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

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.

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.

Structural hysteresis in dragline spider silks induced by supercontraction: an X-ray fiber micro-diffraction study

DOE PAGES

Sampath, Sujatha; Yarger, Jeffery L.

2014-11-27

Interaction with water causes shrinkage and significant changes in the structure of spider dragline silks, which has been referred to as supercontraction in the literature. Preferred orientation or alignment of protein chains with respect to the fiber axis is extensively changed during this supercontraction process. Synchrotron X-ray micro-fiber diffraction experiments have been performed on Nephila clavipes and Argiope aurantia major and minor ampullate dragline spider fibers in the native dry, contracted (by immersion in water) and restretched (from contracted) states. Changes in the orientation of β-sheet nanocrystallites and the oriented component of the amorphous network have been determined from wide-anglemore » X-ray diffraction patterns. While both the crystalline and amorphous components lose preferred orientation on wetting with water, the nano-crystallites regain their orientation on wet-restretching, whereas the oriented amorphous components only partially regain their orientation. Dragline major ampullate silks in both the species contract more than their minor ampullate silks.« less

Applications of synchrotron μ-XRF to study the distribution of biologically important elements in different environmental matrices: a review.

PubMed

Majumdar, Sanghamitra; Peralta-Videa, Jose R; Castillo-Michel, Hiram; Hong, Jie; Rico, Cyren M; Gardea-Torresdey, Jorge L

2012-11-28

Environmental matrices including soils, sediments, and living organisms are reservoirs of several essential as well as non-essential elements. Accurate qualitative and quantitative information on the distribution and interaction of biologically significant elements is vital to understand the role of these elements in environmental and biological samples. Synchrotron micro-X-ray fluorescence (μ-SXRF) allows in situ mapping of biologically important elements at nanometer to sub-micrometer scale with high sensitivity, negligible sample damage and enable tuning of the incident energy as desired. Beamlines in the synchrotron facilities are rapidly increasing their analytical versatility in terms of focusing optics, detector technologies, incident energy, and sample environment. Although extremely competitive, it is now feasible to find stations offering complimentary techniques like micro-X-ray diffraction (μ-XRD) and micro-X-ray absorption spectroscopy (μ-XAS) that will allow a more complete characterization of complex matrices. This review includes the most recent literature on the emerging applications and challenges of μ-SXRF in studying the distribution of biologically important elements and manufactured nanoparticles in soils, sediments, plants, and microbes. The advantages of using μ-SXRF and complimentary techniques in contrast to conventional techniques used for the respective studies are discussed. Copyright © 2012 Elsevier B.V. All rights reserved.

Single-shot full strain tensor determination with microbeam X-ray Laue diffraction and a two-dimensional energy-dispersive detector.

PubMed

Abboud, A; Kirchlechner, C; Keckes, J; Conka Nurdan, T; Send, S; Micha, J S; Ulrich, O; Hartmann, R; Strüder, L; Pietsch, U

2017-06-01

The full strain and stress tensor determination in a triaxially stressed single crystal using X-ray diffraction requires a series of lattice spacing measurements at different crystal orientations. This can be achieved using a tunable X-ray source. This article reports on a novel experimental procedure for single-shot full strain tensor determination using polychromatic synchrotron radiation with an energy range from 5 to 23 keV. Microbeam X-ray Laue diffraction patterns were collected from a copper micro-bending beam along the central axis (centroid of the cross section). Taking advantage of a two-dimensional energy-dispersive X-ray detector (pnCCD), the position and energy of the collected Laue spots were measured for multiple positions on the sample, allowing the measurement of variations in the local microstructure. At the same time, both the deviatoric and hydrostatic components of the elastic strain and stress tensors were calculated.

Synchrotron applications in wood preservation and deterioration

Treesearch

Barbara L. Illman

2003-01-01

Several non-intrusive synchrotron techniques are being used to detect and study wood decay. The techniques use high intensity synchrotron-generated X-rays to determine the atomic structure of materials with imaging, diffraction, and absorption. Some of the techniques are X-ray absorption near edge structure (XANES), X-ray fluorescence spectroscopy (XFS), X-ray...

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.

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.

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.

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.

Micro-crystallography comes of age

PubMed Central

Smith, Janet L.; Fischetti, Robert F.; Yamamoto, Masaki

2012-01-01

The latest revolution in macromolecular crystallography was incited by the development of dedicated, user friendly, micro-crystallography beamlines. Brilliant X-ray beams of diameter 20 microns or less, now available at most synchrotron sources, enable structure determination from samples that previously were inaccessible. Relative to traditional crystallography, crystals with one or more small dimensions have diffraction patterns with vastly improved signal-to-noise when recorded with an appropriately matched beam size. Structures can be solved from isolated, well diffracting regions within inhomogeneous samples. This review summarizes the technological requirements and approaches to producing micro-beams and how they continue to change the practice of crystallography. PMID:23021872

Quantitative microstructural imaging by scanning Laue x-ray micro- and nanodiffraction

DOE PAGES

Chen, Xian; Dejoie, Catherine; Jiang, Tengfei; ...

2016-06-08

We present that local crystal structure, crystal orientation, and crystal deformation can all be probed by Laue diffraction using a submicron x-ray beam. This technique, employed at a synchrotron facility, is particularly suitable for fast mapping the mechanical and microstructural properties of inhomogeneous multiphase polycrystalline samples, as well as imperfect epitaxial films or crystals. As synchrotron Laue x-ray microdiffraction enters its 20th year of existence and new synchrotron nanoprobe facilities are being built and commissioned around the world, we take the opportunity to overview current capabilities as well as the latest technical developments. Fast data collection provided by state-of-the-art areamore » detectors and fully automated pattern indexing algorithms optimized for speed make it possible to map large portions of a sample with fine step size and obtain quantitative images of its microstructure in near real time. Lastly, we extrapolate how the technique is anticipated to evolve in the near future and its potential emerging applications at a free-electron laser facility.« less

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

Micro-x-ray fluorescence, micro-x-ray absorption spectroscopy, and micro-x-ray diffraction investigation of lead speciation after the addition of different phosphorus amendments to a smelter-contaminated soil.

PubMed

Baker, Lucas R; Pierzynski, Gary M; Hettiarachchi, Ganga M; Scheckel, Kirk G; Newville, Matthew

2014-03-01

The stabilization of Pb on additions of P to contaminated soils and mine spoil materials has been well documented. It is clear from the literature that different P sources result in different efficacies of Pb stabilization in the same contaminated material. We hypothesized that the differences in the efficacy of Pb stabilization in contaminated soils on fluid or granular P amendment addition is due to different P reaction processes in and around fertilizer granules and fluid droplets. We used a combination of several synchrotron-based techniques (i.e., spatially resolved micro-X-ray fluorescence, micro-X-ray absorption near-edge structure spectroscopy, and micro-X-ray diffraction) to speciate Pb at two incubation times in a smelter-contaminated soil on addition of several fluid and granular P amendments. The results indicated that the Pb phosphate mineral plumbogummite was an intermediate phase of pyromorphite formation. Additionally, all fluid and granular P sources were able to induce Pb phosphate formation, but fluid phosphoric acid (PA) was the most effective with time and distance from the treatment. Granular phosphate rock and triple super phosphate (TSP) amendments reacted to generate Pb phosphate minerals, with TSP being more effective at greater distances from the point of application. As a result, PA and TSP were the most effective P amendments at inducing Pb phosphate formation, but caution needs to be exercised when adding large amounts of soluble P to the environment. Copyright © by the American Society of Agronomy, Crop Science Society of America, and Soil Science Society of America, Inc.

Synchrotron X-ray micro-beam studies of ancient Egyptian make-up

NASA Astrophysics Data System (ADS)

Martinetto, P.; Anne, M.; Dooryhée, E.; Drakopoulos, M.; Dubus, M.; Salomon, J.; Simionovici, A.; Walter, Ph.

2001-07-01

Vases full of make-up are most often present in the burial furniture of Egyptian tombs dated from the pharaonic period. The powdered cosmetics made of isolated grains are analysed to identify their trace element signature. From this signature we identify the provenance of the mineral ingredients in the make-up and we observe different impurities in products, which have been demonstrated as synthetic substances by previous works. Focused X-ray micro-beam ( 2×5 μm2) is successively tuned at 11 keV, below the L III absorption edge of Pb, and 31.8 keV for global characterisation of the metal impurities. The fluorescence signal integrated over each single grain is detected against the X-ray micro-diffraction pattern collected in transmission with a bi-dimensional detector. Furthermore, for galena grains rich in Zn, the XANES signal at the K-absorption edge of Zn shows its immediate nearest-neighbour environment.

Observation of divergent-beam X-ray diffraction from a crystal of diamond using synchrotron radiation.

PubMed

Glazer, A M; Collins, S P; Zekria, D; Liu, J; Golshan, M

2004-03-01

In 1947 Kathleen Lonsdale conducted a series of experiments on X-ray diffraction using a divergent beam external to a crystal sample. Unlike the Kossel technique, where divergent X-rays are excited by the presence of fluorescing atoms within the crystal, the use of an external divergent source made it possible to study non-fluorescing crystals. The resulting photographs not only illustrated the complexity of X-ray diffraction from crystals in a truly beautiful way, but also demonstrated unprecedented experimental precision. This long-forgotten work is repeated here using a synchrotron radiation source and, once again, considerable merit is found in Lonsdale's technique. The results of this experiment suggest that, through the use of modern 'third-generation' synchrotron sources, divergent-beam diffraction could soon enjoy a renaissance for high-precision lattice-parameter determination and the study of crystal perfection.

Nuclear waste viewed in a new light; a synchrotron study of uranium encapsulated in grout.

PubMed

Stitt, C A; Hart, M; Harker, N J; Hallam, K R; MacFarlane, J; Banos, A; Paraskevoulakos, C; Butcher, E; Padovani, C; Scott, T B

2015-03-21

How do you characterise the contents of a sealed nuclear waste package without breaking it open? This question is important when the contained corrosion products are potentially reactive with air and radioactive. Synchrotron X-rays have been used to perform micro-scale in-situ observation and characterisation of uranium encapsulated in grout; a simulation for a typical intermediate level waste storage packet. X-ray tomography and X-ray powder diffraction generated both qualitative and quantitative data from a grout-encapsulated uranium sample before, and after, deliberately constrained H2 corrosion. Tomographic reconstructions provided a means of assessing the extent, rates and character of the corrosion reactions by comparing the relative densities between the materials and the volume of reaction products. The oxidation of uranium in grout was found to follow the anoxic U+H2O oxidation regime, and the pore network within the grout was observed to influence the growth of uranium hydride sites across the metal surface. Powder diffraction analysis identified the corrosion products as UO2 and UH3, and permitted measurement of corrosion-induced strain. Together, X-ray tomography and diffraction provide means of accurately determining the types and extent of uranium corrosion occurring, thereby offering a future tool for isolating and studying the reactions occurring in real full-scale waste package systems. Copyright © 2014 Elsevier B.V. All rights reserved.

Light in the darkening on Naica gypsum crystals

NASA Astrophysics Data System (ADS)

Castillo-Sandoval, I.; Fuentes-Cobas, L. E.; Fuentes-Montero, M. E.; Esparza-Ponce, H. E.; Carreno-Márquez, J.; Reyes-Cortes, M.; Montero-Cabrera, M. E.

2015-07-01

Naica mine is located in a semi-desertic region at the central-south of Chihuahua State. The Cave of Swords was discovered in 1910 and the Cave of Crystals 90 years later at Naica mines. It is expected that during the last century the human presence has changed the microclimatic conditions inside the cave, resulting in the deterioration of the crystals and the deposition of impurities on gypsum surfaces. As a contribution to the clarification of the mentioned issues, the present work refers to the use of synchrotron radiation for the identification of phases on these surfaces. All the experiments were performed at the Stanford Synchrotron Radiation Lightsource. Grazing incidence X-ray diffraction (GIXRD) and radiography-aided X-ray diffraction (RAXRD) experiments were performed at beamline 11-3. X-Ray micro-fluorescence (μ-SXRF) and micro-X-ray absorption (μ-XANES) were measured at beamline 2-3. Representative results obtained may be summarized as follows: a) Gypsum, galena, sphalerite, hematite and cuprite at the surface of the gypsum crystals were determined. b) The samples micro-structure is affected by impurities. c) The elemental distributions and correlations (0.6-0.9) of Cu, K, Fe, Mn, Pb, Zn, Ca and S were identified by μ-SXRF. The correlations among elemental contents confirmed the phase identification, with the exception of manganese and potassium due to the amorphous nature of some impurity compounds in these samples. The compounds hematite (Fe2O3), β-MnO2, Mn2O3, MnO and/or MnCO3, PbS, PbCO3 and/or PbSO4, ZnO4, ZnS and/or smithsonite (ZnCO3), CuS + Cu Oxide were identified by XANES. Plausibly, these latter compounds do not form crystalline phases.

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

Micro-crystallography comes of age.

PubMed

Smith, Janet L; Fischetti, Robert F; Yamamoto, Masaki

2012-10-01

The latest revolution in macromolecular crystallography was incited by the development of dedicated, user friendly, micro-crystallography beam lines. Brilliant X-ray beams of diameter 20 μm or less, now available at most synchrotron sources, enable structure determination from samples that previously were inaccessible. Relative to traditional crystallography, crystals with one or more small dimensions have diffraction patterns with vastly improved signal-to-noise when recorded with an appropriately matched beam size. Structures can be solved from isolated, well diffracting regions within inhomogeneous samples. This review summarizes the technological requirements and approaches to producing micro-beams and how they continue to change the practice of crystallography. Copyright © 2012 Elsevier Ltd. All rights reserved.

X-ray diffraction study of nanocrystalline and amorphous structure within major and minor ampullate dragline spider silks

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

Sampath, Sujatha; Isdebski, Thomas; Jenkins, Janelle E.

Synchrotron X-ray micro-diffraction experiments were carried out on Nephila clavipes (NC) and Argiope aurantia (AA) major (MA) and minor ampullate (MiA) fibers that make up dragline spider silk. The diffraction patterns show a semi-crystalline structure with {beta}-poly(L-alanine) nanocrystallites embedded in a partially oriented amorphous matrix. A superlattice reflection 'S' diffraction ring is observed, which corresponds to a crystalline component larger in size and is poorly oriented, when compared to the {beta}-poly(L-alanine) nanocrystallites that are commonly observed in dragline spider silks. Crystallite size, crystallinity and orientation about the fiber axis have been determined from the wide-angle X-ray diffraction (WAXD) patterns. Inmore » both NC and AA, the MiA silks are found to be more highly crystalline, when compared with the corresponding MA silks. Detailed analysis on the amorphous matrix shows considerable differences in the degree of order of the oriented amorphous component between the different silks studied and may play a crucial role in determining the mechanical properties of the silks.« less

Irradiation effects and micro-structural changes in large grain uranium dioxide fuel investigated by micro-beam X-ray diffraction

NASA Astrophysics Data System (ADS)

Mieszczynski, C.; Kuri, G.; Degueldre, C.; Martin, M.; Bertsch, J.; Borca, C. N.; Grolimund, D.; Delafoy, Ch.; Simoni, E.

2014-01-01

Microstructural changes in a set of commercial grade UO2 fuel samples have been investigated using synchrotron based micro-focused X-ray fluorescence (μ-XRF) and X-ray diffraction (μ-XRD) techniques. The results are associated with conventional UO2 materials and relatively larger grain chromia-doped UO2 fuels, irradiated in a commercial light water reactor plant (average burn-up: 40 MW d kg-1). The lattice parameters of UO2 in fresh and irradiated specimens have been measured and compared with theoretical predictions. In the pristine state, the doped fuel has a somewhat smaller lattice parameter than the standard UO2 as a result of chromia doping. Increase in micro-strain and lattice parameter in irradiated materials is highlighted. All irradiated samples behave in a similar manner with UO2 lattice expansion occurring upon irradiation, where any Cr induced effect seems insignificant and accumulated lattice defects prevail. Elastic strain energy densities in the irradiated fuels are also evaluated based on the UO2 crystal lattice strain and non-uniform strain. The μ-XRD patterns further allow the evaluation of the crystalline domain size and sub-grain formation at different locations of the irradiated UO2 pellets.

Grazing incidence synchrotron X-ray diffraction of marbles consolidated with diammonium hydrogen phosphate treatments: non-destructive probing of buried minerals

NASA Astrophysics Data System (ADS)

Possenti, Elena; Colombo, Chiara; Conti, Claudia; Gigli, Lara; Merlini, Marco; Plaisier, Jasper Rikkert; Realini, Marco; Gatta, G. Diego

2018-05-01

Diammonium hydrogen phosphate (DAP)-based consolidating treatments react with carbonatic stones and form calcium phosphates phases, whose composition depends on the availability of free calcium ions. In this work, an innovative non-destructive approach based on grazing incidence X-ray diffraction (GIXRD) with synchrotron radiation (SR) is used to investigate DAP-treated Carrara marble specimens and to study the influence of the substrate composition on the crystallization of calcium phosphate phases. The outcomes indicate that the presence of compositional micro-heterogeneity of Carrara marble favours the formation of specific phases. Dicalcium phosphate dihydrate, a calcium phosphate with a low Ca/P molar ratio, is formed on carbonatic phases with a low Ca amount, such as dolomite grains and Mg-containing veins. Furthermore, this study highlights the potentialities of SR-GIXRD as a powerful non-destructive tool for the diagnostic of Cultural Heritage objects since it allows investigating the conservation history of stone materials and their interaction with the environment.

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

Pink-beam serial crystallography

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

Meents, A.; Wiedorn, M. O.; Srajer, V.

