisa

The expression, purification and preliminary X-ray diffraction studies of a chitin-binding domain of the chitinase from P. furiosus are reported. The crystallization and preliminary X-ray diffraction analysis of the chitin-binding domain of chitinase from a hyperthermophilic archaeon, Pyrococcus furiosus, are reported. The recombinant protein was prepared using an Escherichia coli overexpression system and was crystallized by the hanging-drop vapour-diffusion method. An X-ray diffraction data set was collected to 1.70 Å resolution. The crystal belonged to space group P4{sub 3}2{sub 1}2 or P4{sub 1}2{sub 1}2. The unit-cell parameters were determined to be a = b = 48.8, c = 85.0 Å.

Long-Wavelength X-Ray Diffraction and Its Applications in Macromolecular Crystallography.

PubMed

Weiss, Manfred S

2017-01-01

For many years, diffraction experiments in macromolecular crystallography at X-ray wavelengths longer than that of Cu-K α (1.54 Å) have been largely underappreciated. Effects caused by increased X-ray absorption result in the fact that these experiments are more difficult than the standard diffraction experiments at short wavelengths. However, due to the also increased anomalous scattering of many biologically relevant atoms, important additional structural information can be obtained. This information, in turn, can be used for phase determination, for substructure identification, in molecular replacement approaches, as well as in structure refinement. This chapter reviews the possibilities and the difficulties associated with such experiments, and it provides a short description of two macromolecular crystallography synchrotron beam lines dedicated to long-wavelength X-ray diffraction experiments.

Data processing software suite SITENNO for coherent X-ray diffraction imaging using the X-ray free-electron laser SACLA.

PubMed

Sekiguchi, Yuki; Oroguchi, Tomotaka; Takayama, Yuki; Nakasako, Masayoshi

2014-05-01

Coherent X-ray diffraction imaging is a promising technique for visualizing the structures of non-crystalline particles with dimensions of micrometers to sub-micrometers. Recently, X-ray free-electron laser sources have enabled efficient experiments in the `diffraction before destruction' scheme. Diffraction experiments have been conducted at SPring-8 Angstrom Compact free-electron LAser (SACLA) using the custom-made diffraction apparatus KOTOBUKI-1 and two multiport CCD detectors. In the experiments, ten thousands of single-shot diffraction patterns can be collected within several hours. Then, diffraction patterns with significant levels of intensity suitable for structural analysis must be found, direct-beam positions in diffraction patterns determined, diffraction patterns from the two CCD detectors merged, and phase-retrieval calculations for structural analyses performed. A software suite named SITENNO has been developed to semi-automatically apply the four-step processing to a huge number of diffraction data. Here, details of the algorithm used in the suite are described and the performance for approximately 9000 diffraction patterns collected from cuboid-shaped copper oxide particles reported. Using the SITENNO suite, it is possible to conduct experiments with data processing immediately after the data collection, and to characterize the size distribution and internal structures of the non-crystalline particles.

Data processing software suite SITENNO for coherent X-ray diffraction imaging using the X-ray free-electron laser SACLA

PubMed Central

Sekiguchi, Yuki; Oroguchi, Tomotaka; Takayama, Yuki; Nakasako, Masayoshi

2014-01-01

Coherent X-ray diffraction imaging is a promising technique for visualizing the structures of non-crystalline particles with dimensions of micrometers to sub-micrometers. Recently, X-ray free-electron laser sources have enabled efficient experiments in the ‘diffraction before destruction’ scheme. Diffraction experiments have been conducted at SPring-8 Angstrom Compact free-electron LAser (SACLA) using the custom-made diffraction apparatus KOTOBUKI-1 and two multiport CCD detectors. In the experiments, ten thousands of single-shot diffraction patterns can be collected within several hours. Then, diffraction patterns with significant levels of intensity suitable for structural analysis must be found, direct-beam positions in diffraction patterns determined, diffraction patterns from the two CCD detectors merged, and phase-retrieval calculations for structural analyses performed. A software suite named SITENNO has been developed to semi-automatically apply the four-step processing to a huge number of diffraction data. Here, details of the algorithm used in the suite are described and the performance for approximately 9000 diffraction patterns collected from cuboid-shaped copper oxide particles reported. Using the SITENNO suite, it is possible to conduct experiments with data processing immediately after the data collection, and to characterize the size distribution and internal structures of the non-crystalline particles. PMID:24763651

Spectroscopic imaging, diffraction, and holography with x-ray photoemission

DOE Office of Scientific and Technical Information (OSTI.GOV)

Not Available

1992-02-01

X-ray probes are capable of determining the spatial structure of an atom in a specific chemical state, over length scales from about a micron all the way down to atomic resolution. Examples of these probes include photoemission microscopy, energy-dependent photoemission diffraction, photoelectron holography, and X-ray absorption microspectroscopy. Although the method of image formation, chemical-state sensitivity, and length scales can be very different, these X-ray techniques share a common goal of combining a capability for structure determination with chemical-state specificity. This workshop will address recent advances in holographic, diffraction, and direct imaging techniques using X-ray photoemission on both theoretical and experimentalmore » fronts. A particular emphasis will be on novel structure determinations with atomic resolution using photoelectrons.« less

An instrument for in situ coherent x-ray studies of metal-organic vapor phase epitaxy of III-nitrides.

PubMed

Ju, Guangxu; Highland, Matthew J; Yanguas-Gil, Angel; Thompson, Carol; Eastman, Jeffrey A; Zhou, Hua; Brennan, Sean M; Stephenson, G Brian; Fuoss, Paul H

2017-03-01

We describe an instrument that exploits the ongoing revolution in synchrotron sources, optics, and detectors to enable in situ studies of metal-organic vapor phase epitaxy (MOVPE) growth of III-nitride materials using coherent x-ray methods. The system includes high-resolution positioning of the sample and detector including full rotations, an x-ray transparent chamber wall for incident and diffracted beam access over a wide angular range, and minimal thermal sample motion, giving the sub-micron positional stability and reproducibility needed for coherent x-ray studies. The instrument enables surface x-ray photon correlation spectroscopy, microbeam diffraction, and coherent diffraction imaging of atomic-scale surface and film structure and dynamics during growth, to provide fundamental understanding of MOVPE processes.

An instrument for in situ coherent x-ray studies of metal-organic vapor phase epitaxy of III-nitrides

NASA Astrophysics Data System (ADS)

Ju, Guangxu; Highland, Matthew J.; Yanguas-Gil, Angel; Thompson, Carol; Eastman, Jeffrey A.; Zhou, Hua; Brennan, Sean M.; Stephenson, G. Brian; Fuoss, Paul H.

2017-03-01

We describe an instrument that exploits the ongoing revolution in synchrotron sources, optics, and detectors to enable in situ studies of metal-organic vapor phase epitaxy (MOVPE) growth of III-nitride materials using coherent x-ray methods. The system includes high-resolution positioning of the sample and detector including full rotations, an x-ray transparent chamber wall for incident and diffracted beam access over a wide angular range, and minimal thermal sample motion, giving the sub-micron positional stability and reproducibility needed for coherent x-ray studies. The instrument enables surface x-ray photon correlation spectroscopy, microbeam diffraction, and coherent diffraction imaging of atomic-scale surface and film structure and dynamics during growth, to provide fundamental understanding of MOVPE processes.

Algan/Gan Hemt By Magnetron Sputtering System

NASA Astrophysics Data System (ADS)

Garcia Perez, Roman

In this thesis, the growth of the semiconductor materials AlGaN and GaN is achieved by magnetron sputtering for the fabrication of High Electron Mobility Transistors (HEMTs). The study of the deposited nitrides is conducted by spectroscopy, diffraction, and submicron scale microscope methods. The preparation of the materials is performed using different parameters in terms of power, pressure, temperature, gas, and time. Silicon (Si) and Sapphire (Al2O3) wafers are used as substrates. The chemical composition and surface topography of the samples are analyzed to calculate the materials atomic percentages and to observe the devices surface. The instruments used for the semiconductors characterization are X-ray Photoelectron Spectroscopy (XPS), X-ray Diffraction (XRD), Scanning Electron Microscopy (SEM), and Atomic Force Microscope (AFM). The project focused its attention on the reduction of impurities during the deposition, the controlled thicknesses of the thin-films, the atomic configuration of the alloy AlxGa1-xN, and the uniformity of the surfaces.

High-pressure X-ray diffraction and Raman spectroscopy of CaFe2O4-type β-CaCr2O4

NASA Astrophysics Data System (ADS)

Zhai, Shuangmeng; Yin, Yuan; Shieh, Sean R.; Shan, Shuangming; Xue, Weihong; Wang, Ching-Pao; Yang, Ke; Higo, Yuji

2016-04-01

In situ high-pressure synchrotron X-ray diffraction and Raman spectroscopic studies of orthorhombic CaFe2O4-type β-CaCr2O4 chromite were carried out up to 16.2 and 32.0 GPa at room temperature using multi-anvil apparatus and diamond anvil cell, respectively. No phase transition was observed in this study. Fitting a third-order Birch-Murnaghan equation of state to the P-V data yields a zero-pressure volume of V 0 = 286.8(1) Å3, an isothermal bulk modulus of K 0 = 183(5) GPa and the first pressure derivative of isothermal bulk modulus K 0' = 4.1(8). Analyses of axial compressibilities show anisotropic elasticity for β-CaCr2O4 since the a-axis is more compressible than the b- and c-axis. Based on the obtained and previous results, the compressibility of several CaFe2O4-type phases was compared. The high-pressure Raman spectra of β-CaCr2O4 were analyzed to determine the pressure dependences and mode Grüneisen parameters of Raman-active bands. The thermal Grüneisen parameter of β-CaCr2O4 is determined to be 0.93(2), which is smaller than those of CaFe2O4-type CaAl2O4 and MgAl2O4.

Reversible phase transition in vanadium oxide films sputtered on metal substrates

NASA Astrophysics Data System (ADS)

Palai, Debajyoti; Carmel Mary Esther, A.; Porwal, Deeksha; Pradeepkumar, Maurya Sandeep; Raghavendra Kumar, D.; Bera, Parthasarathi; Sridhara, N.; Dey, Arjun

2016-11-01

Vanadium oxide films, deposited on aluminium (Al), titanium (Ti) and tantalum (Ta) metal substrates by pulsed RF magnetron sputtering at a working pressure of 1.5 x10-2 mbar at room temperature are found to display mixed crystalline vanadium oxide phases viz., VO2, V2O3, V2O5. The films have been characterized by field-emission scanning electron microscopy, X-ray diffraction, differential scanning calorimetry (DSC) and X-ray photoelectron spectroscopy, and their thermo-optical and electrical properties have been investigated. Studies of the deposited films by DSC have revealed a reversible-phase transition found in the temperature range of 45-49 °C.

Combined X-ray and neutron fibre diffraction studies of biological and synthetic polymers

NASA Astrophysics Data System (ADS)

Parrot, I. M.; Urban, V.; Gardner, K. H.; Forsyth, V. T.

2005-08-01

The fibrous state is a natural one for polymer molecules which tend to assume regular helical conformations rather than the globular structures characteristic of many proteins. Fibre diffraction therefore has broad application to the study of a wide range of biological and synthetic polymers. The purpose of this paper is to illustrate the general scope of the method and in particular to demonstrate the impact of a combined approach involving both X-ray and neutron diffraction methods. While the flux of modern X-ray synchrotron radiation sources allows high quality datasets to be recorded with good resolution within a very short space of time, neutron studies can provide unique information through the ability to locate hydrogen or deuterium atoms that are often difficult or impossible to locate using X-ray methods. Furthermore, neutron fibre diffraction methods can, through the ability to selectively label specific parts of a structure, be used to highlight novel aspects of polymer structure that can not be studied using X-rays. Two examples are given. The first describes X-ray and neutron diffraction studies of conformational transitions in DNA. The second describes structural studies of the synthetic high-performance polymer poly(p-phenylene terephthalamide) (PPTA), known commercially as Kevlar® or Twaron®.

Conceptual Design for Time-Resolved X-ray Diffraction in a Single Laser-Driven Compression Experiment

NASA Astrophysics Data System (ADS)

Benedetti, Laura Robin; Eggert, J. H.; Kilkenny, J. D.; Bradley, D. K.; Bell, P. M.; Palmer, N. E.; Rygg, J. R.; Boehly, T. R.; Collins, G. W.; Sorce, C.

2017-06-01

Since X-ray diffraction is the most definitive method for identifying crystalline phases of a material, it is an important technique for probing high-energy-density materials during laser-driven compression experiments. We are developing a design for collecting several x-ray diffraction datasets during a single laser-driven experiment, with a goal of achieving temporal resolution better than 1ns. The design combines x-ray streak cameras, for a continuous temporal record of diffraction, with fast x-ray imagers, to collect several diffraction patterns with sufficient solid angle range and resolution to identify crystalline texture. Preliminary experiments will be conducted at the Omega laser and then implemented at the National Ignition Facility. We will describe the status of the conceptual design, highlighting tradeoffs in the design process. We will also discuss the technical issues that must be addressed in order to develop a successful experimental platform. These include: Facility-specific geometric constraints such as unconverted laser light and target alignment; EMP issues when electronic diagnostics are close to the target; X-ray source requirements; and detector capabilities. This work was performed under the auspices of the U.S. Department of Energy by Lawrence Livermore National Laboratory under Contract DE-AC52-07NA27344, LLNL-ABS-725146.

High-pressure synthesis, amorphization, and decomposition of silane.

PubMed

Hanfland, Michael; Proctor, John E; Guillaume, Christophe L; Degtyareva, Olga; Gregoryanz, Eugene

2011-03-04

By compressing elemental silicon and hydrogen in a diamond anvil cell, we have synthesized polymeric silicon tetrahydride (SiH(4)) at 124 GPa and 300 K. In situ synchrotron x-ray diffraction reveals that the compound forms the insulating I4(1)/a structure previously proposed from ab initio calculations for the high-pressure phase of silane. From a series of high-pressure experiments at room and low temperature on silane itself, we find that its tetrahedral molecules break up, while silane undergoes pressure-induced amorphization at pressures above 60 GPa, recrystallizing at 90 GPa into the polymeric crystal structures.

IDATEN and G-SITENNO: GUI-assisted software for coherent X-ray diffraction imaging experiments and data analyses at SACLA.

PubMed

Sekiguchi, Yuki; Yamamoto, Masaki; Oroguchi, Tomotaka; Takayama, Yuki; Suzuki, Shigeyuki; Nakasako, Masayoshi

2014-11-01

Using our custom-made diffraction apparatus KOTOBUKI-1 and two multiport CCD detectors, cryogenic coherent X-ray diffraction imaging experiments have been undertaken at the SPring-8 Angstrom Compact free electron LAser (SACLA) facility. To efficiently perform experiments and data processing, two software suites with user-friendly graphical user interfaces have been developed. The first is a program suite named IDATEN, which was developed to easily conduct four procedures during experiments: aligning KOTOBUKI-1, loading a flash-cooled sample into the cryogenic goniometer stage inside the vacuum chamber of KOTOBUKI-1, adjusting the sample position with respect to the X-ray beam using a pair of telescopes, and collecting diffraction data by raster scanning the sample with X-ray pulses. Named G-SITENNO, the other suite is an automated version of the original SITENNO suite, which was designed for processing diffraction data. These user-friendly software suites are now indispensable for collecting a large number of diffraction patterns and for processing the diffraction patterns immediately after collecting data within a limited beam time.

Dynamical diffraction imaging (topography) with X-ray synchrotron radiation

NASA Technical Reports Server (NTRS)

Kuriyama, M.; Steiner, B. W.; Dobbyn, R. C.

1989-01-01

By contrast to electron microscopy, which yields information on the location of features in small regions of materials, X-ray diffraction imaging can portray minute deviations from perfect crystalline order over larger areas. Synchrotron radiation-based X-ray optics technology uses a highly parallel incident beam to eliminate ambiguities in the interpretation of image details; scattering phenomena previously unobserved are now readily detected. Synchrotron diffraction imaging renders high-resolution, real-time, in situ observations of materials under pertinent environmental conditions possible.

Development of Thin Films as Potential Structural Cathodes to Enable Multifunctional Energy-Storage Structural Composite Batteries for the U.S. Army’s Future Force

DTIC Science & Technology

2011-09-01

glancing angle X - ray diffraction (GAXRD), atomic force microscopy (AFM), scanning electron microscopy (SEM), and electrochemical...Emission SEM FWHM full width at half maximum GAXRD glancing angle X - ray diffraction H3COCH2CH2OH 2-methoxyethanol LiMn2O4 lithium manganese oxide...were characterized by scanning electron microscopy (SEM), X - ray diffraction (XRD), and atomic force microscopy (AFM). In addition,

Simultaneous X-ray fluorescence and scanning X-ray diffraction microscopy at the Australian Synchrotron XFM beamline

DOE Office of Scientific and Technical Information (OSTI.GOV)

Jones, Michael W. M.; Phillips, Nicholas W.; van Riessen, Grant A.

2016-08-11

Owing to its extreme sensitivity, quantitative mapping of elemental distributionsviaX-ray fluorescence microscopy (XFM) has become a key microanalytical technique. The recent realisation of scanning X-ray diffraction microscopy (SXDM) meanwhile provides an avenue for quantitative super-resolved ultra-structural visualization. The similarity of their experimental geometries indicates excellent prospects for simultaneous acquisition. Here, in both step- and fly-scanning modes, robust, simultaneous XFM-SXDM is demonstrated.

Structure and bulk modulus of Ln-doped UO2 (Ln = La, Nd) at high pressure

NASA Astrophysics Data System (ADS)

Rittman, Dylan R.; Park, Sulgiye; Tracy, Cameron L.; Zhang, Lei; Palomares, Raul I.; Lang, Maik; Navrotsky, Alexandra; Mao, Wendy L.; Ewing, Rodney C.

2017-07-01

The structure of lanthanide-doped uranium dioxide, LnxU1-xO2-0.5x+y (Ln = La, Nd), was investigated at pressures up to ∼50-55 GPa. Samples were synthesized with different lanthanides at different concentrations (x ∼ 0.2 and 0.5), and all were slightly hyperstoichiometric (y ∼ 0.25-0.4). In situ high-pressure synchrotron X-ray diffraction was used to investigate their high-pressure phase behavior and determine their bulk moduli. All samples underwent a fluorite-to-cotunnite phase transformation with increasing pressure. The pressure of the phase transformation increased with increasing hyperstoichiometry, which is consistent with results from previous computational simulations. Bulk moduli are inversely proportional to both the ionic radius of the lanthanide and its concentration, as quantified using a weighted cationic radius ratio. This trend was found to be consistent with the behavior of other elastic properties measured for Ln-doped UO2, such as Young's modulus.

An Excel Spreadsheet for a One-Dimensional Fourier Map in X-ray Crystallography

ERIC Educational Resources Information Center

Clegg, William

2004-01-01

The teaching of crystal structure determination with single-crystal X-ray diffraction at undergraduate level faces numerous challenges. Single-crystal X-ray diffraction is used in a vast range of chemical research projects and forms the basis for a high proportion of structural results that are presented to high-school, undergraduate, and graduate…

Laser-induced Multi-energy Processing in Diamond Growth

DTIC Science & Technology

2012-05-01

microscopy (SEM) and energy dispersive X - ray (EDX) measurements, Drs. Yi Liu and Shah Valloppilly from Nebraska Center for Materials and Nanoscience...NCMN) at UNL for help on X - Ray diffraction (XRD) measurements, and Professor Steve W. Martin and Dr. Young Sik Kim from the Department of Material...spectroscopy and X - ray diffraction ................... 62 4.4 Conclusions

Pressure induced band inversion, electronic and structural phase transitions in InTe: A combined experimental and theoretical study

NASA Astrophysics Data System (ADS)

Rajaji, V.; Pal, Koushik; Sarma, Saurav Ch.; Joseph, B.; Peter, Sebastian C.; Waghmare, Umesh V.; Narayana, Chandrabhas

2018-04-01

We report high-pressure Raman scattering measurements on the tetragonal phase of InTe corroborated with the first-principles density functional theory and synchrotron x-ray diffraction measurements. Anomalous pressure-dependent linewidths of the A1 g and Eg phonon modes provide evidence of an isostructural electronic transition at ˜3.6 GPa . The first-principles theoretical analysis reveals that it is associated with a semiconductor-to-metal transition due to increased density of states near the Fermi level. Further, this pressure induced metallization acts as a precursor for structural phase transition to a face centered cubic phase (F m 3 ¯m ) at ˜6.0 GPa . Interestingly, theoretical results reveal a pressure induced band inversion at the Z and M points of the Brillouin zone corresponding to pressures ˜1.0 and ˜1.4 GPa , respectively. As the parity of bands undergoing inversions is the same, the topology of the electronic state remains unchanged, and hence InTe retains its trivial band topology (Z2=0 ) . The pressure dependent behavior of the A1 g and Eg modes can be understood based on the results from the synchrotron x-ray diffraction, which shows anisotropic compressibility of the lattice in the a and c directions. Our Raman measurements up to ˜19 GPa further confirms the pressure induced structural phase transition from a face-centered to primitive cubic (F m 3 ¯m to P m 3 ¯m ) at P ˜15 GPa .