Serial X-ray crystallography allows macromolecular structure determination at both X-ray free electron lasers (XFELs) and, more recently, synchrotron sources. The time resolution for serial synchrotron crystallography experiments has been limited to millisecond timescales with monochromatic beams. The polychromatic, “pink”, beam provides a more than two orders of magnitude increased photon flux and hence allows accessing much shorter timescales in diffraction experiments at synchrotron sources. Here we report the structure determination of two different protein samples by merging pink-beam diffraction patterns from many crystals, each collected with a single 100 ps X-ray pulse exposure per crystal using a setup optimized formore » very low scattering background. In contrast to experiments with monochromatic radiation, data from only 50 crystals were required to obtain complete datasets. The high quality of the diffraction data highlights the potential of this method for studying irreversible reactions at sub-microsecond timescales using high-brightness X-ray facilities.« less

Pink-beam serial crystallography

DOE PAGES

Meents, A.; Wiedorn, M. O.; Srajer, V.; ...

2017-11-03

Serial X-ray crystallography allows macromolecular structure determination at both X-ray free electron lasers (XFELs) and, more recently, synchrotron sources. The time resolution for serial synchrotron crystallography experiments has been limited to millisecond timescales with monochromatic beams. The polychromatic, “pink”, beam provides a more than two orders of magnitude increased photon flux and hence allows accessing much shorter timescales in diffraction experiments at synchrotron sources. Here we report the structure determination of two different protein samples by merging pink-beam diffraction patterns from many crystals, each collected with a single 100 ps X-ray pulse exposure per crystal using a setup optimized formore » very low scattering background. In contrast to experiments with monochromatic radiation, data from only 50 crystals were required to obtain complete datasets. The high quality of the diffraction data highlights the potential of this method for studying irreversible reactions at sub-microsecond timescales using high-brightness X-ray facilities.« less

Applications of X-Ray Micro-Beam for Data Collection.

PubMed

Sanishvili, Ruslan; Fischetti, Robert F

2017-01-01

Micro-diffraction tools for macromolecular crystallography, first developed at the end of 1990s and now an integral part of many synchrotron beamlines, enable some of the experiments which were not feasible just a decade or so ago. These include data collection from very small samples, just a few micrometers in size; from larger, but severely inhomogeneous samples; and from samples which are optically invisible. Improved micro-diffraction tools led to improved signal-to-noise ratio, to mitigation of radiation damage in some cases, and to better-designed diffraction experiments. Small, micron-scale beams can be attained in different ways and knowing the details of the implementation is important in order to design the diffraction experiment properly. Similarly, precision, reproducibility and stability of the goniometry, and caveats of detection systems need to be taken into account. Lastly, to make micro-diffraction widely applicable, the sophistication, robustness, and user-friendliness of these tools are just as important as the technical capabilities.

X-ray and synchrotron methods in studies of cultural heritage sites

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

Koval’chuk, M. V.; Yatsishina, E. B.; Blagov, A. E.

2016-09-15

X-ray and synchrotron methods that are most widely used in studies of cultural heritage objects (including archaeological sites)—X-ray diffraction analysis, X-ray spectroscopy, and visualization techniques— have been considered. The reported examples show high efficiency and informativeness of natural science studies when solving most diverse problems of archaeology, history, the study of art, museology, etc.

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

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.

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

NASA Technical Reports Server (NTRS)

2008-01-01

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

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.

Synchrotron X-ray reciprocal-space mapping, topography and diffraction resolution studies of macromolecular crystal quality.

PubMed

Boggon, T J; Helliwell, J R; Judge, R A; Olczak, A; Siddons, D P; Snell, E H; Stojanoff, V

2000-07-01

A comprehensive study of microgravity and ground-grown chicken egg-white lysozyme crystals is presented using synchrotron X-ray reciprocal-space mapping, topography techniques and diffraction resolution. Microgravity crystals displayed reduced intrinsic mosaicities on average, but no differences in terms of strain over their ground-grown counterparts. Topographic analysis revealed that in the microgravity case the majority of the crystal was contributing to the peak of the reflection at the appropriate Bragg angle. In the ground-control case only a small volume of the crystal contributed to the intensity at the diffraction peak. The techniques prove to be highly complementary, with the reciprocal-space mapping providing a quantitative measure of the crystal mosaicity and strain (or variation in lattice spacing) and the topography providing a qualitative overall assessment of the crystal in terms of its X-ray diffraction properties. Structural data collection was also carried out at the synchrotron.

Synchrotron X-Ray Reciprocal Space Mapping, Topography and Diffraction Resolution Studies of Macromolecular Crystal Quality

NASA Technical Reports Server (NTRS)

Boggon, T. J.; Helliwell, J. R.; Judge, Russell A.; Siddons, D. P.; Snell, Edward H.; Stojanoff, V.

2000-01-01

A comprehensive study of microgravity and ground grown chicken egg white lysozyme crystals is presented using synchrotron X-ray reciprocal space mapping, topography techniques and diffraction resolution. Microgravity crystals displayed, on average, reduced intrinsic mosaicities but no differences in terms of stress over their earth grown counterparts. Topographic analysis revealed that in the microgravity case the majority of the crystal was contributing to the peak of the reflection at the appropriate Bragg angle. In the earth case at the diffraction peak only a small volume of the crystal contributed to the intensity. The techniques prove to be highly complementary with the reciprocal space mapping providing a quantitative measure of the crystal mosaicity and stress (or variation in lattice spacing) and topography providing a qualitative overall assessment of the crystal in terms of its X-ray diffraction properties. Structural data collection was also carried out both at the synchrotron and in the laboratory.

Fracture mechanics by three-dimensional crack-tip synchrotron X-ray microscopy

PubMed Central

Withers, P. J.

2015-01-01

To better understand the relationship between the nucleation and growth of defects and the local stresses and phase changes that cause them, we need both imaging and stress mapping. Here, we explore how this can be achieved by bringing together synchrotron X-ray diffraction and tomographic imaging. Conventionally, these are undertaken on separate synchrotron beamlines; however, instruments capable of both imaging and diffraction are beginning to emerge, such as ID15 at the European Synchrotron Radiation Facility and JEEP at the Diamond Light Source. This review explores the concept of three-dimensional crack-tip X-ray microscopy, bringing them together to probe the crack-tip behaviour under realistic environmental and loading conditions and to extract quantitative fracture mechanics information about the local crack-tip environment. X-ray diffraction provides information about the crack-tip stress field, phase transformations, plastic zone and crack-face tractions and forces. Time-lapse CT, besides providing information about the three-dimensional nature of the crack and its local growth rate, can also provide information as to the activation of extrinsic toughening mechanisms such as crack deflection, crack-tip zone shielding, crack bridging and crack closure. It is shown how crack-tip microscopy allows a quantitative measure of the crack-tip driving force via the stress intensity factor or the crack-tip opening displacement. Finally, further opportunities for synchrotron X-ray microscopy are explored. PMID:25624521

Synchrotron X-ray studies of model SOFC cathodes, part I: Thin film cathodes

DOE PAGES

Chang, Kee-Chul; Ingram, Brian; Ilavsky, Jan; ...

2017-10-14

In this work, we present synchrotron x-ray investigations of thin film La 0.6Sr 0.4Co 0.2Fe 0.8O 3-δ (LSCF) model cathodes for solid oxide fuel cells, grown on electrolyte substrates by pulse laser deposition, in situ during half-cell operations. We observed dynamic segregations of cations, such as Sr and Co, on the surfaces of the film cathodes. The effects of temperature, applied potentials, and capping layers on the segregations were investigated using a surfacesensitive technique of total external reflection x-ray fluorescence. We also studied patterned thin film LSCF cathodes using high-resolution micro-beam diffraction measurements. We find chemical expansion decreases for narrowmore » stripes. This suggests the expansion is dominated by the bulk pathway reactions. Lastly, the chemical expansion vs. the distance from the electrode contact was measured at three temperatures and an oxygen vacancy activation energy was estimated to be ~1.4 eV.« less

Synchrotron X-ray diffraction study of the Ba{sub 1−x}SrSnO{sub 3} solid solution

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

Prodjosantoso, Anti K., E-mail: Prodjosantoso@yahoo.com; Zhou, Qingdi; Kennedy, Brendan J.

At room temperature the sequence of phases with increasing amounts of strontium in the stannate perovskite system Ba{sub 1−x}SrSnO{sub 3} has been established from high resolution synchrotron X-ray powder diffraction. The observed sequence orthorhombic (Pbnm), orthorhombic (Ibmm), tetragonal (I4/mcm), and cubic (Pm3-bar m) is a consequence of the sequential introduction of cooperative tilting of the corner sharing SnO{sub 6} octahedra. The cell volume changes smoothly across the series with no obvious discontinuities associated with the phase transitions. - Graphical abstract: Portions of the synchrotron X-ray diffraction profiles (λ=0.82453 Å) from selected Ba{sub 1−x}Sr{sub x}SnO{sub 3} samples together with the resultsmore » of fitting by the Rietveld method. Highlights: ► Structures of the stannate perovskites Ba{sub 1−x}SrSnO{sub 3} refined from synchrotron XRD. ► The sequence Pm3-bar m→I4/mcm→Ibmm→Pbnm results from tilting of the octahedra. ► The tilting maintains optimal bonding of the cations seen from the BVS analysis.« less

Fixed target matrix for femtosecond time-resolved and in situ serial micro-crystallography

PubMed Central

Mueller, C.; Marx, A.; Epp, S. W.; Zhong, Y.; Kuo, A.; Balo, A. R.; Soman, J.; Schotte, F.; Lemke, H. T.; Owen, R. L.; Pai, E. F.; Pearson, A. R.; Olson, J. S.; Anfinrud, P. A.; Ernst, O. P.; Dwayne Miller, R. J.

2015-01-01

We present a crystallography chip enabling in situ room temperature crystallography at microfocus synchrotron beamlines and X-ray free-electron laser (X-FEL) sources. Compared to other in situ approaches, we observe extremely low background and high diffraction data quality. The chip design is robust and allows fast and efficient loading of thousands of small crystals. The ability to load a large number of protein crystals, at room temperature and with high efficiency, into prescribed positions enables high throughput automated serial crystallography with microfocus synchrotron beamlines. In addition, we demonstrate the application of this chip for femtosecond time-resolved serial crystallography at the Linac Coherent Light Source (LCLS, Menlo Park, California, USA). The chip concept enables multiple images to be acquired from each crystal, allowing differential detection of changes in diffraction intensities in order to obtain high signal-to-noise and fully exploit the time resolution capabilities of XFELs. PMID:26798825

Fixed target matrix for femtosecond time-resolved and in situ serial micro-crystallography.

PubMed

Mueller, C; Marx, A; Epp, S W; Zhong, Y; Kuo, A; Balo, A R; Soman, J; Schotte, F; Lemke, H T; Owen, R L; Pai, E F; Pearson, A R; Olson, J S; Anfinrud, P A; Ernst, O P; Dwayne Miller, R J

2015-09-01

We present a crystallography chip enabling in situ room temperature crystallography at microfocus synchrotron beamlines and X-ray free-electron laser (X-FEL) sources. Compared to other in situ approaches, we observe extremely low background and high diffraction data quality. The chip design is robust and allows fast and efficient loading of thousands of small crystals. The ability to load a large number of protein crystals, at room temperature and with high efficiency, into prescribed positions enables high throughput automated serial crystallography with microfocus synchrotron beamlines. In addition, we demonstrate the application of this chip for femtosecond time-resolved serial crystallography at the Linac Coherent Light Source (LCLS, Menlo Park, California, USA). The chip concept enables multiple images to be acquired from each crystal, allowing differential detection of changes in diffraction intensities in order to obtain high signal-to-noise and fully exploit the time resolution capabilities of XFELs.

Aladdin: Transforming science at SRC

NASA Astrophysics Data System (ADS)

Bisognano, J.; Bissen, M.; Green, M.; Jacobs, K.; Moore, C.; Olson, E.; Severson, M.; Wehlitz, R.

2011-09-01

The Synchrotron Radiation Center (SRC) is dedicated to enabling of innovative research using IR, ultraviolet, and soft X-ray synchrotron radiation. It delivers beam time with high reliability (99%) and continues to improve the Aladdin storage ring complex. A lower emittance tuning has been commissioned to support a microfocus capability. SRC successfully installed an APPLE II undulator providing elliptically polarized light with lattice compensation for flexible scanning. Installation of a new IR beamline at SRC is providing synchrotron chemical imaging with unprecedented structural and chemical information, simultaneously. In addition, SRC has established a strong education and outreach program to bring the knowledge and power of light source science to a wider national community. It is moving forward into the future by developing a new micro focus beamline producing a diffraction-limited focus of about 500 nm at 22 eV, proposing an additional diffraction-limited chemical imaging beamline, and advancing the Wisconsin Free Electron Laser (WiFEL) concept.

Applications of synchrotron radiation to materials science: Diffraction imaging (topography) and microradiography

NASA Technical Reports Server (NTRS)

Kuriyama, Masao

1988-01-01

Synchrotron radiation sources are now available throughout the world. The use of hard X-ray radiation from these sources for materials science is described with emphasis on diffraction imaging for material characterization. With the availability of synchrotron radiation, real-time in situ measurements of dynamic microstructural phenomena have been started. This is a new area where traditional application of X-rays has been superseded. Examples are chosen from limited areas and are by no means exhaustive. The new emerging information will, no doubt, have great impact on materials science and engineering.

Light in the darkening on Naica gypsum crystals

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

Castillo-Sandoval, I.; Fuentes-Cobas, L. E.; Esparza-Ponce, H. E.

2015-07-23

Naica mine is located in a semi-desertic region at the central-south of Chihuahua State. The Cave of Swords was discovered in 1910 and the Cave of Crystals 90 years later at Naica mines. It is expected that during the last century the human presence has changed the microclimatic conditions inside the cave, resulting in the deterioration of the crystals and the deposition of impurities on gypsum surfaces. As a contribution to the clarification of the mentioned issues, the present work refers to the use of synchrotron radiation for the identification of phases on these surfaces. All the experiments were performedmore » at the Stanford Synchrotron Radiation Lightsource. Grazing incidence X-ray diffraction (GIXRD) and radiography-aided X-ray diffraction (RAXRD) experiments were performed at beamline 11-3. X-Ray micro-fluorescence (μ-SXRF) and micro-X-ray absorption (μ-XANES) were measured at beamline 2-3. Representative results obtained may be summarized as follows: a) Gypsum, galena, sphalerite, hematite and cuprite at the surface of the gypsum crystals were determined. b) The samples micro-structure is affected by impurities. c) The elemental distributions and correlations (0.6-0.9) of Cu, K, Fe, Mn, Pb, Zn, Ca and S were identified by μ-SXRF. The correlations among elemental contents confirmed the phase identification, with the exception of manganese and potassium due to the amorphous nature of some impurity compounds in these samples. The compounds hematite (Fe{sub 2}O{sub 3}), β-MnO{sub 2}, Mn{sub 2}O{sub 3}, MnO and/or MnCO{sub 3}, PbS, PbCO{sub 3} and/or PbSO4, ZnO{sub 4}, ZnS and/or smithsonite (ZnCO{sub 3}), CuS + Cu Oxide were identified by XANES. Plausibly, these latter compounds do not form crystalline phases.« less

New Homogeneous Standards by Atomic Layer Deposition for Synchrotron X-ray Fluorescence and Absorption Spectroscopies.

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

Butterworth, A.L.; Becker, N.; Gainsforth, Z.

2012-03-13

Quantification of synchrotron XRF analyses is typically done through comparisons with measurements on the NIST SRM 1832/1833 thin film standards. Unfortunately, these standards are inhomogeneous on small scales at the tens of percent level. We are synthesizing new homogeneous multilayer standards using the Atomic Layer Deposition technique and characterizing them using multiple analytical methods, including ellipsometry, Rutherford Back Scattering at Evans Analytical, Synchrotron X-ray Fluorescence (SXRF) at Advanced Photon Source (APS) Beamline 13-ID, Synchrotron X-ray Absorption Spectroscopy (XAS) at Advanced Light Source (ALS) Beamlines 11.0.2 and 5.3.2.1 and by electron microscopy techniques. Our motivation for developing much-needed cross-calibration of synchrotronmore » techniques is borne from coordinated analyses of particles captured in the aerogel of the NASA Stardust Interstellar Dust Collector (SIDC). The Stardust Interstellar Dust Preliminary Examination (ISPE) team have characterized three sub-nanogram, {approx}1{micro}m-sized fragments considered as candidates to be the first contemporary interstellar dust ever collected, based on their chemistries and trajectories. The candidates were analyzed in small wedges of aerogel in which they were extracted from the larger collector, using high sensitivity, high spatial resolution >3 keV synchrotron x-ray fluorescence spectroscopy (SXRF) and <2 keV synchrotron x-ray transmission microscopy (STXM) during Stardust ISPE. The ISPE synchrotron techniques have complementary capabilities. Hard X-ray SXRF is sensitive to sub-fg mass of elements Z {ge} 20 (calcium) and has a spatial resolution as low as 90nm. X-ray Diffraction data were collected simultaneously with SXRF data. Soft X-ray STXM at ALS beamline 11.0.2 can detect fg-mass of most elements, including cosmochemically important oxygen, magnesium, aluminum and silicon, which are invisible to SXRF in this application. ALS beamline 11.0.2 has spatial resolution better than 25 nm. Limiting factors for Stardust STXM analyses were self-imposed limits of photon dose due to radiation damage concerns, and significant attenuation of <1500 eV X-rays by {approx}80{micro}m thick, {approx}25 mg/cm{sup 3} density silica aerogel capture medium. In practice, the ISPE team characterized the major, light elements using STXM (O, Mg, Al, Si) and the heavier minor and trace elements using SXRF. The two data sets overlapped only with minor Fe and Ni ({approx}1% mass abundance), providing few quantitative cross-checks. New improved standards for cross calibration are essential for consortium-based analyses of Stardust interstellar and cometary particles, IDPs. Indeed, they have far reaching application across the whole synchrotron-based analytical community. We have synthesized three ALD multilayers simultaneously on silicon nitride membranes and silicon and characterized them using RBS (on Si), XRF (on Si{sub 3}N{sub 4}) and STXM/XAS (holey Si{sub 3}N{sub 4}). The systems we have started to work with are Al-Zn-Fe and Y-Mg-Er. We have found these ALD multi-layers to be uniform at {micro}m- to nm scales, and have found excellent consistency between four analytical techniques so far. The ALD films can also be used as a standard for e-beam instruments, eg., TEM EELS or EDX. After some early issues with the consistency of coatings to the back-side of the membrane windows, we are confident to be able to show multi-analytical agreement to within 10%. As the precision improves, we can use the new standards to verify or improve the tabulated cross-sections.« less

Identification of green pigments from fragments of Roman mural paintings of three Roman sites from north of Germania Superior

NASA Astrophysics Data System (ADS)

Debastiani, Rafaela; Simon, Rolf; Goettlicher, Joerg; Heissler, Stefan; Steininger, Ralph; Batchelor, David; Fiederle, Michael; Baumbach, Tilo

2016-10-01

Roman mural green pigment painting fragments from three Roman sites in the north of the Roman province Germania Superior: Koblenz Stadtwald Remstecken (KOSR), Weißenthurm " Am guten Mann" (WEIS) and Mendig Lungenkärchen (MELU), dating from second and third centuries AD were analyzed. The experiments were performed nondestructively using synchrotron-based scanning macro-X-ray fluorescence (SR-MA-XRF), synchrotron-based scanning micro-X-ray fluorescence (SR-μ-XRF), synchrotron-based X-ray diffraction (SR-XRD) and Raman spectroscopy. Correlation between SR-MA-XRF, SR-μ-XRF elemental map distributions and optical images of scanned areas was mainly found for the elements Ca, Fe and K. With XRF, Fe and K were identified correlated with green pigment, but in samples from two sites, Mendig Lungenkärchen and Weißenthurm " Am guten Mann", also Cu was detected in minor concentration. The results of SR-XRD and Raman spectroscopy were limited to one sample from Weißenthurm " Am guten Mann". In this sample, green earth and calcium carbonate were identified by SR-XRD and, additionally, malachite by Raman spectroscopy.

Probing multi-scale mechanical damage in connective tissues using X-ray diffraction.

PubMed

Bianchi, Fabio; Hofmann, Felix; Smith, Andrew J; Thompson, Mark S

2016-11-01

The accumulation of microstructural collagen damage following repetitive loading is linked to painful and debilitating tendon injuries. As a hierarchical, semi-crystalline material, collagen mechanics can be studied using X-ray diffraction. The aim of the study was to describe multi-structural changes in tendon collagen following controlled plastic damage (5% permanent strain). We used small angle X-ray scattering (SAXS) to interrogate the spacing of collagen molecules within a fibril, and wide angle X-ray scattering (WAXS) to measure molecular strains under macroscopic loading. Simultaneous recordings of SAXS and WAXS patterns, together with whole-tissue strain in physiologically hydrated rat-tail tendons were made during increments of in situ tensile loading. Results showed that while tissue level modulus was unchanged, fibril modulus decreased significantly, and molecular modulus significantly increased. Further, analysis of higher order SAXS peaks suggested structural changes in the gap and overlap regions, possibly localising the damage to molecular cross-links. Our results provide new insight into the fundamental damage processes at work in collagenous tissues and point to new directions for their mitigation and repair. This article reports the first in situ loading synchrotron studies on mechanical damage in collagenous tissues. We provide new insight into the nano- and micro-structural mechanisms of damage processes. Pre-damaged tendons showed differential alteration of moduli at macro, micro and nano-scales as measured using X-ray scattering techniques. Detailed analysis of higher order diffraction peaks suggested damage is localised to molecular cross-links. The results are consistent with previous X-ray scattering studies of tendons and also with recent thermal stability studies on damaged material. Detailed understanding of damage mechanisms is essential in the development of new therapies promoting tissue repair. Copyright © 2016 Acta Materialia Inc. Published by Elsevier Ltd. All rights reserved.

Microstructural and micromechanical characterization of IN718 theta shaped specimens built with electron beam melting

DOE PAGES

Cakmak, Ercan; Kirka, Michael M.; Watkins, Thomas R.; ...

2016-02-23

Theta-shaped specimens were additively manufactured out of Inconel 718 powders using an electron beam melting technique, as a model complex load bearing structure. We employed two different build strategies; producing two sets of specimens. Microstructural and micro-mechanical characterizations were performed using electron back-scatter, synchrotron x-ray and in-situ neutron diffraction techniques. In particular, the cross-members of the specimens were the focus of the synchrotron x-ray and in-situ neutron diffraction measurements. The build strategies employed resulted in the formation of distinct microstructures and crystallographic textures, signifying the importance of build-parameter manipulation for microstructural optimization. Large strain anisotropy of the different lattice planesmore » was observed during in-situ loading. Texture was concluded to have a distinct effect upon both the axial and transverse strain responses of the cross-members. In particular, the (200), (220) and (420) transverse lattice strains all showed unexpected overlapping trends in both builds. This was related to the strong {200} textures along the build/loading direction, providing agreement between the experimental and calculated results.« less

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

Solvent minimization induces preferential orientation and crystal clustering in serial micro-crystallography on micro-meshes, in situ plates and on a movable crystal conveyor belt.

PubMed

Soares, Alexei S; Mullen, Jeffrey D; Parekh, Ruchi M; McCarthy, Grace S; Roessler, Christian G; Jackimowicz, Rick; Skinner, John M; Orville, Allen M; Allaire, Marc; Sweet, Robert M

2014-11-01

X-ray diffraction data were obtained at the National Synchrotron Light Source from insulin and lysozyme crystals that were densely deposited on three types of surfaces suitable for serial micro-crystallography: MiTeGen MicroMeshes™, Greiner Bio-One Ltd in situ micro-plates, and a moving kapton crystal conveyor belt that is used to deliver crystals directly into the X-ray beam. 6° wedges of data were taken from ∼100 crystals mounted on each material, and these individual data sets were merged to form nine complete data sets (six from insulin crystals and three from lysozyme crystals). Insulin crystals have a parallelepiped habit with an extended flat face that preferentially aligned with the mounting surfaces, impacting the data collection strategy and the design of the serial crystallography apparatus. Lysozyme crystals had a cuboidal habit and showed no preferential orientation. Preferential orientation occluded regions of reciprocal space when the X-ray beam was incident normal to the data-collection medium surface, requiring a second pass of data collection with the apparatus inclined away from the orthogonal. In addition, crystals measuring less than 20 µm were observed to clump together into clusters of crystals. Clustering required that the X-ray beam be adjusted to match the crystal size to prevent overlapping diffraction patterns. No additional problems were encountered with the serial crystallography strategy of combining small randomly oriented wedges of data from a large number of specimens. High-quality data able to support a realistic molecular replacement solution were readily obtained from both crystal types using all three serial crystallography strategies.

Solvent minimization induces preferential orientation and crystal clustering in serial micro-crystallography on micro-meshes, in situ plates and on a movable crystal conveyor belt

PubMed Central

Soares, Alexei S.; Mullen, Jeffrey D.; Parekh, Ruchi M.; McCarthy, Grace S.; Roessler, Christian G.; Jackimowicz, Rick; Skinner, John M.; Orville, Allen M.; Allaire, Marc; Sweet, Robert M.

2014-01-01

X-ray diffraction data were obtained at the National Synchrotron Light Source from insulin and lysozyme crystals that were densely deposited on three types of surfaces suitable for serial micro-crystallography: MiTeGen MicroMeshes™, Greiner Bio-One Ltd in situ micro-plates, and a moving kapton crystal conveyor belt that is used to deliver crystals directly into the X-ray beam. 6° wedges of data were taken from ∼100 crystals mounted on each material, and these individual data sets were merged to form nine complete data sets (six from insulin crystals and three from lysozyme crystals). Insulin crystals have a parallelepiped habit with an extended flat face that preferentially aligned with the mounting surfaces, impacting the data collection strategy and the design of the serial crystallography apparatus. Lysozyme crystals had a cuboidal habit and showed no preferential orientation. Preferential orientation occluded regions of reciprocal space when the X-ray beam was incident normal to the data-collection medium surface, requiring a second pass of data collection with the apparatus inclined away from the orthogonal. In addition, crystals measuring less than 20 µm were observed to clump together into clusters of crystals. Clustering required that the X-ray beam be adjusted to match the crystal size to prevent overlapping diffraction patterns. No additional problems were encountered with the serial crystallography strategy of combining small randomly oriented wedges of data from a large number of specimens. High-quality data able to support a realistic molecular replacement solution were readily obtained from both crystal types using all three serial crystallography strategies. PMID:25343789

Role of deformation temperature on the evolution and heterogeneity of texture during equal channel angular pressing of magnesium

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

Biswas, Somjeet, E-mail: somjeetbiswas@gmail.com; Department of Materials Engineering, Indian Institute of Science, Bangalore 560012; Laboratory of Excellence on Design of Alloy Metals for low-mAss Structures

Investigations on texture evolution and through-thickness texture heterogeneity during equal channel angular pressing (ECAP) of pure magnesium at 200 °C, 150 °C and room temperature (RT) was carried out by neutron, high energy synchrotron X-ray and electron back-scatter diffraction. Irrespective of the ECAP temperature, a distinctive basal (B) and pyramidal (C{sub 2}) II type of fibers forms. The texture differs in the bottom 1 mm portion, where the B-fiber is shifted ~ 55° due to negative shear attributed to friction. - Highlights: • ECAP of magnesium was carried out at 200 °C, 150 °C and room temperature. • Microstructure andmore » micro-texture evolution was examined using EBSD in FEG–SEM. • Bulk-texture was studied using neutron diffraction and compared with micro-texture. • Through thickness texture heterogeneity was observed by synchrotron radiation. • Changes in these parameters with respect to deformation temperature are discussed.« less

An instrument for in situ time-resolved X-ray imaging and diffraction of laser powder bed fusion additive manufacturing processes

NASA Astrophysics Data System (ADS)

Calta, Nicholas P.; Wang, Jenny; Kiss, Andrew M.; Martin, Aiden A.; Depond, Philip J.; Guss, Gabriel M.; Thampy, Vivek; Fong, Anthony Y.; Weker, Johanna Nelson; Stone, Kevin H.; Tassone, Christopher J.; Kramer, Matthew J.; Toney, Michael F.; Van Buuren, Anthony; Matthews, Manyalibo J.

2018-05-01

In situ X-ray-based measurements of the laser powder bed fusion (LPBF) additive manufacturing process produce unique data for model validation and improved process understanding. Synchrotron X-ray imaging and diffraction provide high resolution, bulk sensitive information with sufficient sampling rates to probe melt pool dynamics as well as phase and microstructure evolution. Here, we describe a laboratory-scale LPBF test bed designed to accommodate diffraction and imaging experiments at a synchrotron X-ray source during LPBF operation. We also present experimental results using Ti-6Al-4V, a widely used aerospace alloy, as a model system. Both imaging and diffraction experiments were carried out at the Stanford Synchrotron Radiation Lightsource. Melt pool dynamics were imaged at frame rates up to 4 kHz with a ˜1.1 μm effective pixel size and revealed the formation of keyhole pores along the melt track due to vapor recoil forces. Diffraction experiments at sampling rates of 1 kHz captured phase evolution and lattice contraction during the rapid cooling present in LPBF within a ˜50 × 100 μm area. We also discuss the utility of these measurements for model validation and process improvement.

An instrument for in situ time-resolved X-ray imaging and diffraction of laser powder bed fusion additive manufacturing processes.

PubMed

Calta, Nicholas P; Wang, Jenny; Kiss, Andrew M; Martin, Aiden A; Depond, Philip J; Guss, Gabriel M; Thampy, Vivek; Fong, Anthony Y; Weker, Johanna Nelson; Stone, Kevin H; Tassone, Christopher J; Kramer, Matthew J; Toney, Michael F; Van Buuren, Anthony; Matthews, Manyalibo J

2018-05-01

In situ X-ray-based measurements of the laser powder bed fusion (LPBF) additive manufacturing process produce unique data for model validation and improved process understanding. Synchrotron X-ray imaging and diffraction provide high resolution, bulk sensitive information with sufficient sampling rates to probe melt pool dynamics as well as phase and microstructure evolution. Here, we describe a laboratory-scale LPBF test bed designed to accommodate diffraction and imaging experiments at a synchrotron X-ray source during LPBF operation. We also present experimental results using Ti-6Al-4V, a widely used aerospace alloy, as a model system. Both imaging and diffraction experiments were carried out at the Stanford Synchrotron Radiation Lightsource. Melt pool dynamics were imaged at frame rates up to 4 kHz with a ∼1.1 μm effective pixel size and revealed the formation of keyhole pores along the melt track due to vapor recoil forces. Diffraction experiments at sampling rates of 1 kHz captured phase evolution and lattice contraction during the rapid cooling present in LPBF within a ∼50 × 100 μm area. We also discuss the utility of these measurements for model validation and process improvement.

An instrument for in situ time-resolved X-ray imaging and diffraction of laser powder bed fusion additive manufacturing processes

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

Calta, Nicholas P.; Wang, Jenny; Kiss, Andrew M.

In situ X-ray-based measurements of the laser powder bed fusion (LPBF) additive manufacturing process produce unique data for model validation and improved process understanding. Synchrotron X-ray imaging and diffraction provide high resolution, bulk sensitive information with sufficient sampling rates to probe melt pool dynamics as well as phase and microstructure evolution. Here, we describe a laboratory-scale LPBF test bed designed to accommodate diffraction and imaging experiments at a synchrotron X-ray source during LPBF operation. We also present experimental results using Ti-6Al-4V, a widely used aerospace alloy, as a model system. Both imaging and diffraction experiments were carried out at themore » Stanford Synchrotron Radiation Lightsource. Melt pool dynamics were imaged at frame rates up to 4 kHz with a ~1.1 μm effective pixel size and revealed the formation of keyhole pores along the melt track due to vapor recoil forces. Diffraction experiments at sampling rates of 1 kHz captured phase evolution and lattice contraction during the rapid cooling present in LPBF within a ~50 × 100 μm area. In conclusion, we also discuss the utility of these measurements for model validation and process improvement.« less

An instrument for in situ time-resolved X-ray imaging and diffraction of laser powder bed fusion additive manufacturing processes

DOE PAGES

Calta, Nicholas P.; Wang, Jenny; Kiss, Andrew M.; ...

2018-05-01

In situ X-ray-based measurements of the laser powder bed fusion (LPBF) additive manufacturing process produce unique data for model validation and improved process understanding. Synchrotron X-ray imaging and diffraction provide high resolution, bulk sensitive information with sufficient sampling rates to probe melt pool dynamics as well as phase and microstructure evolution. Here, we describe a laboratory-scale LPBF test bed designed to accommodate diffraction and imaging experiments at a synchrotron X-ray source during LPBF operation. We also present experimental results using Ti-6Al-4V, a widely used aerospace alloy, as a model system. Both imaging and diffraction experiments were carried out at themore » Stanford Synchrotron Radiation Lightsource. Melt pool dynamics were imaged at frame rates up to 4 kHz with a ~1.1 μm effective pixel size and revealed the formation of keyhole pores along the melt track due to vapor recoil forces. Diffraction experiments at sampling rates of 1 kHz captured phase evolution and lattice contraction during the rapid cooling present in LPBF within a ~50 × 100 μm area. In conclusion, we also discuss the utility of these measurements for model validation and process improvement.« 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.

Bio-metals imaging and speciation in cells using proton and synchrotron radiation X-ray microspectroscopy

PubMed Central

Ortega, Richard; Devès, Guillaume; Carmona, Asunción

2009-01-01

The direct detection of biologically relevant metals in single cells and of their speciation is a challenging task that requires sophisticated analytical developments. The aim of this article is to present the recent achievements in the field of cellular chemical element imaging, and direct speciation analysis, using proton and synchrotron radiation X-ray micro- and nano-analysis. The recent improvements in focusing optics for MeV-accelerated particles and keV X-rays allow application to chemical element analysis in subcellular compartments. The imaging and quantification of trace elements in single cells can be obtained using particle-induced X-ray emission (PIXE). The combination of PIXE with backscattering spectrometry and scanning transmission ion microscopy provides a high accuracy in elemental quantification of cellular organelles. On the other hand, synchrotron radiation X-ray fluorescence provides chemical element imaging with less than 100 nm spatial resolution. Moreover, synchrotron radiation offers the unique capability of spatially resolved chemical speciation using micro-X-ray absorption spectroscopy. The potential of these methods in biomedical investigations will be illustrated with examples of application in the fields of cellular toxicology, and pharmacology, bio-metals and metal-based nano-particles. PMID:19605403

Simultaneous, single-pulse, synchrotron x-ray imaging and diffraction under gas gun loading

DOE PAGES

Fan, D.; Huang, J. W.; Zeng, X. L.; ...

2016-05-23

We develop a mini gas gun system for simultaneous, single-pulse, x-ray diffraction and imaging under high strain-rate loading at the beamline 32-ID of the Advanced Photon Source. In order to increase the reciprocal space covered by a small-area detector, a conventional target chamber is split into two chambers: a narrowed measurement chamber and a relief chamber. The gas gun impact is synchronized with synchrotron x-ray pulses and high-speed cameras. Depending on a camera’s capability, multiframe imaging and diffraction can be achieved. The proof-of-principle experiments are performed on single-crystal sapphire. The diffraction spots and images during impact are analyzed to quantifymore » lattice deformation and fracture; diffraction peak broadening is largely caused by fracture-induced strain inhomogeneity. Finally, our results demonstrate the potential of such multiscale measurements for revealing and understanding high strain-rate phenomena at dynamic extremes.« less

Simultaneous, single-pulse, synchrotron x-ray imaging and diffraction under gas gun loading

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

Fan, D.; Huang, J. W.; Zeng, X. L.