Thermal equation of state of Molybdenum determined from in situ synchrotron X-ray diffraction with laser-heated diamond anvil cells

DOE Office of Scientific and Technical Information (OSTI.GOV)

Huang, Xiaoli; Li, Fangfei; Zhou, Qiang

Here we report that the equation of state (EOS) of Mo is obtained by an integrated technique of laser-heated DAC and synchrotron X-ray diffraction. The cold compression and thermal expansion of Mo have been measured up to 80 GPa at 300 K, and 92 GPa at 3470 K, respectively. The P-V-T data have been treated with both thermodynamic and Mie–Gruneisen-Debye methods for the thermal EOS inversion. The results are self-consistent and in agreement with the static multi-anvil compression data of Litasov et al. (J. Appl. Phys. 113, 093507 (2013)) and the theoretical data of Zeng et al. (J. Phys. Chem.more » B 114, 298 (2010)). Furthermore, these high pressure and high temperature (HPHT) data with high precision firstly complement and close the gap between the resistive heating and the shock compression experiment.« less

Thermal equation of state of Molybdenum determined from in situ synchrotron X-ray diffraction with laser-heated diamond anvil cells

DOE PAGES

Huang, Xiaoli; Li, Fangfei; Zhou, Qiang; ...

2016-02-17

Here we report that the equation of state (EOS) of Mo is obtained by an integrated technique of laser-heated DAC and synchrotron X-ray diffraction. The cold compression and thermal expansion of Mo have been measured up to 80 GPa at 300 K, and 92 GPa at 3470 K, respectively. The P-V-T data have been treated with both thermodynamic and Mie–Gruneisen-Debye methods for the thermal EOS inversion. The results are self-consistent and in agreement with the static multi-anvil compression data of Litasov et al. (J. Appl. Phys. 113, 093507 (2013)) and the theoretical data of Zeng et al. (J. Phys. Chem.more » B 114, 298 (2010)). Furthermore, these high pressure and high temperature (HPHT) data with high precision firstly complement and close the gap between the resistive heating and the shock compression experiment.« less

Single-crystal X-ray diffraction study of SrGeO3 high-pressure perovskite phase at 100 K

NASA Astrophysics Data System (ADS)

Nakatsuka, Akihiko; Arima, Hiroshi; Ohtaka, Osamu; Fujiwara, Keiko; Yoshiasa, Akira

2017-10-01

Single-crystal X-ray diffraction study of SrGeO3 perovskite (cubic; space group Pmɜ¯m) synthesized at 6 GPa and 1223 K was conducted at a low temperature of 100 K. The residual electron density revealed the presence of the bonding electron at the center of the Ge-O bond, in accordance with our previous conclusion that the Ge-O bond is strongly covalent. From comparison with our previous structure-refinement result at 296 K, the mean square displacement (MSD) of the O atom in the direction of the Ge-O bond is suggested to exhibit no significant temperature dependence, in contrast to that in the direction perpendicular to the bond. Thus, the strong covalency of the Ge-O bond can have a large influence on the temperature dependence of thermal vibration of the O atom.

Raman and and x-ray diffraction study of iron and iron-nickel alloys at varying P-T conditions

NASA Astrophysics Data System (ADS)

Goncharov, A.; Struzhkin, V.; Gregoryanz, E.; Maddury, S.; Huang, E.; Hemley, R. J.; Mao, H.

2002-05-01

High-pressure properties of iron and iron-rich alloys are crucial for understanding of the Earth interior, because iron is the major constitute element of the Earth core. Using recently developed [1,2] Raman spectroscopy technique for shear elastic modulus determination, we studied iron-rich alloys of Ni (0 to 20 % Ni) up to 150 GPa, and also at varying temperatures (78-400 K). We find substantial decrease of the Raman hcp-phonon frequency compared to the pure iron, and also considerable anharmonic temperature effects. In contrast, low-temperature x-ray diffraction measurements indicate a usual temperature variation of the lattice constants. Possible implications to the Earth core composition and properties are discussed. [1] A. P. Jephcoat, H. Olijnyk, K. Refson, Eos 80, F929 (1999). [2] S. Merkel et al., Science 288, 1626 (2000).

Performance Characteristics of Waste Glass Powder Substituting Portland Cement in Mortar Mixtures

NASA Astrophysics Data System (ADS)

Kara, P.; Csetényi, L. J.; Borosnyói, A.

2016-04-01

In the present work, soda-lime glass cullet (flint, amber, green) and special glass cullet (soda-alkaline earth-silicate glass coming from low pressure mercury-discharge lamp cullet and incandescent light bulb borosilicate glass waste cullet) were ground into fine powders in a laboratory planetary ball mill for 30 minutes. CEM I 42.5N Portland cement was applied in mortar mixtures, substituted with waste glass powder at levels of 20% and 30%. Characterisation and testing of waste glass powders included fineness by laser diffraction particle size analysis, specific surface area by nitrogen adsorption technique, particle density by pycnometry and chemical analysis by X-ray fluorescence spectrophotometry. Compressive strength, early age shrinkage cracking and drying shrinkage tests, heat of hydration of mortars, temperature of hydration, X-ray diffraction analysis and volume stability tests were performed to observe the influence of waste glass powder substitution for Portland cement on physical and engineering properties of mortar mixtures.

Substrate temperature effect on structural and optical properties of Bi2Te3 thin films

NASA Astrophysics Data System (ADS)

Jariwala, B. S.; Shah, D. V.; Kheraj, Vipul

2012-06-01

Structural and optical properties of Bi2Te3 thin films, thermally evaporated on well-cleaned glass substrates at different substrate temperatures, are reported here. X-ray diffraction was carried out for the structural characterization. XRD patterns of the films exhibit preferential orientation along the [0 1 5] direction for the films deposited at all the substrate temperatures together with other supported planes [2 0 5] & [1 1 0]. All other deposition conditions like thickness, deposition rate and pressure were maintained same throughout the experiment. X-ray diffraction lines confirm that the grown films are polycrystalline in nature with hexagonal crystal structure. The effect of substrate temperature on lattice constants, grain size, micro strain, number of crystallites and dislocation density have been investigated and reported in this paper. Also the substrate temperature effect on the optical property has been also investigated using the FTIR spectroscopy.

Two-dimensional time-resolved X-ray diffraction study of liquid/solid fraction and solid particle size in Fe-C binary system with an electrostatic levitator furnace

NASA Astrophysics Data System (ADS)

Yonemura, M.; Okada, J.; Watanabe, Y.; Ishikawa, T.; Nanao, S.; Shobu, T.; Toyokawa, H.

2013-03-01

Liquid state provides functions such as matter transport or a reaction field and plays an important role in manufacturing processes such as refining, forging or welding. However, experimental procedures are significantly difficult for an observation of solidification process of iron and iron-based alloys in order to identify rapid transformations subjected to fast temperature evolution. Therefore, in order to study the solidification in iron and iron-based alloys, we considered a combination of high energy X-ray diffraction measurements and an electrostatic levitation method (ESL). In order to analyze the liquid/solid fraction, the solidification of melted spherical specimens was measured at a time resolution of 0.1 seconds during rapid cooling using the two-dimensional time-resolved X-ray diffraction. Furthermore, the observation of particle sizes and phase identification was performed on a trial basis using X-ray small angle scattering with X-ray diffraction.

Imaging single cells in a beam of live cyanobacteria with an X-ray laser.

PubMed

van der Schot, Gijs; Svenda, Martin; Maia, Filipe R N C; Hantke, Max; DePonte, Daniel P; Seibert, M Marvin; Aquila, Andrew; Schulz, Joachim; Kirian, Richard; Liang, Mengning; Stellato, Francesco; Iwan, Bianca; Andreasson, Jakob; Timneanu, Nicusor; Westphal, Daniel; Almeida, F Nunes; Odic, Dusko; Hasse, Dirk; Carlsson, Gunilla H; Larsson, Daniel S D; Barty, Anton; Martin, Andrew V; Schorb, Sebastian; Bostedt, Christoph; Bozek, John D; Rolles, Daniel; Rudenko, Artem; Epp, Sascha; Foucar, Lutz; Rudek, Benedikt; Hartmann, Robert; Kimmel, Nils; Holl, Peter; Englert, Lars; Duane Loh, Ne-Te; Chapman, Henry N; Andersson, Inger; Hajdu, Janos; Ekeberg, Tomas

2015-02-11

There exists a conspicuous gap of knowledge about the organization of life at mesoscopic levels. Ultra-fast coherent diffractive imaging with X-ray free-electron lasers can probe structures at the relevant length scales and may reach sub-nanometer resolution on micron-sized living cells. Here we show that we can introduce a beam of aerosolised cyanobacteria into the focus of the Linac Coherent Light Source and record diffraction patterns from individual living cells at very low noise levels and at high hit ratios. We obtain two-dimensional projection images directly from the diffraction patterns, and present the results as synthetic X-ray Nomarski images calculated from the complex-valued reconstructions. We further demonstrate that it is possible to record diffraction data to nanometer resolution on live cells with X-ray lasers. Extension to sub-nanometer resolution is within reach, although improvements in pulse parameters and X-ray area detectors will be necessary to unlock this potential.

Growth of ternary CdxZn1-xO thin films in oxygen ambient using pulsed laser deposition

NASA Astrophysics Data System (ADS)

Sharma, Sugandha; Saini, Basant; Kaur, Ravinder; Gupta, Vinay; Tomar, Monika; Kapoor, Avinashi

2018-05-01

This study reports the growth of cadmium alloyed zinc (CdxZn1-xO) oxide thin films using pulsed laser deposition. The films are deposited on Corning glass substrates at different oxygen pressures of 5, 20, and 40 mTorr. High resolution X-ray diffraction studies reveal mixed phase (hexagonal and cubic) for films deposited at 20 and 40 mTorr, while a cubic phase for film deposited at 5 mTorr pressure. Optical transmittance studies indicate red-shifting of transmission edge as oxygen pressure decreases to 5 mTorr from 20 mTorr, hinting at a possible increase in cadmium content in thin films. Minimum band gap energy is obtained at growth pressure of 5 mTorr. Resistivity measurements have been performed using Hall effect measurement set up at 298 K.

Studies on X-ray diffraction microscopy

NASA Astrophysics Data System (ADS)

Miao, Huijie

This dissertation includes three main parts: studies on coherence requirements for the diffraction microscopy experiments, ice formation on frozen-hydrated sample during data collection, and centering of the diffraction data sets. These three subjects are all in support of our groups overall goal of high resolution 3D imaging of frozen hydrated eukaryotic cells via x-ray diffraction microscopy. X-ray diffraction microscopy requires coherent illumination. However, the actual degree of coherence at some beamlines has never been tested. In research on coherence, our first aim is to determine the transverse coherence width at the sample plane at BL 9.0.1 at the Advanced Light Source in Lawrence Berkeley National Laboratory. An analytical calculation of the coherence at the sample plane is presented. Experimental diffraction patterns of pinhole-pair samples were also taken at the beamline to determine the coherence. Due to the irregular shape of the pinholes and other optics complexity, it was very difficult to fit the data with known theoretical equations as it was traditionally done with 1D data. However, we found out that the auto-correlation function shows clearly three spots. Theoretical calculation have been carried out to show that the degree of coherence can be obtained from the intensities of the three spots. These results are compared with the results from the analytical calculation. We then perform a simulation, showing the required transverse coherence width for reconstructing samples with a given size. Ice accumulation has been a major problem in X-ray diffraction microscopy with frozen hydrated samples. Since the ice structure is different from point to point, we cannot subtract the scattering from ice, nor assume a completely "empty" region outside the finite support constraint area as required for reconstruction. Ice forms during the sample preparation and transfer. However, from the tests we did in September 2007, we found that the ice layer thickens significantly during the data collecting process. One of the tests we did was putting a dry room-temperature grid into the beam, cooling it down to liquid nitrogen temperature, and then collecting the diffraction pattern of it over time. This test showed that, after the cold grid remained in the chamber for a while, a ring could be observed in the diffraction pattern. The time necessary for this ring to be visible is highly dependent on the pressure and vacuum history of the chamber. We will discuss how the chamber pressure influences the ice accumulation rate, how an anti-contamination device can help to reduce the rate, and how this ring forms. The last part of the research is based on simulations and a real data set collected on beamline 9.0.1 at the ALS in Berkeley. In X-ray diffraction microscopy, one of the major challenges when processing the data is to accurately determine the true center of the recorded data; that is, the zero spatial frequency position. Simulations of reconstructing shifted data show that if the center of a 2D diffraction pattern is shifted by more than 3 pixels from its true center, the positivity constraint to the phase, which otherwise might be applied to improve the convergence of the reconstruction algorithm, cannot be imposed. Moreover, the phase unwrapping problem may appear during the reconstruction. These issues undermine the quality of the reconstruction of 2D data. Furthermore, the individual shift in each 2D pattern will lead to errors when assembling a 3D diffraction data cube, making the 3D reconstruction very difficult. We developed a method which uses power spectra of the partial diffraction pattern to pre-align the data. A reconstruction without severe phase unwrapping can then be obtained from the pre-aligned data. Next, the precise zero spatial frequency position can be found by examining the linear ramp present in the reconstructed phase. This method was applied to a freeze-dried yeast data set to show that this approach is effective with experimental data.

Toward comprehensive studies of liquids at high pressures and high temperatures: Combined structure, elastic wave velocity, and viscosity measurements in the Paris-Edinburgh cell

DOE Office of Scientific and Technical Information (OSTI.GOV)

Kono, Yoshio; Park, Changyong; Kenney-Benson, Curtis

2014-08-19

Techniques for measuring liquid structure, elastic wave velocity, and viscosity under high pressure have been integrated using a Paris–Edinburgh cell at Beamline 16-BM-B, HPCAT of the Advanced Photon Source. The Paris–Edinburgh press allows for compressing large volume samples (up to 2 mm in both diameter and length) up to ~7 GPa and 2000 °C. Multi-angle energy dispersive X-ray diffraction provides structure factors of liquid to a large Q of ~19 Å. Ultrasonic techniques have been developed to investigate elastic wave velocity of liquids combined with the X-ray imaging. Falling sphere viscometry, using high-speed X-ray radiography (>1000 frames/s), enables us tomore » investigate a wide range of viscosity, from those of high viscosity silicates or oxides melts to low viscosity (<1 mPa s) liquids and fluids such as liquid metals or salts. The integration of these multiple techniques has promoted comprehensive studies of structure and physical properties of liquids as well as amorphous materials at high pressures and high temperatures, making it possible to investigate correlations between structure and physical properties of liquids in situ.« less

Luminescent properties under X-ray excitation of Ba(1-x)PbxWO4 disordered solid solution

NASA Astrophysics Data System (ADS)

Bakiz, B.; Hallaoui, A.; Taoufyq, A.; Benlhachemi, A.; Guinneton, F.; Villain, S.; Ezahri, M.; Valmalette, J.-C.; Arab, M.; Gavarri, J.-R.

2018-02-01

A series of polycrystalline barium-lead tungstate Ba1-xPbxWO4 with 0 ≤ x ≤ 1 was synthesized using a classical solid-state method with thermal treatment at 1000 °C. These materials were characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM), Fourier Transform Raman (FT-Raman) spectroscopy. X-ray diffraction profile analyses were performed using Rietveld method. These materials crystallized in the scheelite tetragonal structure and behaved as quasi ideal solid solution. Raman spectroscopy confirmed the formation of the solid solution. Structural distortions were evidenced in X-ray diffraction profiles and in vibration Raman spectra. The scanning electron microscopy experiments showed large and rounded irregular grains. Luminescence experiments were performed under X-ray excitation. The luminescence emission profiles have been interpreted in terms of four Gaussian components, with a major contribution of blue emission. The integrated intensity of luminescence reached a maximum value in the composition range x = 0.3-0.6, in relation with distortions of crystal lattice.

Amorphous Phase Characterization Through X-Ray Diffraction Profile Modeling: Implications for Amorphous Phases in Gale Crater Rocks and Soils

NASA Technical Reports Server (NTRS)

Achilles, C. N.; Downs, G. W.; Downs, R. T.; Morris, R. V.; Rampe, E. B.; Ming, D. W.; Chipera, S. J.; Blake, D. F.; Vaniman, D. T.; Bristow, T. F.;

High Pressure Strength Study on NaCl

NASA Astrophysics Data System (ADS)

Mi, Z.; Shieh, S. R.; High Pressure Mineral Physics Group

2010-12-01

Yield strength is regarded as one important property related to rheological characteristics of minerals in the Earth’s interior. The strength study of NaCl, a popular pressure medium in static high pressure experiments, has been carried out under non-hydrostatic conditions in a diamond anvil cell up to 43 GPa at room temperature using radial energy dispersive X-ray diffraction technique. Phase transformation from B1 (rock salt structure) to B2 (CsCl structure) starts at 29.4 GPa, and is complete at 32.1 GPa. Bulk modulus obtained by third order Birch-Manurgham equation of state is 25.5 GPa with pressure derivative 4.6 for B1 phase, and 30.78 GPa with pressure derivative 4.32 GPa for B2 phase, which are in a good agreement with previous studies. The differential stress of NaCl B1 phase shows very gentle increase with pressure, which indicates that NaCl is a very good pressure-transmitting medium at pressure below 30 GPa. However, the differential stress increases more abruptly for B2 phase and this may imply that NaCl can no longer be regarded as a “soft” pressure medium at very high pressures. For B1 phase, (111) is the strongest plane and (200) is the weakest plane, while (200) becomes the strongest plane in B2 phase. Pure NaCl is weaker than mixture MgO and NaCl, which indicates that soft material become stronger when mixed with hard material. The yield strength of B2 obtained through energy dispersive X-ray diffraction technique increase linearly, while the value derived by pressure gradient method shows jagged trend.

Thermal and structural alternations in CuAlMnNi shape memory alloy by the effect of different pressure applications

NASA Astrophysics Data System (ADS)

Canbay, Canan Aksu; Polat, Tercan

2017-09-01

In this work the effects of the applied pressure on the characteristic transformation temperatures, the high temperature order-disorder phase transitions, the variation in diffraction peaks and the surface morphology of the CuAlMnNi shape memory alloy was investigated. The evolution of the transformation temperatures was studied by differential scanning calorimetry (DSC) with different heating and cooling rates. The differential thermal analysis measurements were performed to obtain the ordered-disordered phase transformations from room temperature to 900 °C. The characteristic transformation temperatures and the thermodynamic parameters were highly sensitive to variations in the applied pressure and also the applied pressure affected the thermodynamic parameters. The activation energy of the sample according to applied pressure values calculated by Kissinger method. The structural changes of the samples were studied by X-ray diffraction (XRD) measurements and by optical microscope observations at room temperature.

In situ observation of high-pressure phase transition in silicon carbide under shock loading using ultrafast x-ray diffraction

NASA Astrophysics Data System (ADS)

Tracy, Sally June

2017-06-01

SiC is an important high-strength ceramic material used for a range of technological applications, including lightweight impact shielding and abrasives. SiC is also relevant to geology and planetary science. It may be a host of reduced carbon in the Earth's interior and also occurs in meteorites and impact sites. SiC has also been put forward as a possible major constituent in the proposed class of extra-solar planets known as carbon planets. Previous studies have used wave profile measurements to identify a phase transition under shock loading near 1 Mbar, but lattice-level structural information was not obtained. Here we present the behavior of silicon carbide under shock loading as investigated through a series of time-resolved pump-probe x-ray diffraction measurements up to 200 GPa. Our experiments were conducted at the Materials in Extreme Conditions beamline of the Linac Coherent Light Source. In situ x-ray diffraction data on shock-compressed SiC was collected using a free electron laser source combined with a pulsed high-energy laser. These measurements allow for the determination of time-dependent atomic arrangements, demonstrating that the wurtzite phase of SiC transforms directly to the B1 structure. Our measurements also reveal details of the material texture evolution under shock loading and release.

In situ observation of stishovite formation in shock-compressed fused silica

NASA Astrophysics Data System (ADS)

Tracy, Sally June; Turneaure, Stefan; Duffy, Thomas

2017-06-01

Silica, SiO2, has widespread applications ranging from optical components to refractory materials and is of geological importance as one of the major oxide components of the Earth's crust and mantle. The response of silica phases to dynamic loading has long been of interest for understanding the structural evolution of this fundamental oxide. Under shock compression both crystalline quartz and fused silica are characterized by the occurrence of a broad `mixed-phase region' (15-40 GPa) and a dense, high-pressure phase with much lower compressibility. Despite decades of study, the nature of this transformation and the identity of the high-pressure phase(s) remain poorly understood. In situ x-ray diffraction experiments on shock-compressed fused silica were conducted at the Dynamic Compression Sector of the Advanced Photon Source. The lattice-level structure was investigated through time-resolved x-ray diffraction measurements on samples reaching peak stress ranging from 12 to 47 GPa. Our results demonstrate that SiO2 adopts a dense amorphous structure in the `mixed-phase region' and abruptly transforms to stishovite above 34 GPa. These results provide clear evidence that high-pressure crystalline silicate phases can form from amorphous starting materials on the time-scale of laboratory shock experiments.

Effect of Destined High-Pressure Torsion on the Structure and Mechanical Properties of Rare Earth-Based Metallic Glasses

NASA Astrophysics Data System (ADS)

Zhao, W.; Cheng, H.; Jiang, X.; Wu, M. L.; Li, G.

2018-03-01

Changes in the atomic structure and mechanical properties of rare earth-based metallic glasses caused by destined high-pressure torsion (HPT) were studied by X-ray diffraction synchrotron radiation and nanoindentation. Results showed that destined HPT improved nanohardness and wear resistance, which indicated the significant contributions of this technique. The diffraction patterns showed that the contents of pairs between solvent and solute atoms with a large negative mixing enthalpy increased, whereas those of pairs between solvent atoms and between solute atoms decreased after destined HPT. Thus, the process was improved by increasing the proportion of high-intensity pairs between solvent and solute atoms.