We develop a mini gas gun system for simultaneous, single-pulse, x-ray diffraction and imaging under high strain-rate loading at the beamline 32-ID of the Advanced Photon Source. In order to increase the reciprocal space covered by a small-area detector, a conventional target chamber is split into two chambers: a narrowed measurement chamber and a relief chamber. The gas gun impact is synchronized with synchrotron x-ray pulses and high-speed cameras. Depending on a camera’s capability, multiframe imaging and diffraction can be achieved. The proof-of-principle experiments are performed on single-crystal sapphire. The diffraction spots and images during impact are analyzed to quantifymore » lattice deformation and fracture; diffraction peak broadening is largely caused by fracture-induced strain inhomogeneity. Finally, our results demonstrate the potential of such multiscale measurements for revealing and understanding high strain-rate phenomena at dynamic extremes.« less

CCD sensors in synchrotron X-ray detectors

NASA Astrophysics Data System (ADS)

Strauss, M. G.; Naday, I.; Sherman, I. S.; Kraimer, M. R.; Westbrook, E. M.; Zaluzec, N. J.

1988-04-01

The intense photon flux from advanced synchrotron light sources, such as the 7-GeV synchrotron being designed at Argonne, require integrating-type detectors. Charge-coupled devices (CCDs) are well suited as synchrotron X-ray detectors. When irradiated indirectly via a phosphor followed by reducing optics, diffraction patterns of 100 cm 2 can be imaged on a 2 cm 2 CCD. With a conversion efficiency of ˜ 1 CCD electron/X-ray photon, a peak saturation capacity of > 10 6 X-rays can be obtained. A programmable CCD controller operating at a clock frequency of 20 MHz has been developed. The readout rate is 5 × 10 6 pixels/s and the shift rate in the parallel registers is 10 6 lines/s. The test detector was evaluated in two experiments. In protein crystallography diffraction patterns have been obtained from a lysozyme crystal using a conventional rotating anode X-ray generator. Based on these results we expect to obtain at a synchrotron diffraction images at a rate of ˜ 1 frame/s or a complete 3-dimensional data set from a single crystal in ˜ 2 min. In electron energy-loss spectroscopy (EELS), the CCD was used in a parallel detection mode which is similar to the mode array detectors are used in dispersive EXAFS. With a beam current corresponding to 3 × 10 9 electron/s on the detector, a series of 64 spectra were recorded on the CCD in a continuous sequence without interruption due to readout. The frame-to-frame pixel signal fluctuations had σ = 0.4% from which DQE = 0.4 was obtained, where the detector conversion efficiency was 2.6 CCD electrons/X-ray photon. These multiple frame series also showed the time-resolved modulation of the electron microscope optics by stray magnetic fields.

Advances in indirect detector systems for ultra high-speed hard X-ray imaging with synchrotron light

NASA Astrophysics Data System (ADS)

Olbinado, M. P.; Grenzer, J.; Pradel, P.; De Resseguier, T.; Vagovic, P.; Zdora, M.-C.; Guzenko, V. A.; David, C.; Rack, A.

2018-04-01

We report on indirect X-ray detector systems for various full-field, ultra high-speed X-ray imaging methodologies, such as X-ray phase-contrast radiography, diffraction topography, grating interferometry and speckle-based imaging performed at the hard X-ray imaging beamline ID19 of the European Synchrotron—ESRF. Our work highlights the versatility of indirect X-ray detectors to multiple goals such as single synchrotron pulse isolation, multiple-frame recording up to millions frames per second, high efficiency, and high spatial resolution. Besides the technical advancements, potential applications are briefly introduced and discussed.

A multi-dataset data-collection strategy produces better diffraction data

PubMed Central

Liu, Zhi-Jie; Chen, Lirong; Wu, Dong; Ding, Wei; Zhang, Hua; Zhou, Weihong; Fu, Zheng-Qing; Wang, Bi-Cheng

2011-01-01

A multi-dataset (MDS) data-collection strategy is proposed and analyzed for macromolecular crystal diffraction data acquisition. The theoretical analysis indicated that the MDS strategy can reduce the standard deviation (background noise) of diffraction data compared with the commonly used single-dataset strategy for a fixed X-ray dose. In order to validate the hypothesis experimentally, a data-quality evaluation process, termed a readiness test of the X-ray data-collection system, was developed. The anomalous signals of sulfur atoms in zinc-free insulin crystals were used as the probe to differentiate the quality of data collected using different data-collection strategies. The data-collection results using home-laboratory-based rotating-anode X-ray and synchrotron X-ray systems indicate that the diffraction data collected with the MDS strategy contain more accurate anomalous signals from sulfur atoms than the data collected with a regular data-collection strategy. In addition, the MDS strategy offered more advantages with respect to radiation-damage-sensitive crystals and better usage of rotating-anode as well as synchrotron X-rays. PMID:22011470

New synchrotron powder diffraction facility for long-duration experiments

PubMed Central

Murray, Claire A.; Potter, Jonathan; Day, Sarah J.; Baker, Annabelle R.; Thompson, Stephen P.; Kelly, Jon; Morris, Christopher G.; Tang, Chiu C.

2017-01-01

A new synchrotron X-ray powder diffraction instrument has been built and commissioned for long-duration experiments on beamline I11 at Diamond Light Source. The concept is unique, with design features to house multiple experiments running in parallel, in particular with specific stages for sample environments to study slow kinetic systems or processes. The instrument benefits from a high-brightness X-ray beam and a large area detector. Diffraction data from the commissioning work have shown that the objectives and criteria are met. Supported by two case studies, the results from months of measurements have demonstrated the viability of this large-scale instrument, which is the world’s first dedicated facility for long-term studies (weeks to years) using synchrotron radiation. PMID:28190992

3D Experimental Measurement of Lattice Strain and Fracture Behavior of Sand Particles Using Synchrotron X-Ray Diffraction and Tomography

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

Cil, Mehmet B.; Alshibli, Khalid A.; Kenesei, Peter

3D synchrotron X-ray diffraction (3DXRD) and synchrotron micro-computed tomography (SMT) techniques were used to measure and monitor the lattice strain evolution and fracture behavior of natural Ottawa sand particles subjected to 1D compression loading. The particle-averaged lattice strain within sand particles was measured using 3DXRD and then was used to calculate the corresponding lattice stress tensor. In addition, the evolution and mode of fracture of sand particles was investigated using high-resolution 3D SMT images. The results of diffraction data analyses revealed that the major principal component of the lattice strain or stress tensor increased in most of the particles asmore » the global applied compressive load increased until the onset of fracture. Particle fracture and subsequent rearrangements caused significant variation and fluctuations in measured lattice strain/stress values from one particle to another and from one load step to the next one. SMT image analysis at the particle-scale showed that cracks in fractured sand particles generally initiate and propagate along the plane that connects the two contact points. Fractured particles initially split into two or three major fragments followed by disintegration into multiple smaller fragments in some cases. In conclusion, microscale analysis of fractured particles showed that particle position, morphology, the number and location of contact points play a major role in the occurrence of particle fracture in confined comminution of the sand assembly.« less

3D Experimental Measurement of Lattice Strain and Fracture Behavior of Sand Particles Using Synchrotron X-Ray Diffraction and Tomography

DOE PAGES

Cil, Mehmet B.; Alshibli, Khalid A.; Kenesei, Peter

2017-05-27

3D synchrotron X-ray diffraction (3DXRD) and synchrotron micro-computed tomography (SMT) techniques were used to measure and monitor the lattice strain evolution and fracture behavior of natural Ottawa sand particles subjected to 1D compression loading. The particle-averaged lattice strain within sand particles was measured using 3DXRD and then was used to calculate the corresponding lattice stress tensor. In addition, the evolution and mode of fracture of sand particles was investigated using high-resolution 3D SMT images. The results of diffraction data analyses revealed that the major principal component of the lattice strain or stress tensor increased in most of the particles asmore » the global applied compressive load increased until the onset of fracture. Particle fracture and subsequent rearrangements caused significant variation and fluctuations in measured lattice strain/stress values from one particle to another and from one load step to the next one. SMT image analysis at the particle-scale showed that cracks in fractured sand particles generally initiate and propagate along the plane that connects the two contact points. Fractured particles initially split into two or three major fragments followed by disintegration into multiple smaller fragments in some cases. In conclusion, microscale analysis of fractured particles showed that particle position, morphology, the number and location of contact points play a major role in the occurrence of particle fracture in confined comminution of the sand assembly.« less

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.

Hard and soft X-ray microscopy and tomography in catalysis: bridging the different time and length scales.

PubMed

Grunwaldt, Jan-Dierk; Schroer, Christian G

2010-12-01

X-ray microscopic techniques are excellent and presently emerging techniques for chemical imaging of heterogeneous catalysts. Spatially resolved studies in heterogeneous catalysis require the understanding of both the macro and the microstructure, since both have decisive influence on the final performance of the industrially applied catalysts. A particularly important aspect is the study of the catalysts during their preparation, activation and under operating conditions, where X-rays have an inherent advantage due to their good penetration length especially in the hard X-ray regime. Whereas reaction cell design for hard X-rays is straightforward, recently smart in situ cells have also been reported for the soft X-ray regime. In the first part of the tutorial review, the constraints from a catalysis view are outlined, then the scanning and full-field X-ray microscopy as well as coherent X-ray diffraction imaging techniques are described together with the challenging design of suitable environmental cells. Selected examples demonstrate the application of X-ray microscopy and tomography to monitor structural gradients in catalytic reactors and catalyst preparation with micrometre resolution but also the possibility to follow structural changes in the sub-100 nm regime. Moreover, the potential of the new synchrotron radiation sources with higher brilliance, recent milestones in focusing of hard X-rays as well as spatiotemporal studies are highlighted. The tutorial review concludes with a view on future developments in the field of X-ray microscopy that will have strong impact on the understanding of catalysts in the future and should be combined with in situ electron microscopic studies on the nanoscale and other spectroscopic studies like microRaman, microIR and microUV-vis on the macroscale.

The crystal structure of paramagnetic copper(II) oxalate (CuC₂O₄): formation and thermal decomposition of randomly stacked anisotropic nano-sized crystallites.

PubMed

Christensen, Axel Nørlund; Lebech, Bente; Andersen, Niels Hessel; Grivel, Jean-Claude

2014-11-28

Synthetic copper(II) oxalate, CuC2O4, was obtained in a precipitation reaction between a copper(II) solution and an aqueous solution of oxalic acid. The product was identified from its conventional X-ray powder patterns which match that of the copper mineral Moolooite reported to have the composition CuC2O4·0.44H2O. Time resolved in situ investigations of the thermal decomposition of copper(II) oxalate using synchrotron X-ray powder diffraction showed that in air the compound converts to Cu2O at 215 °C and oxidizes to CuO at 345 °C. Thermo gravimetric analysis performed in an inert Ar-gas reveals that the material contains no crystal water and reduces to pure Cu at 295 °C. Magnetic susceptibility measurements in the temperature range from 2 K to 300 K show intriguing paramagnetic behaviour with no sign of magnetic order down to 2 K. A crystal structure investigation is made based on powder diffraction data using one neutron diffraction pattern obtained at 5 K (λ = 1.5949(1) Å) combined with one conventional and two synchrotron X-ray diffraction patterns obtained at ambient temperature using λ = 1.54056, 1.0981 and λ = 0.50483(1) Å, respectively. Based on the X-ray synchrotron data the resulting crystal structure is described in the monoclinic space group P2₁/c (#14) in the P12₁/n1 setting with unit cell parameters a = 5.9598(1) Å, b = 5.6089(1) Å, c = 5.1138 (1) Å, β = 115.320(1)°. The composition is CuC2O4 with atomic coordinates determined by FullProf refinement of the neutron diffraction data. The crystal structure consists of a random stacking of CuC2O4 micro-crystallites where half the Cu-atoms are placed at (2a) and the other half at (2b) positions with the corresponding oxalate molecules centred around the corresponding (2b) and (2a) site positions, respectively. The diffraction patterns obtained for both kinds of radiation show considerable broadening of several Bragg peaks caused by highly anisotropic microstructural size and strain effects. In contrast to the water reported to be present in Moolooite, neither thermogravimetric nor the in situ thermal decomposition investigations and crystal structure analysis of the neutron diffraction data revealed any trace of water. An appendix contains details about the profile parameters for the diffractometers used at the European Synchrotron Radiation Facility and the Institute Max von Laue-Paul Langevin.

Challenges for Synchrotron X-Ray Optics

NASA Astrophysics Data System (ADS)

Freund, Andreas K.

2002-12-01

It is the task of x-ray optics to adapt the raw beam generated by modern sources such as synchrotron storage rings to a great variety of experimental requirements in terms of intensity, spot size, polarization and other parameters. The very high quality of synchrotron radiation (source size of a few microns and beam divergence of a few micro-radians) and the extreme x-ray flux (power of several hundred Watts in a few square mm) make this task quite difficult. In particular the heat load aspect is very important in the conditioning process of the brute x-ray power to make it suitable for being used on the experimental stations. Cryogenically cooled silicon crystals and water-cooled diamond crystals can presently fulfill this task, but limits will soon be reached and new schemes and materials must be envisioned. A major tendency of instrument improvement has always been to concentrate more photons into a smaller spot utilizing a whole variety of focusing devices such as Fresnel zone plates, refractive lenses and systems based on bent surfaces, for example, Kirkpatrick-Baez systems. Apart from the resistance of the sample, the ultimate limits are determined by the source size and strength on one side, by materials properties, cooling, mounting and bending schemes on the other side, and fundamentally by the diffraction process. There is also the important aspect of coherence that can be both a nuisance and a blessing for the experiments, in particular for imaging techniques. Its conservation puts additional constraints on the quality of the optical elements. The overview of the present challenges includes the properties of present and also mentions aspects of future x-ray sources such as the "ultimate" storage ring and free electron lasers. These challenges range from the thermal performances of monochromators to the surface quality of mirrors, from coherence preservation of modern multilayers to short pulse preservation by crystals, and from micro- and nano-focusing techniques to the accuracy and stability of mechanical supports.

Solvent minimization induces preferential orientation and crystal clustering in serial micro-crystallography on micro-meshes, in situ plates and on a movable crystal conveyor belt

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

Soares, Alexei S.; Mullen, Jeffrey D.; Parekh, Ruchi M.

X-ray diffraction data were obtained at the National Synchrotron Light Source from insulin and lysozyme crystals that were densely deposited on three types of surfaces suitable for serial micro-crystallography: MiTeGen MicroMeshes™, Greiner Bio-One Ltdin situmicro-plates, and a moving kapton crystal conveyor belt that is used to deliver crystals directly into the X-ray beam. 6° wedges of data were taken from ~100 crystals mounted on each material, and these individual data sets were merged to form nine complete data sets (six from insulin crystals and three from lysozyme crystals). Insulin crystals have a parallelepiped habit with an extended flat face thatmore » preferentially aligned with the mounting surfaces, impacting the data collection strategy and the design of the serial crystallography apparatus. Lysozyme crystals had a cuboidal habit and showed no preferential orientation. Preferential orientation occluded regions of reciprocal space when the X-ray beam was incident normal to the data-collection medium surface, requiring a second pass of data collection with the apparatus inclined away from the orthogonal. In addition, crystals measuring less than 20 µm were observed to clump together into clusters of crystals. Clustering required that the X-ray beam be adjusted to match the crystal size to prevent overlapping diffraction patterns. No additional problems were encountered with the serial crystallography strategy of combining small randomly oriented wedges of data from a large number of specimens. Lastly, high-quality data able to support a realistic molecular replacement solution were readily obtained from both crystal types using all three serial crystallography strategies.« less

Solvent minimization induces preferential orientation and crystal clustering in serial micro-crystallography on micro-meshes, in situ plates and on a movable crystal conveyor belt

DOE PAGES

Soares, Alexei S.; Mullen, Jeffrey D.; Parekh, Ruchi M.; ...

2014-10-09

X-ray diffraction data were obtained at the National Synchrotron Light Source from insulin and lysozyme crystals that were densely deposited on three types of surfaces suitable for serial micro-crystallography: MiTeGen MicroMeshes™, Greiner Bio-One Ltdin situmicro-plates, and a moving kapton crystal conveyor belt that is used to deliver crystals directly into the X-ray beam. 6° wedges of data were taken from ~100 crystals mounted on each material, and these individual data sets were merged to form nine complete data sets (six from insulin crystals and three from lysozyme crystals). Insulin crystals have a parallelepiped habit with an extended flat face thatmore » preferentially aligned with the mounting surfaces, impacting the data collection strategy and the design of the serial crystallography apparatus. Lysozyme crystals had a cuboidal habit and showed no preferential orientation. Preferential orientation occluded regions of reciprocal space when the X-ray beam was incident normal to the data-collection medium surface, requiring a second pass of data collection with the apparatus inclined away from the orthogonal. In addition, crystals measuring less than 20 µm were observed to clump together into clusters of crystals. Clustering required that the X-ray beam be adjusted to match the crystal size to prevent overlapping diffraction patterns. No additional problems were encountered with the serial crystallography strategy of combining small randomly oriented wedges of data from a large number of specimens. Lastly, high-quality data able to support a realistic molecular replacement solution were readily obtained from both crystal types using all three serial crystallography strategies.« less

Synchrotron radiation microbeam X-ray diffraction for nondestructive assessments of local structural properties of faceted InGaN/GaN quantum wells

NASA Astrophysics Data System (ADS)

Sakaki, Atsushi; Funato, Mitsuru; Kawamura, Tomoaki; Araki, Jun; Kawakami, Yoichi

2018-03-01

Synchrotron radiation (SR) X-ray diffraction with a sub-µm spatial resolution is used to nondestructively evaluate the local thickness and alloy composition of three-dimensionally faceted InGaN/GaN quantum wells (QWs). The (0001) facet QW on a trapezoidal structure composed of (0001), \\{ 11\\bar{2}2\\} , and \\{ 11\\bar{2}0\\} facets is nonuniform, most likely owing to the migration of adatoms between facets. The thickness and composition markedly vary within a short distance for the \\{ 11\\bar{2}2\\} facet QW of another pyramidal structure. The QW parameters acquired by SR microbeam X-ray diffraction reproduce the local emission property assessed by cathodoluminescence, thereby indicating the high reliability of this method.