X-ray Diffraction, Big and Small

NASA Image and Video Library

2012-10-30

A conventional X-ray diffraction instrument left is the size of a large refrigerator, in contrast to the compact size of the Chemistry and Mineralogy CheMin instrument on NASA Curiosity rover top right.

Coherent diffraction of single Rice Dwarf virus particles using hard X-rays at the Linac Coherent Light Source

PubMed Central

Munke, Anna; Andreasson, Jakob; Aquila, Andrew; Awel, Salah; Ayyer, Kartik; Barty, Anton; Bean, Richard J.; Berntsen, Peter; Bielecki, Johan; Boutet, Sébastien; Bucher, Maximilian; Chapman, Henry N.; Daurer, Benedikt J.; DeMirci, Hasan; Elser, Veit; Fromme, Petra; Hajdu, Janos; Hantke, Max F.; Higashiura, Akifumi; Hogue, Brenda G.; Hosseinizadeh, Ahmad; Kim, Yoonhee; Kirian, Richard A.; Reddy, Hemanth K.N.; Lan, Ti-Yen; Larsson, Daniel S.D.; Liu, Haiguang; Loh, N. Duane; Maia, Filipe R.N.C.; Mancuso, Adrian P.; Mühlig, Kerstin; Nakagawa, Atsushi; Nam, Daewoong; Nelson, Garrett; Nettelblad, Carl; Okamoto, Kenta; Ourmazd, Abbas; Rose, Max; van der Schot, Gijs; Schwander, Peter; Seibert, M. Marvin; Sellberg, Jonas A.; Sierra, Raymond G.; Song, Changyong; Svenda, Martin; Timneanu, Nicusor; Vartanyants, Ivan A.; Westphal, Daniel; Wiedorn, Max O.; Williams, Garth J.; Xavier, Paulraj Lourdu; Yoon, Chun Hong; Zook, James

2016-01-01

Single particle diffractive imaging data from Rice Dwarf Virus (RDV) were recorded using the Coherent X-ray Imaging (CXI) instrument at the Linac Coherent Light Source (LCLS). RDV was chosen as it is a well-characterized model system, useful for proof-of-principle experiments, system optimization and algorithm development. RDV, an icosahedral virus of about 70 nm in diameter, was aerosolized and injected into the approximately 0.1 μm diameter focused hard X-ray beam at the CXI instrument of LCLS. Diffraction patterns from RDV with signal to 5.9 Ångström were recorded. The diffraction data are available through the Coherent X-ray Imaging Data Bank (CXIDB) as a resource for algorithm development, the contents of which are described here. PMID:27478984

Signal-to-noise and radiation exposure considerations in conventional and diffraction x-ray microscopy

DOE PAGES

Huang, Xiaojing; Miao, Huijie; Steinbrener, Jan; ...

2009-01-01

Using a signal-to-noise ratio estimation based on correlations between multiple simulated images, we compare the dose efficiency of two soft x-ray imaging systems: incoherent brightfield imaging using zone plate optics in a transmission x-ray microscope (TXM), and x-ray diffraction microscopy (XDM) where an image is reconstructed from the far-field coherent diffraction pattern. In XDM one must computationally phase weak diffraction signals; in TXM one suffers signal losses due to the finite numerical aperture and efficiency of the optics. In simulations with objects representing isolated cells such as yeast, we find that XDM has the potential for delivering equivalent resolution imagesmore » using fewer photons. As a result, this can be an important advantage for studying radiation-sensitive biological and soft matter specimens.« less

Utilizing broadband X-rays in a Bragg coherent X-ray diffraction imaging experiment

DOE PAGES

Cha, Wonsuk; Liu, Wenjun; Harder, Ross; ...

2016-07-26

A method is presented to simplify Bragg coherent X-ray diffraction imaging studies of complex heterogeneous crystalline materials with a two-stage screening/imaging process that utilizes polychromatic and monochromatic coherent X-rays and is compatible with in situ sample environments. Coherent white-beam diffraction is used to identify an individual crystal particle or grain that displays desired properties within a larger population. A three-dimensional reciprocal-space map suitable for diffraction imaging is then measured for the Bragg peak of interest using a monochromatic beam energy scan that requires no sample motion, thus simplifyingin situchamber design. This approach was demonstrated with Au nanoparticles and will enable,more » for example, individual grains in a polycrystalline material of specific orientation to be selected, then imaged in three dimensions while under load.« less

Coherent diffraction of single Rice Dwarf virus particles using hard X-rays at the Linac Coherent Light Source

DOE PAGES

Munke, Anna; Andreasson, Jakob; Aquila, Andrew; ...

2016-08-01

Single particle diffractive imaging data from Rice Dwarf Virus (RDV) were recorded using the Coherent X-ray Imaging (CXI) instrument at the Linac Coherent Light Source (LCLS). RDV was chosen as it is a well-characterized model system, useful for proof-of-principle experiments, system optimization and algorithm development. RDV, an icosahedral virus of about 70 nm in diameter, was aerosolized and injected into the approximately 0.1 μm diameter focused hard X-ray beam at the CXI instrument of LCLS. Diffraction patterns from RDV with signal to 5.9 Ångström were recorded. Here, the diffraction data are available through the Coherent X-ray Imaging Data Bank (CXIDB)more » as a resource for algorithm development, the contents of which are described here.« less

Influence of neutron irradiation on the microstructure of nuclear graphite: An X-ray diffraction study

NASA Astrophysics Data System (ADS)

Zhou, Z.; Bouwman, W. G.; Schut, H.; van Staveren, T. O.; Heijna, M. C. R.; Pappas, C.

2017-04-01

Neutron irradiation effects on the microstructure of nuclear graphite have been investigated by X-ray diffraction on virgin and low doses (∼ 1.3 and ∼ 2.2 dpa), high temperature (750° C) irradiated samples. The diffraction patterns were interpreted using a model, which takes into account the turbostratic disorder. Besides the lattice constants, the model introduces two distinct coherent lengths in the c-axis and the basal plane, that characterise the volumes from which X-rays are scattered coherently. The methodology used in this work allows to quantify the effect of irradiation damage on the microstructure of nuclear graphite seen by X-ray diffraction. The results show that the changes of the deduced structural parameters are in agreement with previous observations from electron microscopy, but not directly related to macroscopic changes.

Utilizing broadband X-rays in a Bragg coherent X-ray diffraction imaging experiment.

PubMed

Cha, Wonsuk; Liu, Wenjun; Harder, Ross; Xu, Ruqing; Fuoss, Paul H; Hruszkewycz, Stephan O

2016-09-01

A method is presented to simplify Bragg coherent X-ray diffraction imaging studies of complex heterogeneous crystalline materials with a two-stage screening/imaging process that utilizes polychromatic and monochromatic coherent X-rays and is compatible with in situ sample environments. Coherent white-beam diffraction is used to identify an individual crystal particle or grain that displays desired properties within a larger population. A three-dimensional reciprocal-space map suitable for diffraction imaging is then measured for the Bragg peak of interest using a monochromatic beam energy scan that requires no sample motion, thus simplifying in situ chamber design. This approach was demonstrated with Au nanoparticles and will enable, for example, individual grains in a polycrystalline material of specific orientation to be selected, then imaged in three dimensions while under load.

Time-spliced X-ray diffraction imaging of magnetism dynamics in a NdNiO3 thin film

NASA Astrophysics Data System (ADS)

Beyerlein, Kenneth R.

2018-03-01

Diffraction imaging of nonequilibrium dynamics at atomic resolution is becoming possible with X-ray free-electron lasers. However, there are unresolved problems with applying this method to objects that are confined in only one dimension. Here I show that reliable one-dimensional coherent diffraction imaging is possible by splicing together images recovered from different time delays in an optical pump X-ray probe experiment. The time and space evolution of antiferromagnetic order in a vibrationally excited complex oxide heterostructure is recovered from time-resolved measurements of a resonant soft X-ray diffraction peak. Midinfrared excitation of the substrate is shown to lead to a demagnetization front that propagates at a velocity exceeding the speed of sound, a critical observation for the understanding of driven phase transitions in complex condensed matter.

Coherent diffraction of single Rice Dwarf virus particles using hard X-rays at the Linac Coherent Light Source.

PubMed

Munke, Anna; Andreasson, Jakob; Aquila, Andrew; Awel, Salah; Ayyer, Kartik; Barty, Anton; Bean, Richard J; Berntsen, Peter; Bielecki, Johan; Boutet, Sébastien; Bucher, Maximilian; Chapman, Henry N; Daurer, Benedikt J; DeMirci, Hasan; Elser, Veit; Fromme, Petra; Hajdu, Janos; Hantke, Max F; Higashiura, Akifumi; Hogue, Brenda G; Hosseinizadeh, Ahmad; Kim, Yoonhee; Kirian, Richard A; Reddy, Hemanth K N; Lan, Ti-Yen; Larsson, Daniel S D; Liu, Haiguang; Loh, N Duane; Maia, Filipe R N C; Mancuso, Adrian P; Mühlig, Kerstin; Nakagawa, Atsushi; Nam, Daewoong; Nelson, Garrett; Nettelblad, Carl; Okamoto, Kenta; Ourmazd, Abbas; Rose, Max; van der Schot, Gijs; Schwander, Peter; Seibert, M Marvin; Sellberg, Jonas A; Sierra, Raymond G; Song, Changyong; Svenda, Martin; Timneanu, Nicusor; Vartanyants, Ivan A; Westphal, Daniel; Wiedorn, Max O; Williams, Garth J; Xavier, Paulraj Lourdu; Yoon, Chun Hong; Zook, James

2016-08-01

Single particle diffractive imaging data from Rice Dwarf Virus (RDV) were recorded using the Coherent X-ray Imaging (CXI) instrument at the Linac Coherent Light Source (LCLS). RDV was chosen as it is a well-characterized model system, useful for proof-of-principle experiments, system optimization and algorithm development. RDV, an icosahedral virus of about 70 nm in diameter, was aerosolized and injected into the approximately 0.1 μm diameter focused hard X-ray beam at the CXI instrument of LCLS. Diffraction patterns from RDV with signal to 5.9 Ångström were recorded. The diffraction data are available through the Coherent X-ray Imaging Data Bank (CXIDB) as a resource for algorithm development, the contents of which are described here.

Time-spliced X-ray diffraction imaging of magnetism dynamics in a NdNiO3 thin film.

PubMed

Beyerlein, Kenneth R

2018-02-27

Diffraction imaging of nonequilibrium dynamics at atomic resolution is becoming possible with X-ray free-electron lasers. However, there are unresolved problems with applying this method to objects that are confined in only one dimension. Here I show that reliable one-dimensional coherent diffraction imaging is possible by splicing together images recovered from different time delays in an optical pump X-ray probe experiment. The time and space evolution of antiferromagnetic order in a vibrationally excited complex oxide heterostructure is recovered from time-resolved measurements of a resonant soft X-ray diffraction peak. Midinfrared excitation of the substrate is shown to lead to a demagnetization front that propagates at a velocity exceeding the speed of sound, a critical observation for the understanding of driven phase transitions in complex condensed matter.