Symposium LL: Nanowires--Synthesis Properties Assembly and Application

DTIC Science & Technology

2010-09-10

dedicated hard x - ray microscopy beamline is operated in partnership with the Advanced Photon Source to provide fluorescence, diffraction, and...characterized by scanning electron microscopy (SEM), transmission electron microscopy (TEM) and X - ray diffraction (XRD) measurements, proving it to be...Investigation of Preferred Growth Direction of GaN Nanorods by Synchrotron X - ray Reciprocal Space Mapping. Yuri Sohn1, Sanghwa Lee1, Chinkyo Kim1 and Dong

Fixed target matrix for femtosecond time-resolved and in situ serial micro-crystallography

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

Mueller, C.; Marx, A.; Epp, S. W.

We present a crystallography chip enabling in situ room temperature crystallography at microfocus synchrotron beamlines and X-ray free-electron laser (X-FEL) sources. Compared to other in situ approaches, we observe extremely low background and high diffraction data quality. The chip design is robust and allows fast and efficient loading of thousands of small crystals. The ability to load a large number of protein crystals, at room temperature and with high efficiency, into prescribed positions enables high throughput automated serial crystallography with microfocus synchrotron beamlines. In addition, we demonstrate the application of this chip for femtosecond time-resolved serial crystallography at the Linacmore » Coherent Light Source (LCLS, Menlo Park, California, USA). As a result, the chip concept enables multiple images to be acquired from each crystal, allowing differential detection of changes in diffraction intensities in order to obtain high signal-to-noise and fully exploit the time resolution capabilities of XFELs.« less

Fixed target matrix for femtosecond time-resolved and in situ serial micro-crystallography

DOE PAGES

Mueller, C.; Marx, A.; Epp, S. W.; ...

2015-08-18

We present a crystallography chip enabling in situ room temperature crystallography at microfocus synchrotron beamlines and X-ray free-electron laser (X-FEL) sources. Compared to other in situ approaches, we observe extremely low background and high diffraction data quality. The chip design is robust and allows fast and efficient loading of thousands of small crystals. The ability to load a large number of protein crystals, at room temperature and with high efficiency, into prescribed positions enables high throughput automated serial crystallography with microfocus synchrotron beamlines. In addition, we demonstrate the application of this chip for femtosecond time-resolved serial crystallography at the Linacmore » Coherent Light Source (LCLS, Menlo Park, California, USA). As a result, the chip concept enables multiple images to be acquired from each crystal, allowing differential detection of changes in diffraction intensities in order to obtain high signal-to-noise and fully exploit the time resolution capabilities of XFELs.« less

Insights into metals in individual fine particles from municipal solid waste using synchrotron radiation-based micro-analytical techniques.

PubMed

Zhu, Yumin; Zhang, Hua; Shao, Liming; He, Pinjing

2015-01-01

Excessive inter-contamination with heavy metals hampers the application of biological treatment products derived from mixed or mechanically-sorted municipal solid waste (MSW). In this study, we investigated fine particles of <2mm, which are small fractions in MSW but constitute a significant component of the total heavy metal content, using bulk detection techniques. A total of 17 individual fine particles were evaluated using synchrotron radiation-based micro-X-ray fluorescence and micro-X-ray diffraction. We also discussed the association, speciation and source apportionment of heavy metals. Metals were found to exist in a diffuse distribution with heterogeneous intensities and intense hot-spots of <10 μm within the fine particles. Zn-Cu, Pb-Fe and Fe-Mn-Cr had significant correlations in terms of spatial distribution. The overlapped enrichment, spatial association, and the mineral phases of metals revealed the potential sources of fine particles from size-reduced waste fractions (such as scraps of organic wastes or ceramics) or from the importation of other particles. The diverse sources of heavy metal pollutants within the fine particles suggested that separate collection and treatment of the biodegradable waste fraction (such as food waste) is a preferable means of facilitating the beneficial utilization of the stabilized products. Copyright © 2014. Published by Elsevier B.V.

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.

Anisotropic deformation of extruded magnesium alloy AZ31 under uniaxial compression: A study with simultaneous in situ synchrotron x-ray imaging and diffraction

DOE PAGES

Lu, L.; Huang, J. W.; Fan, D.; ...

2016-08-29

In situ synchrotron x-ray imaging and diffraction are used to investigate anisotropic deformation of an extruded magnesium alloy AZ31 under uniaxial compression along two different directions, with the loading axis (LA) either parallel or perpendicular to the extrusion direction (ED), referred to as LA∥ED and LAED, respectively. Multiscale measurements including stress–strain curves (macroscale), x-ray digital image correlation (mesoscale), and diffraction (microscale) are obtained simultaneously. Electron backscatter diffraction is performed on samples collected at various strains to characterize deformation twins. The rapid increase in strain hardening rate for the LA∥ED loading is attributed to marked {101¯2} extension twinning and subsequent homogenizationmore » of deformation, while dislocation motion leads to inhomogeneous deformation and a decrease in strain hardening rate.« less

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.

Spherical quartz crystals investigated with synchrotron radiation

DOE PAGES

Pereira, N. R.; Macrander, A. T.; Hill, K. W.; ...

2015-10-27

The quality of x-ray spectra and images obtained from plasmas with spherically bent crystals depends in part on the crystal's x-ray diffraction across the entire crystal surface. We employ the energy selectivity and high intensity of synchrotron radiation to examine typical spherical crystals from alpha-quartz for their diffraction quality, in a perpendicular geometry that is particularly convenient to examine sagittal focusing. The crystal's local diffraction is not ideal: the most noticeable problems come from isolated regions that so far have failed to correlate with visible imperfections. In conclusion, excluding diffraction from such problem spots has little effect on the focusmore » beyond a decrease in background.« less

A novel high-temperature furnace for combined in situ synchrotron X-ray diffraction and infrared thermal imaging to investigate the effects of thermal gradients upon the structure of ceramic materials

PubMed Central

Robinson, James B.; Brown, Leon D.; Jervis, Rhodri; Taiwo, Oluwadamilola O.; Millichamp, Jason; Mason, Thomas J.; Neville, Tobias P.; Eastwood, David S.; Reinhard, Christina; Lee, Peter D.; Brett, Daniel J. L.; Shearing, Paul R.

2014-01-01

A new technique combining in situ X-ray diffraction using synchrotron radiation and infrared thermal imaging is reported. The technique enables the application, generation and measurement of significant thermal gradients, and furthermore allows the direct spatial correlation of thermal and crystallographic measurements. The design and implementation of a novel furnace enabling the simultaneous thermal and X-ray measurements is described. The technique is expected to have wide applicability in material science and engineering; here it has been applied to the study of solid oxide fuel cells at high temperature. PMID:25178003

Structure of nanocrystalline calcium silicate hydrates: insights from X-ray diffraction, synchrotron X-ray absorption and nuclear magnetic resonance.

PubMed

Grangeon, Sylvain; Claret, Francis; Roosz, Cédric; Sato, Tsutomu; Gaboreau, Stéphane; Linard, Yannick

2016-06-01

The structure of nanocrystalline calcium silicate hydrates (C-S-H) having Ca/Si ratios ranging between 0.57 ± 0.05 and 1.47 ± 0.04 was studied using an electron probe micro-analyser, powder X-ray diffraction, 29 Si magic angle spinning NMR, and Fourier-transform infrared and synchrotron X-ray absorption spectroscopies. All samples can be described as nanocrystalline and defective tobermorite. At low Ca/Si ratio, the Si chains are defect free and the Si Q 3 and Q 2 environments account, respectively, for up to 40.2 ± 1.5% and 55.6 ± 3.0% of the total Si, with part of the Q 3 Si being attributable to remnants of the synthesis reactant. As the Ca/Si ratio increases up to 0.87 ± 0.02, the Si Q 3 environment decreases down to 0 and is preferentially replaced by the Q 2 environment, which reaches 87.9 ± 2.0%. At higher ratios, Q 2 decreases down to 32.0 ± 7.6% for Ca/Si = 1.38 ± 0.03 and is replaced by the Q 1 environment, which peaks at 68.1 ± 3.8%. The combination of X-ray diffraction and NMR allowed capturing the depolymerization of Si chains as well as a two-step variation in the layer-to-layer distance. This latter first increases from ∼11.3 Å (for samples having a Ca/Si ratio <∼0.6) up to 12.25 Å at Ca/Si = 0.87 ± 0.02, probably as a result of a weaker layer-to-layer connectivity, and then decreases down to 11 Å when the Ca/Si ratio reaches 1.38 ± 0.03. The decrease in layer-to-layer distance results from the incorporation of interlayer Ca that may form a Ca(OH) 2 -like structure, nanocrystalline and intermixed with C-S-H layers, at high Ca/Si ratios.

High-energy transmission Laue micro-beam X-ray diffraction: a probe for intra-granular lattice orientation and elastic strain in thicker samples.

PubMed

Hofmann, Felix; Song, Xu; Abbey, Brian; Jun, Tea-Sung; Korsunsky, Alexander M

2012-05-01

An understanding of the mechanical response of modern engineering alloys to complex loading conditions is essential for the design of load-bearing components in high-performance safety-critical aerospace applications. A detailed knowledge of how material behaviour is modified by fatigue and the ability to predict failure reliably are vital for enhanced component performance. Unlike macroscopic bulk properties (e.g. stiffness, yield stress, etc.) that depend on the average behaviour of many grains, material failure is governed by `weakest link'-type mechanisms. It is strongly dependent on the anisotropic single-crystal elastic-plastic behaviour, local morphology and microstructure, and grain-to-grain interactions. For the development and validation of models that capture these complex phenomena, the ability to probe deformation behaviour at the micro-scale is key. The diffraction of highly penetrating synchrotron X-rays is well suited to this purpose and micro-beam Laue diffraction is a particularly powerful tool that has emerged in recent years. Typically it uses photon energies of 5-25 keV, limiting penetration into the material, so that only thin samples or near-surface regions can be studied. In this paper the development of high-energy transmission Laue (HETL) micro-beam X-ray diffraction is described, extending the micro-beam Laue technique to significantly higher photon energies (50-150 keV). It allows the probing of thicker sample sections, with the potential for grain-level characterization of real engineering components. The new HETL technique is used to study the deformation behaviour of individual grains in a large-grained polycrystalline nickel sample during in situ tensile loading. Refinement of the Laue diffraction patterns yields lattice orientations and qualitative information about elastic strains. After deformation, bands of high lattice misorientation can be identified in the sample. Orientation spread within individual scattering volumes is studied using a pattern-matching approach. The results highlight the inability of a simple Schmid-factor model to capture the behaviour of individual grains and illustrate the need for complementary mechanical modelling.

Time-resolved coherent X-ray diffraction imaging of surface acoustic waves

PubMed Central

Nicolas, Jan-David; Reusch, Tobias; Osterhoff, Markus; Sprung, Michael; Schülein, Florian J. R.; Krenner, Hubert J.; Wixforth, Achim; Salditt, Tim

2014-01-01

Time-resolved coherent X-ray diffraction experiments of standing surface acoustic waves, illuminated under grazing incidence by a nanofocused synchrotron beam, are reported. The data have been recorded in stroboscopic mode at controlled and varied phase between the acoustic frequency generator and the synchrotron bunch train. At each time delay (phase angle), the coherent far-field diffraction pattern in the small-angle regime is inverted by an iterative algorithm to yield the local instantaneous surface height profile along the optical axis. The results show that periodic nanoscale dynamics can be imaged at high temporal resolution in the range of 50 ps (pulse length). PMID:25294979

Time-resolved coherent X-ray diffraction imaging of surface acoustic waves.

PubMed

Nicolas, Jan-David; Reusch, Tobias; Osterhoff, Markus; Sprung, Michael; Schülein, Florian J R; Krenner, Hubert J; Wixforth, Achim; Salditt, Tim

2014-10-01

Time-resolved coherent X-ray diffraction experiments of standing surface acoustic waves, illuminated under grazing incidence by a nanofocused synchrotron beam, are reported. The data have been recorded in stroboscopic mode at controlled and varied phase between the acoustic frequency generator and the synchrotron bunch train. At each time delay (phase angle), the coherent far-field diffraction pattern in the small-angle regime is inverted by an iterative algorithm to yield the local instantaneous surface height profile along the optical axis. The results show that periodic nanoscale dynamics can be imaged at high temporal resolution in the range of 50 ps (pulse length).

Symmetry and light stuffing of H o 2 T i 2 O 7 ,   E r 2 T i 2 O 7 , and Y b 2 T i 2 O 7 characterized by synchrotron x-ray diffraction

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

Baroudi, Kristen; Gaulin, Bruce D.; Lapidus, Saul H.

2015-07-01

The Ho2Ti2O7, Er2Ti2O7 and Yb2Ti2O7 pyrochlores were studied by synchrotron X-ray diffraction to determine whether the (002) peak, forbidden in the pyrochlore space group Fd-3m but observed in single crystal neutron scattering measurements, is present due to a deviation of their pyrochlore structure from Fd-3m symmetry. Synchrotron diffraction measurements on precisely synthesized stoichiometric and non-stoichiometric powders and a crushed floating zone crystal of Ho2Ti2O7 revealed that the (002) reflection is absent in all cases to a sensitivity of approximately one part in 30,000 of the strongest X-ray diffraction peak. This indicates to high sensitivity that the structural space group ofmore » these rare earth titanate pyrochlores is Fd-3m, and that thus the (002) peak observed in the neutron scattering experiments has a non-structural origin. The cell parameters and internal strain for lightly stuffed Ho2+xTi2-xO7 are also presented.« less

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.

Residual stress determination in oxide layers at different length scales combining Raman spectroscopy and X-ray diffraction: Application to chromia-forming metallic alloys

DOE PAGES

Guerain, Mathieu; Grosseau-Poussard, Jean-Luc; Geandier, Guillaume; ...

2017-11-21

In oxidizing environments, the protection of metals and alloys against further oxidation at high temperature is provided by the oxide film itself. This protection is efficient only if the formed film adheres well to the metal (substrate), i.e., without microcracks and spalls induced by thermomechanical stresses. In this study, the residual stresses at both macroscopic and microscopic scales in the oxide film adhering to the substrate and over the damaged areas have been rigorously determined on the same samples for both techniques. Ni-30Cr and Fe-47Cr alloys have been oxidized together at 900 and 1000 °C, respectively, to create films withmore » a thickness of a few microns. A multi-scale approach was adopted: macroscopic stress was determined by conventional X-ray diffraction and Raman spectroscopy, while microscopic residual stress mappings were performed over different types of bucklings using Raman micro-spectroscopy and synchrotron micro-diffraction. A very good agreement is found at macro- and microscales between the residual stress values obtained with both techniques, giving confidence on the reliability of the measurements. In addition, relevant structural information at the interface between the metallic substrate and the oxide layer was collected by micro-diffraction, a non-destructive technique that allows mapping through the oxide layer, and both the grain size and the crystallographic orientation of the supporting polycrystalline metal located either under a buckling or not were measured.« less

Residual stress determination in oxide layers at different length scales combining Raman spectroscopy and X-ray diffraction: Application to chromia-forming metallic alloys

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

Guerain, Mathieu; Grosseau-Poussard, Jean-Luc; Geandier, Guillaume

In oxidizing environments, the protection of metals and alloys against further oxidation at high temperature is provided by the oxide film itself. This protection is efficient only if the formed film adheres well to the metal (substrate), i.e., without microcracks and spalls induced by thermomechanical stresses. In this study, the residual stresses at both macroscopic and microscopic scales in the oxide film adhering to the substrate and over the damaged areas have been rigorously determined on the same samples for both techniques. Ni-30Cr and Fe-47Cr alloys have been oxidized together at 900 and 1000 °C, respectively, to create films withmore » a thickness of a few microns. A multi-scale approach was adopted: macroscopic stress was determined by conventional X-ray diffraction and Raman spectroscopy, while microscopic residual stress mappings were performed over different types of bucklings using Raman micro-spectroscopy and synchrotron micro-diffraction. A very good agreement is found at macro- and microscales between the residual stress values obtained with both techniques, giving confidence on the reliability of the measurements. In addition, relevant structural information at the interface between the metallic substrate and the oxide layer was collected by micro-diffraction, a non-destructive technique that allows mapping through the oxide layer, and both the grain size and the crystallographic orientation of the supporting polycrystalline metal located either under a buckling or not were measured.« less

Residual stress determination in oxide layers at different length scales combining Raman spectroscopy and X-ray diffraction: Application to chromia-forming metallic alloys

NASA Astrophysics Data System (ADS)

Guerain, Mathieu; Grosseau-Poussard, Jean-Luc; Geandier, Guillaume; Panicaud, Benoit; Tamura, Nobumichi; Kunz, Martin; Dejoie, Catherine; Micha, Jean-Sebastien; Thiaudière, Dominique; Goudeau, Philippe

2017-11-01

In oxidizing environments, the protection of metals and alloys against further oxidation at high temperature is provided by the oxide film itself. This protection is efficient only if the formed film adheres well to the metal (substrate), i.e., without microcracks and spalls induced by thermomechanical stresses. In this study, the residual stresses at both macroscopic and microscopic scales in the oxide film adhering to the substrate and over the damaged areas have been rigorously determined on the same samples for both techniques. Ni-30Cr and Fe-47Cr alloys have been oxidized together at 900 and 1000 °C, respectively, to create films with a thickness of a few microns. A multi-scale approach was adopted: macroscopic stress was determined by conventional X-ray diffraction and Raman spectroscopy, while microscopic residual stress mappings were performed over different types of bucklings using Raman micro-spectroscopy and synchrotron micro-diffraction. A very good agreement is found at macro- and microscales between the residual stress values obtained with both techniques, giving confidence on the reliability of the measurements. In addition, relevant structural information at the interface between the metallic substrate and the oxide layer was collected by micro-diffraction, a non-destructive technique that allows mapping through the oxide layer, and both the grain size and the crystallographic orientation of the supporting polycrystalline metal located either under a buckling or not were measured.

X-ray laser–induced electron dynamics observed by femtosecond diffraction from nanocrystals of Buckminsterfullerene

PubMed Central

Abbey, Brian; Dilanian, Ruben A.; Darmanin, Connie; Ryan, Rebecca A.; Putkunz, Corey T.; Martin, Andrew V.; Wood, David; Streltsov, Victor; Jones, Michael W. M.; Gaffney, Naylyn; Hofmann, Felix; Williams, Garth J.; Boutet, Sébastien; Messerschmidt, Marc; Seibert, M. Marvin; Williams, Sophie; Curwood, Evan; Balaur, Eugeniu; Peele, Andrew G.; Nugent, Keith A.; Quiney, Harry M.

2016-01-01

X-ray free-electron lasers (XFELs) deliver x-ray pulses with a coherent flux that is approximately eight orders of magnitude greater than that available from a modern third-generation synchrotron source. The power density of an XFEL pulse may be so high that it can modify the electronic properties of a sample on a femtosecond time scale. Exploration of the interaction of intense coherent x-ray pulses and matter is both of intrinsic scientific interest and of critical importance to the interpretation of experiments that probe the structures of materials using high-brightness femtosecond XFEL pulses. We report observations of the diffraction of extremely intense 32-fs nanofocused x-ray pulses by a powder sample of crystalline C60. We find that the diffraction pattern at the highest available incident power significantly differs from the one obtained using either third-generation synchrotron sources or XFEL sources operating at low output power and does not correspond to the diffraction pattern expected from any known phase of crystalline C60. We interpret these data as evidence of a long-range, coherent dynamic electronic distortion that is driven by the interaction of the periodic array of C60 molecular targets with intense x-ray pulses of femtosecond duration. PMID:27626076

Simultaneous, single-pulse, synchrotron x-ray imaging and diffraction under gas gun loading

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

Fan, D.; Luo, S. N., E-mail: sluo@pims.ac.cn; Key Laboratory of Advanced Technologies of Materials, Ministry of Education, Southwest Jiaotong University, Chengdu, Sichuan 610031

We develop a mini gas gun system for simultaneous, single-pulse, x-ray diffraction and imaging under high strain-rate loading at the beamline 32-ID of the Advanced Photon Source. In order to increase the reciprocal space covered by a small-area detector, a conventional target chamber is split into two chambers: a narrowed measurement chamber and a relief chamber. The gas gun impact is synchronized with synchrotron x-ray pulses and high-speed cameras. Depending on a camera’s capability, multiframe imaging and diffraction can be achieved. The proof-of-principle experiments are performed on single-crystal sapphire. The diffraction spots and images during impact are analyzed to quantifymore » lattice deformation and fracture; fracture is dominated by splitting cracks followed by wing cracks, and diffraction peaks are broadened likely due to mosaic spread. Our results demonstrate the potential of such multiscale measurements for studying high strain-rate phenomena at dynamic extremes.« less

In situ synchrotron X-ray diffraction study on epitaxial-growth dynamics of III–V semiconductors

NASA Astrophysics Data System (ADS)

Takahasi, Masamitu

2018-05-01

The application of in situ synchrotron X-ray diffraction (XRD) to the molecular-beam epitaxial (MBE) growth of III–V semiconductors is overviewed along with backgrounds of the diffraction theory and instrumentation. X-rays are sensitive not only to the surface of growing films but also to buried interfacial structures because of their large penetration depth. Moreover, a spatial coherence length up to µm order makes X-rays widely applicable to the characterization of low-dimensional structures, such as quantum dots and wires. In situ XRD studies during growth were performed using an X-ray diffractometer, which was combined with an MBE chamber. X-ray reciprocal space mapping at a speed matching a typical growth rate was achieved using intense X-rays available from a synchrotron light source and an area detector. The importance of measuring the three-dimensional distribution of XRD intensity in a reciprocal space map is demonstrated for the MBE growth of two-, one-, and zero-dimensional structures. A large amount of information about the growth process of two-dimensional InGaAs/GaAs(001) epitaxial films has been provided by three-dimensional X-ray reciprocal mappings, including the anisotropic strain relaxation, the compositional inhomogeneity, and the evolution of surface and interfacial roughness. For one-dimensional GaAs nanowires grown in a Au-catalyzed vapor-liquid–solid mode, the relationship between the diameter of the nanowires and the formation of polytypes has been suggested on the basis of in situ XRD measurements. In situ three-dimensional X-ray reciprocal space mapping is also shown to be useful for determining the lateral and vertical sizes of self-assembled InAs/GaAs(001) quantum dots as well as their internal strain distributions during growth.

Crystallographic Study of Itokawa Particle, RA-QD02-0127 by Using Energy-Scanning X-Ray Diffraction Method with Synchrotron Radiation

NASA Astrophysics Data System (ADS)

Hagiya, K.; Ohsumi, K.; Komatsu, M.; Mikouchi, T.; Zolensky, M. E.; Hirata, A.; Yamaguchi, S.; Kurokawa, A.

2016-08-01

Crystallographic study of Itokawa particle, RA-QD02-0127 by using new X-ray diffraction method was performed. The purpose of this study is to understand better the metamorphic and impact shock history of asteroid Itokawa, and other S-class asteroids.

Thorough small-angle X-ray scattering analysis of the instability of liquid micro-jets in air.

PubMed

Marmiroli, Benedetta; Cacho-Nerin, Fernando; Sartori, Barbara; Pérez, Javier; Amenitsch, Heinz

2014-01-01

Liquid jets are of interest, both for their industrial relevance and for scientific applications (more important, in particular for X-rays, after the advent of free-electron lasers that require liquid jets as sample carrier). Instability mechanisms have been described theoretically and by numerical simulation, but confirmed by few experimental techniques. In fact, these are mainly based on cameras, which is limited by the imaging resolution, and on light scattering, which is hindered by absorption, reflection, Mie scattering and multiple scattering due to complex air/liquid interfaces during jet break-up. In this communication it is demonstrated that synchrotron small-angle X-ray scattering (SAXS) can give quantitative information on liquid jet dynamics at the nanoscale, by detecting time-dependent morphology and break-up length. Jets ejected from circular tubes of different diameters (100-450 µm) and speeds (0.7-21 m s(-1)) have been explored to cover the Rayleigh and first wind-induced regimes. Various solvents (water, ethanol, 2-propanol) and their mixtures have been examined. The determination of the liquid jet behaviour becomes essential, as it provides background data in subsequent studies of chemical and biological reactions using SAXS or X-ray diffraction based on synchrotron radiation and free-electron lasers.

Observation of Structure of Surfaces and Interfaces by Synchrotron X-ray Diffraction: Atomic-Scale Imaging and Time-Resolved Measurements

NASA Astrophysics Data System (ADS)

Wakabayashi, Yusuke; Shirasawa, Tetsuroh; Voegeli, Wolfgang; Takahashi, Toshio

2018-06-01

The recent developments in synchrotron optics, X-ray detectors, and data analysis algorithms have enhanced the capability of the surface X-ray diffraction technique. This technique has been used to clarify the atomic arrangement around surfaces in a non-contact and nondestructive manner. An overview of surface X-ray diffraction, from the historical development to recent topics, is presented. In the early stage of this technique, surface reconstructions of simple semiconductors or metals were studied. Currently, the surface or interface structures of complicated functional materials are examined with sub-Å resolution. As examples, the surface structure determination of organic semiconductors and of a one-dimensional structure on silicon are presented. A new frontier is time-resolved interfacial structure analysis. A recent observation of the structure and dynamics of the electric double layer of ionic liquids, and an investigation of the structural evolution in the wettability transition on a TiO2 surface that utilizes a newly designed time-resolved surface diffractometer, are presented.

The X-ray Fluorescence Microscopy Beamline at the Australian Synchrotron

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

Paterson, D.; Jonge, M. D. de; Howard, D. L.

2011-09-09

A hard x-ray micro-nanoprobe has commenced operation at the Australian Synchrotron providing versatile x-ray fluorescence microscopy across an incident energy range from 4 to 25 keV. Two x-ray probes are used to collect {mu}-XRF and {mu}-XANES for elemental and chemical microanalysis: a Kirkpatrick-Baez mirror microprobe for micron resolution studies and a Fresnel zone plate nanoprobe capable of 60-nm resolution. Some unique aspects of the beamline design and operation are discussed. An advanced energy dispersive x-ray fluorescence detection scheme named Maia has been developed for the beamline, which enables ultrafast x-ray fluorescence microscopy.

Magnetic x-ray scattering studies of holmium using synchro- tron radiation

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

Gibbs, D.; Moncton, D.E.; D'Amico, K.L.

1985-07-08

We present the results of magnetic x-ray scattering experiments on the rare-earth metal holmium using synchrotron radiation. Direct high-resolution measurements of the nominally incommensurate magnetic satellite reflections reveal new lock-in behavior which we explain within a simple spin-discommensuration model. As a result of magnetoelastic coupling, the spin-discommensuration array produces additional x-ray diffraction satellites. Their observation further substantiates the model and demonstrates additional advantages of synchrotron radiation for magnetic-structure studies.

Application of X-ray synchrotron microscopy instrumentation in biology

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

Gasperini, F. M.; Pereira, G. R.; Granjeiro, J. M.

2011-07-01

X-ray micro-fluorescence imaging technique has been used as a significant tool in order to investigate minerals contents in some kinds of materials. The aim of this study was to evaluate the elemental distribution of calcium and zinc in bone substitute materials (nano-hydroxyapatite spheres) and cortical bones through X-Ray Micro-fluorescence analysis with the increment of Synchrotron Radiation in order to evaluate the characteristics of the newly formed bone and its interface, the preexisting bone and biomaterials by the arrangement of collagen fibers and its birefringence. The elemental mapping was carried out at Brazilian Synchrotron Light Laboratory, Campinas - Sao Paulo, Brazilmore » working at D09-XRF beam line. Based on this study, the results suggest that hydroxyapatite-based biomaterials are biocompatible, promote osteo-conduction and favored bone repair. (authors)« less

Complementary use of monochromatic and white-beam X-ray micro-diffraction for the investigation of ancient materials

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

Dejoie, Catherine; Tamura, Nobumichi; Kunz, Martin

Archaeological artefacts are often heterogeneous materials where several phases coexist in a wide grain size distribution. Most of the time, retrieving structure information at the micrometre scale is of great importance for these materials. Particularly, the organization of different phases at the micrometre scale is closely related to optical or mechanical properties, manufacturing processes, functionalities in ancient times and long-term conservation. Between classic X-ray powder diffraction with a millimetre beam and transmission electron microscopy, a gap exists and structure and phase information at the micrometre scale are missing. Using a micrometre-size synchrotron X-ray beam, a hybrid approach combining both monochromaticmore » powder micro-diffraction and Laue single-crystal micro-diffraction was deployed to obtain information from nanometre- and micrometre-size phases, respectively. Therefore providing a way to bridge the aforementioned gap, this unique methodology was applied to three different types of ancient materials that all show a strong heterogeneity. In Roman terra sigillata, the specific distribution of nanocrystalline hematite is mainly responsible for the deep-red tone of the slip, while the distribution of micrometre-size quartz in ceramic bodies reflects the change of manufacturing process between pre-sigillata and high-quality sigillata periods. In the second example, we investigated the modifications occurring in Neolithic and geological flints after a heating process. By separating the diffracted signal coming from the nano- and the micrometre scale, we observed a domain size increase for nanocrystalline quartz in geological flints and a relaxation of the residual strain in larger detritic quartz. In conclusion, through the study of a Roman iron nail, we showed that the carburation process to strengthen the steel was mainly a surface process that formed 10–20 µm size domains of single–crystal ferrite and nanocrystalline cementite.« less

Complementary use of monochromatic and white-beam X-ray micro-diffraction for the investigation of ancient materials

DOE PAGES

Dejoie, Catherine; Tamura, Nobumichi; Kunz, Martin; ...

2015-09-20

Archaeological artefacts are often heterogeneous materials where several phases coexist in a wide grain size distribution. Most of the time, retrieving structure information at the micrometre scale is of great importance for these materials. Particularly, the organization of different phases at the micrometre scale is closely related to optical or mechanical properties, manufacturing processes, functionalities in ancient times and long-term conservation. Between classic X-ray powder diffraction with a millimetre beam and transmission electron microscopy, a gap exists and structure and phase information at the micrometre scale are missing. Using a micrometre-size synchrotron X-ray beam, a hybrid approach combining both monochromaticmore » powder micro-diffraction and Laue single-crystal micro-diffraction was deployed to obtain information from nanometre- and micrometre-size phases, respectively. Therefore providing a way to bridge the aforementioned gap, this unique methodology was applied to three different types of ancient materials that all show a strong heterogeneity. In Roman terra sigillata, the specific distribution of nanocrystalline hematite is mainly responsible for the deep-red tone of the slip, while the distribution of micrometre-size quartz in ceramic bodies reflects the change of manufacturing process between pre-sigillata and high-quality sigillata periods. In the second example, we investigated the modifications occurring in Neolithic and geological flints after a heating process. By separating the diffracted signal coming from the nano- and the micrometre scale, we observed a domain size increase for nanocrystalline quartz in geological flints and a relaxation of the residual strain in larger detritic quartz. In conclusion, through the study of a Roman iron nail, we showed that the carburation process to strengthen the steel was mainly a surface process that formed 10–20 µm size domains of single–crystal ferrite and nanocrystalline cementite.« less

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

Time-resolved structural studies at synchrotrons and X-ray free electron lasers: opportunities and challenges

PubMed Central

Neutze, Richard; Moffat, Keith

2012-01-01

X-ray free electron lasers (XFELs) are potentially revolutionary X-ray sources because of their very short pulse duration, extreme peak brilliance and high spatial coherence, features that distinguish them from today’s synchrotron sources. We review recent time-resolved Laue diffraction and time-resolved wide angle X-ray scattering (WAXS) studies at synchrotron sources, and initial static studies at XFELs. XFELs have the potential to transform the field of time-resolved structural biology, yet many challenges arise in devising and adapting hardware, experimental design and data analysis strategies to exploit their unusual properties. Despite these challenges, we are confident that XFEL sources are poised to shed new light on ultrafast protein reaction dynamics. PMID:23021004

Arsenic speciation in sinter mineralization from a hydrothermal channel of El Tatio geothermal field, Chile

NASA Astrophysics Data System (ADS)

Alsina, Marco A.; Zanella, Luciana; Hoel, Cathleen; Pizarro, Gonzalo E.; Gaillard, Jean-François; Pasten, Pablo A.

2014-10-01

El Tatio geothermal field is the principal natural source of arsenic for the Loa River, the main surface water resource in the hyper-arid Atacama Desert (Antofagasta Region, Northern Chile). Prior investigations by bulk X-ray absorption spectroscopy have identified hydrous ferric oxides as the principal arsenic-containing phase in sinter material from El Tatio, suggesting sorption as the main mechanism for arsenic scavenging by the solid phases of these hot spring environments. Here we examine siliceous sinter material sampled from a hydrothermal channel using synchrotron based X-ray micro-probe techniques, including As and Fe Kα X-ray fluorescence (μ-XRF), As K-edge X-ray absorption near edge structure (μ-XANES), and X-ray diffraction (μ-XRD). Least-squares linear fitting of μ-XANES spectra shows that arsenic is predominantly present as arsenate sorbed on hydrous ferric oxides (63% molar proportion), but we also identify nodular arsenide micro-mineralizations (37% molar proportion) similar to loellingite (FeAs2), not previously detected during bulk-scale analysis of the sinter material. Presence of arsenide mineralizations indicates development of anoxic environments on the surface of the siliceous sinter, and suggests a more complex biogeochemistry for arsenic than previously observed for circum-neutral pH brine hot spring environments.

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.

From cells to laminate: probing and modeling residual stress evolution in thin silicon photovoltaic modules using synchrotron X-ray micro-diffraction experiments and finite element simulations

DOE PAGES

Tippabhotla, Sasi Kumar; Radchenko, Ihor; Song, W. J. R.; ...

2017-04-12

Fracture of silicon crystalline solar cells has recently been observed in increasing percentages especially in solar photovoltaic (PV) modules involving thinner silicon solar cells (<200 μm). Many failures due to fracture have been reported from the field because of environmental loading (snow, wind, etc.) as well as mishandling of the solar PV modules (during installation, maintenance, etc.). However, a significantly higher number of failures have also been reported during module encapsulation (lamination) indicating high residual stress in the modules and thus more prone to cell cracking. Here in this paper we report through the use of synchrotron X-ray submicron diffractionmore » coupled with physics-based finite element modeling, the complete residual stress evolution in mono-crystalline silicon solar cells during PV module integration process. For the first time, we unravel the reason for the high stress and cracking of silicon cells near soldered inter-connects. Our experiments revealed a significant increase of residual stress in the silicon cell near the solder joint after lamination. Moreover, our finite element simulations show that this increase of stress during lamination is a result of highly localized bending of the cell near the soldered inter-connects. Further, the synchrotron X-ray submicron diffraction has proven to be a very effective way to quantitatively probe mechanical stress in encapsulated silicon solar cells. Thus, this technique has ultimately enabled these findings leading to the enlightening of the role of soldering and encapsulation processes on the cell residual stress. This model can be further used to suggest methodologies that could lead to lower stress in encapsulated silicon solar cells, which are the subjects of our continued investigations.« less

From cells to laminate: probing and modeling residual stress evolution in thin silicon photovoltaic modules using synchrotron X-ray micro-diffraction experiments and finite element simulations

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

Tippabhotla, Sasi Kumar; Radchenko, Ihor; Song, W. J. R.