Preliminary small-angle X-ray scattering and X-ray diffraction studies of the BTB domain of lola protein from Drosophila melanogaster

NASA Astrophysics Data System (ADS)

Boyko, K. M.; Nikolaeva, A. Yu.; Kachalova, G. S.; Bonchuk, A. N.; Dorovatovskii, P. V.; Popov, V. O.

2017-11-01

The Drosophila genome has several dozens of transcription factors (TTK group) containing BTB domains assembled into octamers. The LOLA protein belongs to this family. The purification, crystallization, and preliminary X-ray diffraction and small-angle X-ray scattering (SAXS) studies of the BTB domain of this protein are reported. The crystallization conditions were found by the vapor-diffusion technique. A very low diffraction resolution (8.7 Å resolution) of the crystals was insufficient for the determination of the threedimensional structure of the BTB domain. The SAXS study demonstrated that the BTB domain of the LOLA protein exists as an octamer in solution.

Synchrotron X-ray powder diffraction data of LASSBio-1515: A new N-acylhydrazone derivative compound

NASA Astrophysics Data System (ADS)

Costa, F. N.; Braz, D.; Ferreira, F. F.; da Silva, T. F.; Barreiro, E. J.; Lima, L. M.; Colaço, M. V.; Kuplich, L.; Barroso, R. C.

2014-02-01

In this work, synchrotron X-ray powder diffraction data allowed for a successful indexing of LASSBio-1515 compound, candidate to analgesic and anti-inflammatory activity. X-ray powder diffraction data collected in transmission and high-throughput geometries were used to analyze this compound. The X-ray wavelength of the synchrotron radiation used in this study was determined to be λ=1.55054 Å. LASSBio-1515 was found to be monoclinic with space group P21/c and unit cell parameters a=11.26255(16) Å, b=12.59785(16) Å, c=8.8540(1) Å, β=90.5972(7)° and V=1256.17(3) Å3.

High-speed classification of coherent X-ray diffraction patterns on the K computer for high-resolution single biomolecule imaging.

PubMed

Tokuhisa, Atsushi; Arai, Junya; Joti, Yasumasa; Ohno, Yoshiyuki; Kameyama, Toyohisa; Yamamoto, Keiji; Hatanaka, Masayuki; Gerofi, Balazs; Shimada, Akio; Kurokawa, Motoyoshi; Shoji, Fumiyoshi; Okada, Kensuke; Sugimoto, Takashi; Yamaga, Mitsuhiro; Tanaka, Ryotaro; Yokokawa, Mitsuo; Hori, Atsushi; Ishikawa, Yutaka; Hatsui, Takaki; Go, Nobuhiro

2013-11-01

Single-particle coherent X-ray diffraction imaging using an X-ray free-electron laser has the potential to reveal the three-dimensional structure of a biological supra-molecule at sub-nanometer resolution. In order to realise this method, it is necessary to analyze as many as 1 × 10(6) noisy X-ray diffraction patterns, each for an unknown random target orientation. To cope with the severe quantum noise, patterns need to be classified according to their similarities and average similar patterns to improve the signal-to-noise ratio. A high-speed scalable scheme has been developed to carry out classification on the K computer, a 10PFLOPS supercomputer at RIKEN Advanced Institute for Computational Science. It is designed to work on the real-time basis with the experimental diffraction pattern collection at the X-ray free-electron laser facility SACLA so that the result of classification can be feedback for optimizing experimental parameters during the experiment. The present status of our effort developing the system and also a result of application to a set of simulated diffraction patterns is reported. About 1 × 10(6) diffraction patterns were successfully classificatied by running 255 separate 1 h jobs in 385-node mode.

High-speed classification of coherent X-ray diffraction patterns on the K computer for high-resolution single biomolecule imaging

PubMed Central

Tokuhisa, Atsushi; Arai, Junya; Joti, Yasumasa; Ohno, Yoshiyuki; Kameyama, Toyohisa; Yamamoto, Keiji; Hatanaka, Masayuki; Gerofi, Balazs; Shimada, Akio; Kurokawa, Motoyoshi; Shoji, Fumiyoshi; Okada, Kensuke; Sugimoto, Takashi; Yamaga, Mitsuhiro; Tanaka, Ryotaro; Yokokawa, Mitsuo; Hori, Atsushi; Ishikawa, Yutaka; Hatsui, Takaki; Go, Nobuhiro

2013-01-01

Single-particle coherent X-ray diffraction imaging using an X-ray free-electron laser has the potential to reveal the three-dimensional structure of a biological supra-molecule at sub-nanometer resolution. In order to realise this method, it is necessary to analyze as many as 1 × 106 noisy X-ray diffraction patterns, each for an unknown random target orientation. To cope with the severe quantum noise, patterns need to be classified according to their similarities and average similar patterns to improve the signal-to-noise ratio. A high-speed scalable scheme has been developed to carry out classification on the K computer, a 10PFLOPS supercomputer at RIKEN Advanced Institute for Computational Science. It is designed to work on the real-time basis with the experimental diffraction pattern collection at the X-ray free-electron laser facility SACLA so that the result of classification can be feedback for optimizing experimental parameters during the experiment. The present status of our effort developing the system and also a result of application to a set of simulated diffraction patterns is reported. About 1 × 106 diffraction patterns were successfully classificatied by running 255 separate 1 h jobs in 385-node mode. PMID:24121336

Elucidating the Wavelength Dependence of Phonon Scattering in Nanoparticle-Matrix Composites using Phonon Spectroscopy

DTIC Science & Technology

2016-07-11

composites with x - ray diffraction (XRD), transmission electron microscopy (TEM), scanning electron microscopy (SEM), Rutherford backscattering spectroscopy...RBS), particle-induced x - ray emission (PIXE), and energy dispersive x - ray spectroscopy (EDX). This work complements earlier works on CdSe...sample shows only In2Se3 and CdIn2Se4 XRD peaks (Figure 1.4e), it is stoichiometrically   Figure 1.4. X - ray diffraction patterns of (a) γ-In2Se3

Applications of High Throughput (Combinatorial) Methodologies to Electronic, Magnetic, Optical, and Energy-Related Materials

DTIC Science & Technology

2013-06-17

of the films without having to fabricate capacitors. In addition, the use of X - ray diffraction (XRD) analysis enabled Chikyow et al.40 to identify an...effects of Al doping and annealing on the thermal stabil- ity of the Y2O3/Si gate stack were studied by X - ray photoemission spectroscopy (XPS) and X - ray ...the major diffraction features in the phase distribution. For a given structural phase, the X - ray peak intensity allows one to track the compositional

Aplanatic and quasi-aplanatic diffraction gratings

DOEpatents

Hettrick, M.C.

1987-09-14

A reflection diffraction grating having a series of transverse minute grooves of progressively varying spacing along a concave surface enables use of such gratings for x-ray or longer wavelength imaging of objects. The variable groove spacing establishes aplanatism or substantially uniform magnetification across the optical aperture. The grating may be sued, for example, in x-ray microscopes or telescopes of the imaging type and in x-ray microprobed. Increased spatial resolution and field of view may be realized in x-ray imaging. 5 figs.

An instrument for in situ coherent x-ray studies of metal-organic vapor phase epitaxy of III-nitrides

DOE PAGES

Ju, Guangxu; Highland, Matthew J.; Yanguas-Gil, Angel; ...

2017-03-21

Here, we describe an instrument that exploits the ongoing revolution in synchrotron sources, optics, and detectors to enable in situ studies of metal-organic vapor phase epitaxy (MOVPE) growth of III-nitride materials using coherent x-ray methods. The system includes high-resolution positioning of the sample and detector including full rotations, an x-ray transparent chamber wall for incident and diffracted beam access over a wide angular range, and minimal thermal sample motion, giving the sub-micron positional stability and reproducibility needed for coherent x-ray studies. The instrument enables surface x-ray photon correlation spectroscopy, microbeam diffraction, and coherent diffraction imaging of atomic-scale surface and filmmore » structure and dynamics during growth, to provide fundamental understanding of MOVPE processes.« less

Towards shot-noise limited diffraction experiments with table-top femtosecond hard x-ray sources.

PubMed

Holtz, Marcel; Hauf, Christoph; Weisshaupt, Jannick; Salvador, Antonio-Andres Hernandez; Woerner, Michael; Elsaesser, Thomas

2017-09-01

Table-top laser-driven hard x-ray sources with kilohertz repetition rates are an attractive alternative to large-scale accelerator-based systems and have found widespread applications in x-ray studies of ultrafast structural dynamics. Hard x-ray pulses of 100 fs duration have been generated at the Cu K α wavelength with a photon flux of up to 10 9 photons per pulse into the full solid angle, perfectly synchronized to the sub-100-fs optical pulses from the driving laser system. Based on spontaneous x-ray emission, such sources display a particular noise behavior which impacts the sensitivity of x-ray diffraction experiments. We present a detailed analysis of the photon statistics and temporal fluctuations of the x-ray flux, together with experimental strategies to optimize the sensitivity of optical pump/x-ray probe experiments. We demonstrate measurements close to the shot-noise limit of the x-ray source.

Towards shot-noise limited diffraction experiments with table-top femtosecond hard x-ray sources

PubMed Central

Holtz, Marcel; Hauf, Christoph; Weisshaupt, Jannick; Salvador, Antonio-Andres Hernandez; Woerner, Michael; Elsaesser, Thomas

2017-01-01

Table-top laser-driven hard x-ray sources with kilohertz repetition rates are an attractive alternative to large-scale accelerator-based systems and have found widespread applications in x-ray studies of ultrafast structural dynamics. Hard x-ray pulses of 100 fs duration have been generated at the Cu Kα wavelength with a photon flux of up to 109 photons per pulse into the full solid angle, perfectly synchronized to the sub-100-fs optical pulses from the driving laser system. Based on spontaneous x-ray emission, such sources display a particular noise behavior which impacts the sensitivity of x-ray diffraction experiments. We present a detailed analysis of the photon statistics and temporal fluctuations of the x-ray flux, together with experimental strategies to optimize the sensitivity of optical pump/x-ray probe experiments. We demonstrate measurements close to the shot-noise limit of the x-ray source. PMID:28795079

Synthesis of Novel Extended Phases of Molecular Solids at High Pressures and Temperatures

DOE Office of Scientific and Technical Information (OSTI.GOV)