Fracture of silicon crystalline solar cells has recently been observed in increasing percentages especially in solar photovoltaic (PV) modules involving thinner silicon solar cells (<200 μm). Many failures due to fracture have been reported from the field because of environmental loading (snow, wind, etc.) as well as mishandling of the solar PV modules (during installation, maintenance, etc.). However, a significantly higher number of failures have also been reported during module encapsulation (lamination) indicating high residual stress in the modules and thus more prone to cell cracking. Here in this paper we report through the use of synchrotron X-ray submicron diffractionmore » coupled with physics-based finite element modeling, the complete residual stress evolution in mono-crystalline silicon solar cells during PV module integration process. For the first time, we unravel the reason for the high stress and cracking of silicon cells near soldered inter-connects. Our experiments revealed a significant increase of residual stress in the silicon cell near the solder joint after lamination. Moreover, our finite element simulations show that this increase of stress during lamination is a result of highly localized bending of the cell near the soldered inter-connects. Further, the synchrotron X-ray submicron diffraction has proven to be a very effective way to quantitatively probe mechanical stress in encapsulated silicon solar cells. Thus, this technique has ultimately enabled these findings leading to the enlightening of the role of soldering and encapsulation processes on the cell residual stress. This model can be further used to suggest methodologies that could lead to lower stress in encapsulated silicon solar cells, which are the subjects of our continued investigations.« less

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.

Development of an adaptable coherent x-ray diffraction microscope with the emphasis on imaging hydrated specimens.

PubMed

Nam, Daewoong; Park, Jaehyun; Gallagher-Jones, Marcus; Shimada, Hiroki; Kim, Sangsoo; Kim, Sunam; Kohmura, Yoshiki; Ishikawa, Tetsuya; Song, Changyong

2013-11-01

This paper describes the development of a versatile coherent x-ray diffraction microscope capable of imaging biological specimens in solution. The microscope is a flexible platform accommodating various conditions, from low vacuum (10(-2) Pa) to helium gas filled ambient pressure. This flexibility greatly expands the application area, from in situ materials science to biology systems in their native state, by significantly relaxing restrictions to the sample environment. The coherent diffraction microscope has been used successfully to image a yeast cell immersed in buffer solution. We believe that the design of this coherent diffraction microscope can be directly adapted to various platforms such as table top soft x-ray laser, synchrotron x-ray sources, and x-ray free electron laser with minor relevant adjustments.

Development of an adaptable coherent x-ray diffraction microscope with the emphasis on imaging hydrated specimens

NASA Astrophysics Data System (ADS)

Nam, Daewoong; Park, Jaehyun; Gallagher-Jones, Marcus; Shimada, Hiroki; Kim, Sangsoo; Kim, Sunam; Kohmura, Yoshiki; Ishikawa, Tetsuya; Song, Changyong

2013-11-01

This paper describes the development of a versatile coherent x-ray diffraction microscope capable of imaging biological specimens in solution. The microscope is a flexible platform accommodating various conditions, from low vacuum (10-2 Pa) to helium gas filled ambient pressure. This flexibility greatly expands the application area, from in situ materials science to biology systems in their native state, by significantly relaxing restrictions to the sample environment. The coherent diffraction microscope has been used successfully to image a yeast cell immersed in buffer solution. We believe that the design of this coherent diffraction microscope can be directly adapted to various platforms such as table top soft x-ray laser, synchrotron x-ray sources, and x-ray free electron laser with minor relevant adjustments.

Partially coherent X-ray wavefront propagation simulations including grazing-incidence focusing optics.

PubMed

Canestrari, Niccolo; Chubar, Oleg; Reininger, Ruben

2014-09-01

X-ray beamlines in modern synchrotron radiation sources make extensive use of grazing-incidence reflective optics, in particular Kirkpatrick-Baez elliptical mirror systems. These systems can focus the incoming X-rays down to nanometer-scale spot sizes while maintaining relatively large acceptance apertures and high flux in the focused radiation spots. In low-emittance storage rings and in free-electron lasers such systems are used with partially or even nearly fully coherent X-ray beams and often target diffraction-limited resolution. Therefore, their accurate simulation and modeling has to be performed within the framework of wave optics. Here the implementation and benchmarking of a wave-optics method for the simulation of grazing-incidence mirrors based on the local stationary-phase approximation or, in other words, the local propagation of the radiation electric field along geometrical rays, is described. The proposed method is CPU-efficient and fully compatible with the numerical methods of Fourier optics. It has been implemented in the Synchrotron Radiation Workshop (SRW) computer code and extensively tested against the geometrical ray-tracing code SHADOW. The test simulations have been performed for cases without and with diffraction at mirror apertures, including cases where the grazing-incidence mirrors can be hardly approximated by ideal lenses. Good agreement between the SRW and SHADOW simulation results is observed in the cases without diffraction. The differences between the simulation results obtained by the two codes in diffraction-dominated cases for illumination with fully or partially coherent radiation are analyzed and interpreted. The application of the new method for the simulation of wavefront propagation through a high-resolution X-ray microspectroscopy beamline at the National Synchrotron Light Source II (Brookhaven National Laboratory, USA) is demonstrated.

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

In-situ synchrotron wide-angle X-ray diffraction as a rapid method for cocrystal/salt screening.

PubMed

Dong, Pin; Lin, Ling; Li, Yongcheng; Huang, Zhengwei; Lang, Tianqun; Wu, Chuanbin; Lu, Ming

2015-12-30

The purpose of this work was to explore in-situ synchrotron wide-angle X-ray diffraction (WAXD) as a rapid and accurate tool to screen and monitor the formation of cocrystal/salts during heating. The active pharmaceutical ingredients (caffeine, carbamazepine and lamotrigine) were respectively mixed with the coformer (saccharin), and then heated by the hot stage. Real-time process monitoring was performed using synchrotron WAXD to assess cocrystal formation and subsequently compared to differential scanning calorimetry (DSC) measurements. The effect of heating rates and cocrystal growth behavior were investigated. Synchrotron WAXD was fast and sensitive to detect cocrystal formation with the appearance of characteristic diffraction rings, even at the heating rate of 30°C/min, while DSC curves showed overlapped peaks. Unlike the indirect characterization of DSC on endo/exothermic peaks, synchrotron WAXD can directly and qualitatively determine cocrystal by diffraction peaks. The diffraction intensity-temperature curves and the corresponding first-derivative curves clearly exhibited the growth behavior of cocrystal upon heating, providing useful information to optimize the process temperature of hot melt extrusion to continuously manufacture cocrystal. The study suggests that in-situ synchrotron WAXD could provide a one-step process to screen cocrystal at high efficiency and reveal the details of cocrystal/salts growth behavior. Copyright © 2015 Elsevier B.V. All rights reserved.

Pressure-induced Lifshitz transition in NbP: Raman, x-ray diffraction, electrical transport, and density functional theory

NASA Astrophysics Data System (ADS)

Gupta, Satyendra Nath; Singh, Anjali; Pal, Koushik; Muthu, D. V. S.; Shekhar, C.; Qi, Yanpeng; Naumov, Pavel G.; Medvedev, Sergey A.; Felser, C.; Waghmare, U. V.; Sood, A. K.

2018-02-01

We report high-pressure Raman, synchrotron x-ray diffraction, and electrical transport studies on Weyl semimetals NbP and TaP along with first-principles density functional theoretical (DFT) analysis. The frequencies of first-order Raman modes of NbP harden with increasing pressure and exhibit a slope change at Pc˜9 GPa. The pressure-dependent resistivity exhibits a minimum at Pc. The temperature coefficient of resistivity below Pc is positive as expected for semimetals but changes significantly in the high-pressure phase. Using DFT calculations, we show that these anomalies are associated with a pressure-induced Lifshitz transition, which involves the appearance of electron and hole pockets in its electronic structure. In contrast, the results of Raman and synchrotron x-ray diffraction experiments on TaP and DFT calculations show that TaP is quite robust under pressure and does not undergo any phase transition.

{ital In-situ} x-ray investigation of hydrogen charging in thin film bimetallic electrodes

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

Jisrawi, N.M.; Wiesmann, H.; Ruckman, M.W.

Hydrogen uptake and discharge by thin metallic films under potentiostatic control was studied using x-ray diffraction at the National Synchrotron Light Source (NSLS). The formation of metal-hydrogen phases in Pd, Pd-capped Nb and Pd/Nb multilayer electrode structures was deduced from x-ray diffraction data and correlated with the cyclic voltammetry (CV) peaks. The x-ray data was also used to construct a plot of the hydrogen concentration as a function of cell potential for a multilayered thin film. {copyright} {ital 1997 Materials Research Society.}

Improvement of the efficient referencing and sample positioning system for micro focused synchrotron X-ray techniques

NASA Astrophysics Data System (ADS)

Spangenberg, T.; Göttlicher, J.; Steininger, R.

2016-05-01

An efficient referencing and sample positioning system is a basic tool for a micro focus beamline at a synchrotron. The seven years ago introduced command line based system was upgraded at SUL-X beamline at ANKA [1]. A new combination of current server client techniques offers direct control and facilitates unexperienced users the handling of this frequently used tool.

Hyperspectral Analyses of Wild 2 Grains Using Synchrotron Radiation

NASA Astrophysics Data System (ADS)

Simionovici, A. S.; Lemelle, L.; Ferroir, T.; Gillet, P.; Borg, J.; Grossemy, F.; Djouadi, Z.; Bleuet, P.; Susini, J.

2006-12-01

This work is part of the Preliminary Examination Team (PET) on Bulk Chemistry investigation of Wild 2 cometary grains brought back to Earth by the NASA Stardust mission [1]. X-rays are among the least destructive yet sensitive micro-probes, capable of analysing minute samples embedded in low density collectors, so methods based on Synchrotron Radiation had access to Stardust samples in priority. The main goal of the PET was to produce a preliminary characterization of the abundance and nature of the elements present in the returned samples [2]. In this phase it was paramount to analyze the grains in-situ, in the aerogel foam of the collectors to record the total mass fragments and avoid extraction risks. We have performed measurements on beamlines ID22/ID21 of the ESRF synchrotron in Grenoble, France, devoted to high/low energy microspectroscopy and recorded results on a collection of 6 keystones. Terminal particles as well as fragmentation tracks in the aerogel were mapped out with micron resolution, recording total mass composition for elements of Z>15 by means of X-ray fluorescence [3], as well as structural information by X-ray diffraction. This allowed the direct identification of the mineralogy of some of the grains. Finally, we recorded the evolution of the charge states of S and Fe as a function of the position in the track by means of micro-Xanes measurements. All these analyses were combined to produce a description of the Wild 2 cometary grains [4], as well as a history of their formation and of the thermal interactions during their slowing down in the aerogel collectors. [1] Brownlee, D. E. et al., LPSC XXXVII, abstract nr. 2286, 2006. [2] G. J. Flynn et al., LPSC XXXVII, abstract nr. 1217, 2006. [3] A. Simionovici, P. Chevallier, Chap. 7, Handbook of Practical X-Ray Fluorescence Analysis, 66-83, Springer, 2006. [4] G. J. Flynn et al., Science, (submitted), 2006.

MICROANALYSIS OF MATERIALS USING SYNCHROTRON RADIATION.

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

JONES,K.W.; FENG,H.

2000-12-01

High intensity synchrotron radiation produces photons with wavelengths that extend from the infrared to hard x rays with energies of hundreds of keV with uniquely high photon intensities that can be used to determine the composition and properties of materials using a variety of techniques. Most of these techniques represent extensions of earlier work performed with ordinary tube-type x-ray sources. The properties of the synchrotron source such as the continuous range of energy, high degree of photon polarization, pulsed beams, and photon flux many orders of magnitude higher than from x-ray tubes have made possible major advances in the possiblemore » chemical applications. We describe here ways that materials analyses can be made using the high intensity beams for measurements with small beam sizes and/or high detection sensitivity. The relevant characteristics of synchrotron x-ray sources are briefly summarized to give an idea of the x-ray parameters to be exploited. The experimental techniques considered include x-ray fluorescence, absorption, and diffraction. Examples of typical experimental apparatus used in these experiments are considered together with descriptions of actual applications.« less

X ray reflection masks: Manufacturing, characterization and first tests

NASA Astrophysics Data System (ADS)

Rahn, Stephen

1992-09-01

SXPL (Soft X-ray Projection Lithography) multilayer mirrors are characterized, laterally structured and then used as reflection masks in a projecting lithography procedure. Mo/Si-multilayer mirrors with a 2d in the region of 14 nm were characterized by Cu-k(alpha) grazing incidence as well as soft X-ray normal incidence reflectivity measurements. The multilayer mirrors were patterned by reactive ion etching with CF4 using a photoresist as etch mask, thus producing X-ray reflection masks. The masks were tested at the synchrotron radiation laboratory of the electron accelerator ELSA. A double crystal X-ray monochromator was modified so as to allow about 0.5 sq cm of the reflection mask to be illuminated by white synchrotron radiation. The reflected patterns were projected (with an energy of 100 eV) onto a resist and structure sizes down to 8 micrometers were nicely reproduced. Smaller structures were distorted by Fresnel-diffraction. The theoretically calculated diffraction images agree very well with the observed images.

Ion beam analysis in cultural heritage studies: Milestones and perspectives

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

Dran, Jean-Claude; Calligaro, Thomas

2013-07-18

For three decades, ion beam analysis (IBA) in external mode was considered as the best choice for the characterisation of cultural heritage materials, as it combines excellent analytical performance and non-invasive character. However, in recent years, other analytical techniques arose as serious competitors, such as those based on synchrotron radiation (X-ray absorption, fluorescence or diffraction) or those using portable instruments (XRF, micro-Raman). It is shown that nevertheless IBA remains unmatched thanks to two unique features, namely the analysis of light elements and the high-resolution 3D chemical imaging.

X-ray diffraction imaging (topography) of electroopticcrystals by synchrotron radiation

NASA Technical Reports Server (NTRS)

Steiner, Bruce; Kuriyama, Masao; Dobbyn, Ronald C.; Laor, Uri

1988-01-01

Information of special interest to crystal growers and device physicists now available from monochromatic synchrotron diffraction imaging (topography) is reviewed. Illustrations are taken from a variety of electro-optic crystals. Aspects of the detailed understanding of crystal growth processes obtainable from carefully selected samples are described. Finally, new experimental opportunities now available for exploitation are indicated.

Idealized powder diffraction patterns for cellulose polymorphs

USDA-ARS?s Scientific Manuscript database

Cellulose samples are routinely analyzed by X-ray diffraction to determine their crystal type (polymorph) and crystallinity. However, the connection is seldom made between those efforts and the crystal structures of cellulose that have been determined with synchrotron X-radiation and neutron diffrac...

Multilayer diffraction at 104 keV

NASA Technical Reports Server (NTRS)

Krieger, Allen S.; Blake, Richard L.; Siddons, D. P.

1993-01-01

We have measured the diffraction peak of a W:Si synthetic multilayer reflector at 104 keV using the High Energy Bonse-Hart Camera at the X-17B hard X-ray wiggler beam line of the National Synchrotron Light Source at Brookhaven National Laboratory. The characteristics of the diffraction peak are described and compared to theory.

Protein crystal structure from non-oriented, single-axis sparse X-ray data

DOE PAGES

Wierman, Jennifer L.; Lan, Ti-Yen; Tate, Mark W.; ...

2016-01-01

X-ray free-electron lasers (XFELs) have inspired the development of serial femtosecond crystallography (SFX) as a method to solve the structure of proteins. SFX datasets are collected from a sequence of protein microcrystals injected across ultrashort X-ray pulses. The idea behind SFX is that diffraction from the intense, ultrashort X-ray pulses leaves the crystal before the crystal is obliterated by the effects of the X-ray pulse. The success of SFX at XFELs has catalyzed interest in analogous experiments at synchrotron-radiation (SR) sources, where data are collected from many small crystals and the ultrashort pulses are replaced by exposure times that aremore » kept short enough to avoid significant crystal damage. The diffraction signal from each short exposure is so `sparse' in recorded photons that the process of recording the crystal intensity is itself a reconstruction problem. Using theEMCalgorithm, a successful reconstruction is demonstrated here in a sparsity regime where there are no Bragg peaks that conventionally would serve to determine the orientation of the crystal in each exposure. In this proof-of-principle experiment, a hen egg-white lysozyme (HEWL) crystal rotating about a single axis was illuminated by an X-ray beam from an X-ray generator to simulate the diffraction patterns of microcrystals from synchrotron radiation. Millions of these sparse frames, typically containing only ~200 photons per frame, were recorded using a fast-framing detector. It is shown that reconstruction of three-dimensional diffraction intensity is possible using theEMCalgorithm, even with these extremely sparse frames and without knowledge of the rotation angle. Further, the reconstructed intensity can be phased and refined to solve the protein structure using traditional crystallographic software. In conclusion, this suggests that synchrotron-based serial crystallography of micrometre-sized crystals can be practical with the aid of theEMCalgorithm even in cases where the data are sparse.« less

Protein crystal structure from non-oriented, single-axis sparse X-ray data

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

Wierman, Jennifer L.; Lan, Ti-Yen; Tate, Mark W.

X-ray free-electron lasers (XFELs) have inspired the development of serial femtosecond crystallography (SFX) as a method to solve the structure of proteins. SFX datasets are collected from a sequence of protein microcrystals injected across ultrashort X-ray pulses. The idea behind SFX is that diffraction from the intense, ultrashort X-ray pulses leaves the crystal before the crystal is obliterated by the effects of the X-ray pulse. The success of SFX at XFELs has catalyzed interest in analogous experiments at synchrotron-radiation (SR) sources, where data are collected from many small crystals and the ultrashort pulses are replaced by exposure times that aremore » kept short enough to avoid significant crystal damage. The diffraction signal from each short exposure is so `sparse' in recorded photons that the process of recording the crystal intensity is itself a reconstruction problem. Using theEMCalgorithm, a successful reconstruction is demonstrated here in a sparsity regime where there are no Bragg peaks that conventionally would serve to determine the orientation of the crystal in each exposure. In this proof-of-principle experiment, a hen egg-white lysozyme (HEWL) crystal rotating about a single axis was illuminated by an X-ray beam from an X-ray generator to simulate the diffraction patterns of microcrystals from synchrotron radiation. Millions of these sparse frames, typically containing only ~200 photons per frame, were recorded using a fast-framing detector. It is shown that reconstruction of three-dimensional diffraction intensity is possible using theEMCalgorithm, even with these extremely sparse frames and without knowledge of the rotation angle. Further, the reconstructed intensity can be phased and refined to solve the protein structure using traditional crystallographic software. In conclusion, this suggests that synchrotron-based serial crystallography of micrometre-sized crystals can be practical with the aid of theEMCalgorithm even in cases where the data are sparse.« less

Insights into the varnishes of historical musical instruments using synchrotron micro-analytical methods

NASA Astrophysics Data System (ADS)

Echard, J.-P.; Cotte, M.; Dooryhee, E.; Bertrand, L.