Yoo, C; Evans, W; Cynn, H

2004-03-30

This study is for in-situ investigation of chemical bonding and molecular structure of low z-elements and simple molecular solids at high pressures and temperatures using 3rd-generation synchrotron x-ray diffraction. To understand the contribution of the empty d-electron orbital of Mg in relation to the formation of molecular solids like MgO, which is one of the important Earth lower mantle materials and MgB{sub 2}, which has recently been the focus of intense superconducting material research, we have performed double-sided laser heating experiments using a diamond anvil cell (DAC). Understanding the structural stability and the formation of the above Mg-compounds requires studyingmore » Mg itself as well as the relevant compounds. BL10XU at the Spring-8 was used to study phase stability and make accurate equation of state (EOS) determinations of Mg coupled with external heating and the double-sided laser heating technique. Monochromatic x-ray at 30 keV (0.4135 {angstrom}) was focused to about 40 {micro}m at the sample and the diffracted x-ray were recorded using a high-resolution image plate (3000 x 3000 pixels with a 0.1 mm resolution per pixel). EOS parameters for hcp and bcc Mg were determined by fitting to a Birch-Murnaghan equation. An isothermal compression of Mg at 300 K up to 100 GPa provides EOS parameters (B{sub 0}, B{sub 0}{prime}, and V{sub 0}) comparable for both hcp and bcc phases, which is similar to the cases for hcp and fcc phases measured in cobalt and xenon. Similar EOS parameters for both low and high pressure phases with a very small or no measurable volume discontinuity at the phase transition pressure suggests that the hcp-bcc structural transition of Mg may be driven by a stacking fault due to a shear instability as seen in xenon and cobalt. Compared to the recent estimation determined using a large volume press [1], our B{sub 0} is smaller by more than 10% suggesting that the difference may be due to non-hydrostatic conditions. The phase boundary of Mg up to 650 K was determined using external resistive heating in air. The results show a noticeable hysteresis during forward and backward transitions. The initial negative slope of the phase boundary agrees very well with the value predicted by theory[2]. Double-side laser heating at several pressures below 20 GPa with simultaneous in-situ x-ray diffraction indicates that hcp is the dominant stable phase and a double hexagonal close packed structure (dhcp) is not seen at high temperatures and high pressures, unlike the observations of recent studies of Mg using a large volume press, claiming dhcp below 20 GPa between 1350 and 1050 K. We suggest that the dhcp may appear as nonequilibrium phase induced by shear stress.« less

X-ray shearing interferometer

DOEpatents

Koch, Jeffrey A [Livermore, CA

2003-07-08

An x-ray interferometer for analyzing high density plasmas and optically opaque materials includes a point-like x-ray source for providing a broadband x-ray source. The x-rays are directed through a target material and then are reflected by a high-quality ellipsoidally-bent imaging crystal to a diffraction grating disposed at 1.times. magnification. A spherically-bent imaging crystal is employed when the x-rays that are incident on the crystal surface are normal to that surface. The diffraction grating produces multiple beams which interfere with one another to produce an interference pattern which contains information about the target. A detector is disposed at the position of the image of the target produced by the interfering beams.

DOE Office of Scientific and Technical Information (OSTI.GOV)

Groenen, Rik; Smit, Jasper; Orsel, Kasper

The oxidation of species in the plasma plume during pulsed laser deposition controls both the stoichiometry as well as the growth kinetics of the deposited SrTiO{sub 3} thin films, instead of the commonly assumed mass distribution in the plasma plume and the kinetic energy of the arriving species. It was observed by X-ray diffraction that SrTiO{sub 3} stoichiometry depends on the composition of the background gas during deposition, where in a relative small pressure range between 10{sup −2} mbars and 10{sup −1} mbars oxygen partial pressure, the resulting film becomes fully stoichiometric. Furthermore, upon increasing the oxygen (partial) pressure, themore » growth mode changes from 3D island growth to a 2D layer-by-layer growth mode as observed by reflection high energy electron diffraction.« less

Pressure-induced amorphization and collapse of magnetic order in the type-I clathrate Eu8Ga16Ge30

NASA Astrophysics Data System (ADS)

Mardegan, J. R. L.; Fabbris, G.; Veiga, L. S. I.; Adriano, C.; Avila, M. A.; Haskel, D.; Giles, C.

2013-10-01

We investigate the low temperature structural and electronic properties of the type-I clathrate Eu8Ga16Ge30 under pressure using x-ray powder diffraction (XRD), x-ray absorption near-edge structure (XANES), and x-ray magnetic circular dichroism (XMCD) techniques. The XRD measurements reveal a transition to an amorphous phase above 18 GPa. Unlike previous reports on other clathrate compounds, no volume collapse is observed prior to the crystalline-amorphous phase transition which takes place when the unit cell volume is reduced to 81% of its ambient pressure value. Fits of the pressure-dependent relative volume to a Murnaghan equation of state yield a bulk modulus B0=65±3 GPa and a pressure derivative B0'=3.3±0.5. The Eu L2-edge XMCD data shows quenching of the magnetic order at a pressure coincident with the crystalline-amorphous phase transition. This information along with the persistence of an Eu2+ valence state observed in the XANES spectra up to the highest pressure point (22 GPa) indicates that the suppression of XMCD intensity is due to the loss of long range magnetic order. When compared with other clathrates, the results point to the importance of guest ion-cage interactions in determining the mechanical stability of the framework structure and the critical pressure for amorphization. Finally, the crystalline structure is not found to recover after pressure release, resulting in an amorphous material that is at least metastable at ambient pressure and temperature.

Symposium N: Materials and Devices for Thermal-to-Electric Energy Conversion

DTIC Science & Technology

2010-08-24

X - ray diffraction, transmission electron microscopy, scanning electron microscopy, and dynamic light scattering. Thermal conductivity measurements...SEM), X - ray diffraction (XRD) measurements as well as Raman spectroscopy. The results from these techniques indicate a clear modification...was examined by using scanning electron microscope (SEM; HITACHI S-4500 model) attached with an energy dispersive x - ray spectroscopy. The electrical

A high-pressure van der Waals compound in solid nitrogen-helium mixtures

NASA Technical Reports Server (NTRS)

Vos, W. L.; Finger, L. W.; Hemley, R. J.; Hu, J. Z.; Mao, H. K.; Schouten, J. A.

1992-01-01

A detailed diamond anvil-cell study using synchrotron X-ray diffraction, Raman scattering, and optical microscopy has been conducted for the He-N system, with a view to the weakly-bound van der Waals molecule interactions that can be formed in the gas phase. High pressure is found to stabilize the formation of a stoichiometric, solid van der Waals compound of He(N2)11 composition which may exemplify a novel class of compounds found at high pressures in the interiors of the outer planets and their satellites.

High pressure phase transitions and compressibilities of Er2Zr2O7 and Ho2Zr2O7

NASA Astrophysics Data System (ADS)

Zhang, F. X.; Lang, M.; Becker, U.; Ewing, R. C.; Lian, J.

2008-01-01

Phase stability and compressibility of rare earth zirconates with the defect-fluorite structure were investigated by in situ synchrotron x-ray diffraction. A sluggish defect-fluorite to a cotunnitelike phase transformation occurred at pressures of ˜22 and ˜30GPa for Er2Zr2O7 and Ho2Zr2O7, respectively. Enhanced compressibility was found for the high pressure phase as a result of increasing cation coordination number and cation-anion bond length.

Kinetics and mechanism of the pressure-induced lamellar order/disorder transition in phosphatidylethanolamine: a time-resolved X-ray diffraction study.

PubMed

Mencke, A P; Caffrey, M

1991-03-05

By using synchrotron radiation, a movie was made of the X-ray scattering pattern from a biological liquid crystal undergoing a phase transition induced by a pressure jump. The system studied includes the fully hydrated phospholipid dihexadecylphosphatidylethanolamine in the lamellar gel (L beta') phase at a temperature of 68 degrees C and a pressure of 9.7 MPa (1400 psig). Following the rapid release of pressure to atmospheric the L beta' phase transforms slowly into the lamellar liquid crystal (L alpha) phase. The pressure perturbation is applied with the intention of producing a sudden phase disequilibrium followed by monitoring the system as it relaxes to its new equilibrium condition. Remarkably, the proportion of sample in the L alpha phase grows linearly with time, taking 37 s to totally consume the L beta' phase. The time dependencies of radius, peak intensity, and width of the powder diffraction ring of the low-angle (001) lamellar reflections were obtained from the movie by image processing. The concept of an "effective pressure" is introduced to account for the temperature variations that accompany the phase transition and to establish that the observed large transit time is indeed intrinsic to the sample and not due to heat exchange with the environment. The reverse transformation, L alpha to L beta', induced by a sudden jump from atmospheric pressure to 9.7 MPa, is complete in less than 13 s. These measurements represent a new approach for studying the kinetics of lipid phase transitions and for gaining insights into the mechanism of the lamellar order/disorder transition.

Lattice preferred orientation in MnGeO3 post-perovskite at high-temperature

NASA Astrophysics Data System (ADS)

Nagaya, Y.; Hirose, K.; Sata, N.; Ohishi, Y.

2009-12-01

In the Earth’s lowermost mantle which is called D” layer, shear-wave splitting is often observed. The velocity of horizontally polarized S-waves are faster than polarized S-waves in many areas of the D” layer. The D” layer is now recognized as being made up with the post-perovskite (PPv)-type MgSiO3 phase. MgSiO3 PPv has a strong elastic anisotropy because of its layered crystal structure. Therefore, it is expected that a lattice preferred orientation (LPO) of PPv may explain the observed seismic anisotropy. LPOs of PPv have been investigated by the high-pressure experiments using a diamond anvil cell (DAC) (Merkel et al., 2006; 2007; Okada et al., 2009). However, the reported experiments using the DAC were made only at the room temperature. In order to understand the nature of PPv deformation under the lower mantle conditions, it is necessary to operate the deformation experiments at high-temperature (~2500 K). In this study, so as to examine the LPO and the dominant slip plane of PPv at simultaneously high P-T conditions, we conducted the high-temperature plastic deformation experiments in a laser-heated diamond anvil cell (LHDAC) using synchrotron radial X-ray diffraction techniques at the beamline BL10XU, SPring-8. In the radial X-ray diffraction experiments, X-ray was irradiated to the sample perpendicular to the compression axis through gasket. LPO was investigated on the basis of the variations of diffraction intensity. We adopted a cubic boron nitride and beryllium composite gasket to obtain a radial X-ray diffraction pattern. In order to deform a sample at high temperature, we had newly developed a membrane system for the deformation experiments. We are able to regulate the gas pressure in the membrane of the DAC, and therefore compress the sample at high temperature during the laser heating. Starting material was orthopyroxene (OPx) with a composition of MnGeO3, which is an analogue of MgSiO3. First, MnGeO3 PPv was synthesized directly from OPx around 60 GPa in the LHDAC. Subsequently, PPv was plastically deformed by further compression at high-temperature during the laser heating. We also conducted the room-temperature deformation experiments. We will discuss the deformation mechanism of the PPv at high P-T conditions.

In situ electrochemical high-energy X-ray diffraction using a capillary working electrode cell geometry

DOE Office of Scientific and Technical Information (OSTI.GOV)

Young, Matthias J.; Bedford, Nicholas M.; Jiang, Naisheng

The ability to generate new electrochemically active materials for energy generation and storage with improved properties will likely be derived from an understanding of atomic-scale structure/function relationships during electrochemical events. Here, the design and implementation of a new capillary electrochemical cell designed specifically forin situhigh-energy X-ray diffraction measurements is described. By increasing the amount of electrochemically active material in the X-ray path while implementing low-Zcell materials with anisotropic scattering profiles, an order of magnitude enhancement in diffracted X-ray signal over traditional cell geometries for multiple electrochemically active materials is demonstrated. This signal improvement is crucial for high-energy X-ray diffraction measurementsmore » and subsequent Fourier transformation into atomic pair distribution functions for atomic-scale structural analysis. As an example, clear structural changes in LiCoO 2under reductive and oxidative conditions using the capillary cell are demonstrated, which agree with prior studies. Accurate modeling of the LiCoO 2diffraction data using reverse Monte Carlo simulations further verifies accurate background subtraction and strong signal from the electrochemically active material, enabled by the capillary working electrode geometry.« less

In Situ 3D Coherent X-ray Diffraction Imaging of Shock Experiments: Possible?

NASA Astrophysics Data System (ADS)

Barber, John

2011-03-01

In traditional coherent X-ray diffraction imaging (CXDI), a 2D or quasi-2D object is illuminated by a beam of coherent X-rays to produce a diffraction pattern, which is then manipulated via a process known as iterative phase retrieval to reconstruct an image of the original 2D sample. Recently, there have been dramatic advances in methods for performing fully 3D CXDI of a sample from a single diffraction pattern [Raines et al, Nature 463 214-7 (2010)], and these methods have been used to image samples tens of microns in size using soft X-rays. In this work, I explore the theoretical possibility of applying 3D CXDI techniques to the in situ imaging of the interaction between a shock front and a polycrystal, a far more stringent problem. A delicate trade-off is required between photon energy, spot size, imaging resolution, and the dimensions of the experimental setup. In this talk, I will outline the experimental and computational requirements for performing such an experiment, and I will present images and movies from simulations of one such hypothetical experiment, including both the time-resolved X-ray diffraction patterns and the time-resolved sample imagery.

High spatial resolution X-ray and gamma ray imaging system using diffraction crystals

DOEpatents

Smither, Robert K [Hinsdale, IL

2011-05-17

A method and a device for high spatial resolution imaging of a plurality of sources of x-ray and gamma-ray radiation are provided. The device comprises a plurality of arrays, with each array comprising a plurality of elements comprising a first collimator, a diffracting crystal, a second collimator, and a detector.

New Developments at the ALS High-Pressure Beamline 12.2.2

NASA Astrophysics Data System (ADS)

Kunz, M.; MacDowell, A. A.; Yan, J.; Beavers, C. C. G.; Doran, A.; Williams, Q. C.

2015-12-01

ALS-beamline 12.2.2 celebrated its 10-year anniversary as a beamline collaboratively operated by the ALS and COMPRES. The anniversary coincided with a major rebuild and expansion of its capabilities for in-situ high-pressure and high-temperature X-ray diffraction. A rebuild of the 12.2.2 laser heating table was completed and commissioned in the past year. The new design relies on a vertically positioned small (~1m x 1m) breadboard that is placed perpendicularly to the incident X-ray beam next to the sample stage. Upstream and downstream viewing-, IR-laser and pyrometry-optics are mounted on opposite surfaces of the breadboard. On-line ruby fluorescence optics including a blue diode laser are also mounted on the upstream surface. The much reduced dimensions of the design lead to smaller mechanical lever arms and thus to a significant suppression of vibrations. This was confirmed in the commissioning phase with high-quality optical images (~ 2 μm resolution) as well as a very stable hotspot in DAC samples. A further optimized pyrometry code was cross-calibrated against thermal expansions of Pt and Ta, and was found to agree with those values within experimental uncertainties. Pyrometry relies on imaging the full hot-spot onto a spectrometer and combining the thus obtained average temperature with an intensity map collected at 700 nm to produce a temperature contour map of the entire sample chamber. Besides axial laser heating, double-sided radial laser heating is also being developed and commissioned. The X-ray source of 12.2.2 makes it an ideal station to focus on high-pressure single crystal diffraction. The present set-up operates parasitically with a single rotation axis on the in-situ laser heating powder diffraction sample stage in concert with a fast (15 fps) amorphous silicon/diode array detector. Although this set-up poses limitations with respect to accessible reciprocal space, high pressure single crystal structure solution and refinements of organic compounds incl. anisotropic displacement parameters have been demonstrated. Imminent development plans aim for the installation of a rugged multi-axis diffractometer on its own dedicated end-station in combination with with a compact fast detector on the 2-theta arm. This will be capable of carrying state of the art wide opening angle DAC's (BX90).

Photoluminescence studies on Cd(1-x)Zn(x)S:Mn2+ nanocrystals.

PubMed

Sethi, Ruchi; Kumar, Lokendra; Pandey, A C

2009-09-01

Highly monodispersed, undoped and doped with Mn2+, binary and ternary (CdS, ZnS, Cd(1-x)Zn(x)S) compound semiconductor nanocrystals have been synthesized by co-precipitation method using citric acid as a stabilizer. As prepared sample are characterized by X-ray diffraction, Small angle X-ray scattering, Transmission electron microscope, Optical absorption and Photoluminescence spectroscopy, for their optical and structural properties. X-ray diffraction, Small angle X-ray scattering and Transmission electron microscope results confirm the preparation of monodispersed nanocrystals. Photoluminescence studies show a significant blue shift in the wavelength with an increasing concentration of Zn in alloy nanocrystals.

Observation of sagittal X-ray diffraction by surface acoustic waves in Bragg geometry.

PubMed

Vadilonga, Simone; Zizak, Ivo; Roshchupkin, Dmitry; Evgenii, Emelin; Petsiuk, Andrei; Leitenberger, Wolfram; Erko, Alexei

2017-04-01

X-ray Bragg diffraction in sagittal geometry on a Y-cut langasite crystal (La 3 Ga 5 SiO 14 ) modulated by Λ = 3 µm Rayleigh surface acoustic waves was studied at the BESSY II synchrotron radiation facility. Owing to the crystal lattice modulation by the surface acoustic wave diffraction, satellites appear. Their intensity and angular separation depend on the amplitude and wavelength of the ultrasonic superlattice. Experimental results are compared with the corresponding theoretical model that exploits the kinematical diffraction theory. This experiment shows that the propagation of the surface acoustic waves creates a dynamical diffraction grating on the crystal surface, and this can be used for space-time modulation of an X-ray beam.

Observation of sagittal X-ray diffraction by surface acoustic waves in Bragg geometry1

PubMed Central

Vadilonga, Simone; Zizak, Ivo; Roshchupkin, Dmitry; Evgenii, Emelin; Petsiuk, Andrei; Leitenberger, Wolfram; Erko, Alexei

2017-01-01

X-ray Bragg diffraction in sagittal geometry on a Y-cut langasite crystal (La3Ga5SiO14) modulated by Λ = 3 µm Rayleigh surface acoustic waves was studied at the BESSY II synchrotron radiation facility. Owing to the crystal lattice modulation by the surface acoustic wave diffraction, satellites appear. Their intensity and angular separation depend on the amplitude and wavelength of the ultrasonic superlattice. Experimental results are compared with the corresponding theoretical model that exploits the kinematical diffraction theory. This experiment shows that the propagation of the surface acoustic waves creates a dynamical diffraction grating on the crystal surface, and this can be used for space–time modulation of an X-ray beam. PMID:28381976

Antiferromagnetic interaction between A'-site Mn spins in A-site-ordered perovskite YMn3Al4O12.

PubMed

Tohyama, Takenori; Saito, Takashi; Mizumaki, Masaichiro; Agui, Akane; Shimakawa, Yuichi

2010-03-01

The A-site-ordered perovskite YMn(3)Al(4)O(12) was prepared by high-pressure synthesis. Structural analysis with synchrotron powder X-ray diffraction data and the Mn L-edges X-ray absorption spectrum revealed that the compound has a chemical composition Y(3+)Mn(3+)(3)Al(3+)(4)O(2-)(12) with magnetic Mn(3+) at the A' site and non-magnetic Al(3+) at the B site. An antiferromagnetic interaction between the A'-site Mn(3+) spins is induced by the nearest neighboring Mn-Mn direct exchange interaction and causes an antiferromagnetic transition at 34.3 K.

Method for improving x-ray diffraction determinations of residual stress in nickel-base alloys

DOEpatents

Berman, R.M.; Cohen, I.

1988-04-26

A process for improving the technique of measuring residual stress by x-ray diffraction in pieces of nickel-base alloys is discussed. Part of a predetermined area of the surface of a nickel-base alloy is covered with a dispersion. This exposes the covered and uncovered portions of the surface of the alloy to x-rays by way of an x-ray diffractometry apparatus, making x-ray diffraction determinations of the exposed surface, and measuring the residual stress in the alloy based on these determinations. The dispersion is opaque to x-rays and serves a dual purpose, since it masks off unsatisfactory signals such that only a small portion of the surface is measured, and it supplies an internal standard by providing diffractogram peaks comparable to the peaks of the nickel alloy so that the alloy peaks can be very accurately located regardless of any sources of error external to the sample. 2 figs.

Dynamic x-ray imaging of laser-driven nanoplasmas

NASA Astrophysics Data System (ADS)

Fennel, Thomas

2016-05-01

A major promise of current x-ray science at free electron lasers is the realization of unprecedented imaging capabilities for resolving the structure and ultrafast dynamics of matter with nanometer spatial and femtosecond temporal resolution or even below via single-shot x-ray diffraction. Laser-driven atomic clusters and nanoparticles provide an ideal platform for developing and demonstrating the required technology to extract the ultrafast transient spatiotemporal dynamics from the diffraction images. In this talk, the perspectives and challenges of dynamic x-ray imaging will be discussed using complete self-consistent microscopic electromagnetic simulations of IR pump x-ray probe imaging for the example of clusters. The results of the microscopic particle-in-cell simulations (MicPIC) enable the simulation-assisted reconstruction of corresponding experimental data. This capability is demonstrated by converting recently measured LCLS data into a ultrahigh resolution movie of laser-induced plasma expansion. Finally, routes towards reaching attosecond time resolution in the visualization of complex dynamical processes in matter by x-ray diffraction will be discussed.

Phase transformation of GaAs at high pressures and temperatures

NASA Astrophysics Data System (ADS)

Ono, Shigeaki; Kikegawa, Takumi

2018-02-01

The high-pressure behavior of gallium arsenide, GaAs, has been investigated using an in-situ X-ray powder diffraction technique in a diamond anvil cell combined with a resistance heating method, at pressures and temperatures up to 25 GPa and 1000 K respectively. The pressure-induced phase transition from a zincblende to an orthorhombic (Cmcm) structure was observed. This transition occurred at 17.3 GPa and at room temperature, where a negative temperature dependence for this transition was confirmed. The transition boundary was determined to be P (GPa) = 18.0 - 0.0025 × T (K).