2008-07-01

Though ancient violins and other stringed instruments are often revered for the beauty of their varnishes, the varnishing techniques are not much known. In particular, very few detailed varnish analyses have been published so far. Since 2002, a research program at the Musée de la musique (Paris) is dedicated to a detailed description of varnishes on famous ancient musical instruments using a series of novel analytical methods. For the first time, results are presented on the study of the varnish from a late 16th century Venetian lute, using synchrotron micro-analytical methods. Identification of both organic and inorganic compounds distributed within the individual layers of a varnish microsample has been performed using spatially resolved synchrotron Fourier transform infrared microscopy. The univocal identification of the mineral phases is obtained through synchrotron powder X-ray diffraction. The materials identified may be of utmost importance to understand the varnishing process and its similarities with some painting techniques. In particular, the proteinaceous binding medium and the calcium sulfate components (bassanite and anhydrite) that have been identified in the lower layers of the varnish microsample could be related, to a certain extent, to the ground materials of earlier Italian paintings.

X-Ray Topography of Tetragonal Lysozyme Grown by the Temperature-Controlled Technique

NASA Technical Reports Server (NTRS)

Stojanoff, V.; Siddons, D. P.; Monaco, Lisa A.; Vekilov, Peter; Rosenberger, Franz

1997-01-01

Growth-induced defects in lysozyme crystals were observed by white-beam and monochromatic X-ray topography at the National Synchrotron Light Source (NSLS) at the Brookhaven National Laboratory (BNL). The topographic methods were non-destructive to the extent that traditional diffraction data collection could be performed to high resolution after topography. It was found that changes in growth parameters, defect concentration as detected by X-ray topography, and the diffraction quality obtainable from the crystals were all strongly correlated. In addition, crystals with fewer defects showed lower mosaicity and higher diffraction resolution as expected.

Uranium speciation as a function of depth in contaminated hanford sediments--a micro-XRF, micro-XRD, and micro- and bulk-XAFS study.

PubMed

Singer, David M; Zachara, John M; Brown, Gordon E

2009-02-01

The distribution and speciation of U and Cu in contaminated vadose zone and aquifer sediments from the U.S. DOE Hanford site (300 Area) were determined using a combination of synchrotron-based micro-X-ray fluorescence (microXRF) imaging, micro-X-ray absorption near edge structure (microXANES) spectroscopy, and micro-X-ray diffraction (microXRD) techniques combined with bulk U LIII-edge X-ray absorption fine structure (XAFS) spectroscopy. Samples were collected from within the inactive North Process Pond (NPP2) at 8 ft (2.4 m, NPP2-8) depth and 12 ft (3.7 m, NPP2-12) depth in the vadose zone, and fines were isolated from turbid groundwater just below the water Table (12-14 ft, approximately 4 m, NPP2-GW). microXRF imaging, microXRD, and microXANES spectroscopy revealed two major U occurrences within the vadose and groundwater zones: (1) low to moderate concentrations of U(VI) associated with fine-textured grain coatings that were consistently found to contain clinochlore (referred to here as chlorite) observed in all three samples, and (2) U(VI)-Cu(II) hotspots consisting of micrometer-sized particles associated with surface coatings on grains of muscovite and chlorite observed in samples NPP2-8' and NPP2-GW. In the aquifer fines (NPP2-GW), these particles were identified as cuprosklodowskite (cps: Cu[(UO2)(SiO2OH)]2 x 6H2O) and metatorbernite (mtb: Cu(UO2)2(PO4)2 x 8H2O). In contrast, the U-Cu-containing particles in the vadose zone were X-ray amorphous. Analyses of U LIII-edge XAFS spectra by linear-combination fitting indicated that U speciation consisted of (1) approximately 75% uranyl sorbed to chlorite and approximately 25% mtb-like X-ray amorphous U-Cu-phosphates (8 ft depth), (2) nearly 100% sorbed uranyl (12 ft depth), and (3) approximately 70% uranyl sorbed to chlorite and approximately 30% cps/mtb (groundwater zone). These findings suggest that dissolution of U(VI)-Cu(II)-bearing solids as well as desorption of U(VI), mainly from phyllosilicates, are important persistent sources of U(VI) to the associated uranium groundwater plume in Hanford Area 300.

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.

New frontiers in water purification: highly stable amphopolycarboxyglycinate-stabilized Ag-AgCl nanocomposite and its newly discovered potential

NASA Astrophysics Data System (ADS)

Krutyakov, Yurii A.; Zherebin, Pavel M.; Kudrinskiy, Alexey A.; Zubavichus, Yan V.; Presniakov, Mikhail Yu; Yapryntsev, Alexey D.; Karabtseva, Anastasia V.; Mikhaylov, Dmitry M.; Lisichkin, Georgii V.

2016-09-01

A simple synthetic procedure for high-stable dispersions of porous composite Ag/AgCl nanoparticles stabilized with amphoteric surfactant sodium tallow amphopolycarboxyglycinate has been proposed for the first time. The prepared samples were characterized by UV-vis spectroscopy, x-ray powder diffraction (XRD), x-ray photoelectron spectroscopy, small area electron diffraction (SAED), scanning electron microscopy (SEM), transmission electron microscopy (TEM), high-resolution transmission electron microscopy (HRTEM), and electron probe micro-analysis. In addition, measurements (carried out at the Kurchatov synchrotron radiation source stations) of the Ag K-edge extended x-ray absorption fine structure (EXAFS) and x-ray absorption near edge structure (XANES) spectra and XRD of the prepared nanoparticles have been performed. The obtained results suggest that small-sized Ag clusters are homogeneously distributed in the mass of the AgCl nanoparticle (~80 nm) formed during the synthesis. The Ag/AgCl dispersion demonstrates photocatalytic activity (with respect to methyl orange) and high bactericidal activity against E. coli. This activity is superior to the activity of both Ag and AgCl nanoparticles stabilized by the same surfactant. Thus, porous composite Ag/AgCl nanoparticles can be used as a multifunctional agent that is able to remove both pollutants and bacterium from water.

Microfabrication: LIGA-X and applications

NASA Astrophysics Data System (ADS)

Kupka, R. K.; Bouamrane, F.; Cremers, C.; Megtert, S.

2000-09-01

X-ray LIGA (Lithography, Electrogrowth, Moulding) is one of today's key technologies in microfabrication and upcoming modern (meso)-(nano) fabrication, already used and anticipated for micromechanics (micromotors, microsensors, spinnerets, etc.), micro-optics, micro-hydrodynamics (fluidic devices), microbiology, in medicine, in biology, and in chemistry for microchemical reactors. It compares to micro-electromechanical systems (MEMS) technology, offering a larger, non-silicon choice of materials and better inherent precision. X-ray LIGA relies on synchrotron radiation to obtain necessary X-ray fluxes and uses X-ray proximity printing. Inherent advantages are its extreme precision, depth of field and very low intrinsic surface roughness. However, the quality of fabricated structures often depends on secondary effects during exposure and effects like resist adhesion. UV-LIGA, relying on thick UV resists is an alternative for projects requiring less precision. Modulating the spectral properties of synchrotron radiation, different regimes of X-ray lithography lead to (a) the mass-fabrication of classical nanostructures, (b) the fabrication of high aspect ratio nanostructures (HARNST), (c) the fabrication of high aspect ratio microstructures (HARMST), and (d) the fabrication of high aspect ratio centimeter structures (HARCST). Reviewing very recent activities around X-ray LIGA, we show the versatility of the method, obviously finding its region of application there, where it is best and other competing microtechnologies are less advantageous. An example of surface-based X-ray and particle lenses (orthogonal reflection optics (ORO)) made by X-ray LIGA is given.

Phase imaging using highly coherent X-rays: radiography, tomography, diffraction topography.

PubMed

Baruchel, J; Cloetens, P; Härtwig, J; Ludwig, W; Mancini, L; Pernot, P; Schlenker, M

2000-05-01

Several hard X-rays imaging techniques greatly benefit from the coherence of the beams delivered by the modern synchrotron radiation sources. This is illustrated with examples recorded on the 'long' (145 m) ID19 'imaging' beamline of the ESRF. Phase imaging is directly related to the small angular size of the source as seen from one point of the sample ('effective divergence' approximately microradians). When using the ;propagation' technique, phase radiography and tomography are instrumentally very simple. They are often used in the 'edge detection' regime, where the jumps of density are clearly observed. The in situ damage assessment of micro-heterogeneous materials is one example of the many applications. Recently a more quantitative approach has been developed, which provides a three-dimensional density mapping of the sample ('holotomography'). The combination of diffraction topography and phase-contrast imaging constitutes a powerful tool. The observation of holes of discrete sizes in quasicrystals, and the investigation of poled ferroelectric materials, result from this combination.

In-vivo analysis of the uptake process of heavy metals through maize roots by using synchrotron X-ray fluorescence spectroscopy

NASA Astrophysics Data System (ADS)

Hwang, Bae Geun; Lee, Sang Joon; Gil, Kyehwan

2016-12-01

The uptake of heavy metals by plants has been receiving much attention for crop contamination and phytoremediation. We employed synchrotron X-ray fluorescence (XRF) spectroscopy for an in-vivo analysis of heavy-metal uptake through a strand of maize root. A focused X-ray beam of 2.5 × 2.5 μm2 in physical dimensions was scanned along horizontal lines of the maize root at intervals of 3 μm at the 4B X-ray micro-diffraction beamline of the Pohang Accelerator Laboratory (PAL). Time-resolved mapping of the fluorescence intensities from multiple metallic elements in the root tissues provided information about the radial distributions of heavy-metal elements and their temporal variations. The concentrated core stream of heavy-metal elements spread radially up to roughly 500 μm, corresponding to 40 % of the root diameter. The absorption characteristics of three heavy metals, Cr, Mn and Ni, and their physiological features were analyzed. The absolute concentrations and the contents of the heavy-metal elements in the tested maize roots were quantitatively evaluated by using the calibration curve obtained from reference samples with preset concentrations. The uptake quantities of the tested heavy-metal elements are noticeably different, although their molecular weights are similar. This study should be helpful for understanding plant physiology related with heavy-metal uptake.

Spectroscopic evidence for uranium bearing precipitates in vadose zone sediments at the Hanford 300-area site

USGS Publications Warehouse

Arai, Y.; Marcus, M.A.; Tamura, N.; Davis, J.A.; Zachara, J.M.

2007-01-01

Uranium (U) solid-state speciation in vadose zone sediments collected beneath the former North Process Pond (NPP) in the 300 Area of the Hanford site (Washington) was investigated using multi-scale techniques. In 30 day batch experiments, only a small fraction of total U (???7.4%) was released to artificial groundwater solutions equilibrated with 1% pCO2. Synchrotron-based micro-X-ray fluorescence spectroscopy analyses showed that U was distributed among at least two types of species: (i) U discrete grains associated with Cu and (ii) areas with intermediate U concentrations on grains and grain coatings. Metatorbernite (Cu[UO2]2[PO 4]2??8H2O) and uranophane (Ca[UO 2]2[SiO3(OH)]2?? 5H 2O) at some U discrete grains, and muscovite at U intermediate concentration areas, were identified in synchrotron-based micro-X-ray diffraction. Scanning electron microscopy/energy dispersive X-ray analyses revealed 8-10 ??m size metatorbernite particles that were embedded in C-, Al-, and Si-rich coatings on quartz and albite grains. In ??- and bulk-X-ray absorption structure (??-XAS and XAS) spectroscopy analyses, the structure of metatorbernite with additional U-C and U-U coordination environments was consistently observed at U discrete grains with high U concentrations. The consistency of the ??- and bulk-XAS analyses suggests that metatorbernite may comprise a significant fraction of the total U in the sample. The entrapped, micrometer-sized metatorbernite particles in C-, Al-, and Si-rich coatings, along with the more soluble precipitated uranyl carbonates and uranophane, likely control the long-term release of U to water associated with the vadose zone sediments. ?? 2007 American Chemical Society.

Imaging cellular and subcellular structure of human brain tissue using micro computed tomography

NASA Astrophysics Data System (ADS)

Khimchenko, Anna; Bikis, Christos; Schweighauser, Gabriel; Hench, Jürgen; Joita-Pacureanu, Alexandra-Teodora; Thalmann, Peter; Deyhle, Hans; Osmani, Bekim; Chicherova, Natalia; Hieber, Simone E.; Cloetens, Peter; Müller-Gerbl, Magdalena; Schulz, Georg; Müller, Bert

2017-09-01

Brain tissues have been an attractive subject for investigations in neuropathology, neuroscience, and neurobiol- ogy. Nevertheless, existing imaging methodologies have intrinsic limitations in three-dimensional (3D) label-free visualisation of extended tissue samples down to (sub)cellular level. For a long time, these morphological features were visualised by electron or light microscopies. In addition to being time-consuming, microscopic investigation includes specimen fixation, embedding, sectioning, staining, and imaging with the associated artefacts. More- over, optical microscopy remains hampered by a fundamental limit in the spatial resolution that is imposed by the diffraction of visible light wavefront. In contrast, various tomography approaches do not require a complex specimen preparation and can now reach a true (sub)cellular resolution. Even laboratory-based micro computed tomography in the absorption-contrast mode of formalin-fixed paraffin-embedded (FFPE) human cerebellum yields an image contrast comparable to conventional histological sections. Data of a superior image quality was obtained by means of synchrotron radiation-based single-distance X-ray phase-contrast tomography enabling the visualisation of non-stained Purkinje cells down to the subcellular level and automated cell counting. The question arises, whether the data quality of the hard X-ray tomography can be superior to optical microscopy. Herein, we discuss the label-free investigation of the human brain ultramorphology be means of synchrotron radiation-based hard X-ray magnified phase-contrast in-line tomography at the nano-imaging beamline ID16A (ESRF, Grenoble, France). As an example, we present images of FFPE human cerebellum block. Hard X-ray tomography can provide detailed information on human tissues in health and disease with a spatial resolution below the optical limit, improving understanding of the neuro-degenerative diseases.

Effect of Tube-Based X-Ray Microtomography Imaging on the Amino Acid and Amine Content of the Murchison CM2 Chondrite

NASA Technical Reports Server (NTRS)

Glavin, D. P.; Friedrich, J. M.; Aponte, J. C.; Dworkin, J. P.; Ebel, D. S.; Elsila, J. E.; Hill, M.; McLain, H. L.; Towbin, W. H.

2017-01-01

X-ray and synchrotron X-ray micro-computed tomography (micro-CT) are increasingly being used for three dimensional reconnaissance imaging of chondrites and returned extraterrestrial material prior to detailed chemical and mineralogical analyses. Although micro-CT imaging is generally considered to be a non-destructive technique since silicate and metallic minerals in chondrites are not affected by X-ray exposures at the intensities and wavelengths typically used, there are concerns that the use of micro-CT could be detrimental to the organics in carbonaceous chondrites. We recently conducted a synchrotron micro-CT experiment on a powdered sample of the Murchison CM2 carbonaceous chondrite exposed to a monochromatic high energy (approximately 48 kiloelectronvolts) total X-ray radiation dose of approximately 1 kilogray (kGy) using the Advanced Photon Source beamline 13-BMD (13-Bending Magnet-D Beamline) at Argonne National Laboratory and found that there were no detectable changes in the amino acid abundances or enantiomeric compositions in the chondrite after exposure relative to a Murchison control sample that was not exposed. However, lower energy bremsstrahlung X-rays could interact more with amino acids and other lower molecular weight amines in meteorites. To test for this possibility, three separate micro-CT imaging experiments of the Murchison meteorite using the GE Phoenix v/tome/x s 240 kilovolt microfocus high resolution tungsten target X-ray tube instrument at the American Museum of Natural History (AMNH) were conducted and the amino acid abundances and enantiomeric compositions were determined. We also investigated the abundances of the C1-C5 amines in Murchison which were not analyzed in the first study.

Crystal structure of pentasodium hydrogen dicitrate from synchrotron X-ray powder diffraction data and DFT comparison

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

Rammohan, Alagappa; Kaduk, James A.

2017-01-27

The crystal structure of pentasodium hydrogen dicitrate, Na 5H(C 6H 5O 7) 2, has been solved and refined using synchrotron X-ray powder diffraction data, and optimized using density functional techniques. Each of the two independent citrate anions is joined into a dimer by very strong centrosymmetric O—H...O hydrogen bonds, with O...O distances of 2.419 and 2.409 Å. Four octahedrally coordinated Na +ions share edges to form open layers parallel to theabplane. A fifth Na +ion in trigonal–bipyramidal coordination shares faces with NaO 6octahedra on both sides of these layers.

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.

Erratum to: Psammoma bodies in two types of human ovarian tumours: a mineralogical study

NASA Astrophysics Data System (ADS)

Meng, Fanlu; Wang, Changqiu; Li, Yan; Lu, Anhuai; Mei, Fang; Liu, Jianying; Du, Jingyun; Zhang, Yan

2015-06-01

Psammoma body (PB) is a common form of calcification in pathological diagnosis and closely relevant to tumours. This paper focuses on the mineralogical characteristics of PBs in ovarian serous cancer and teratoma by using polarization microscope (POM), environmental scanning electron microscope (ESEM), micro-Fourier transform infrared spectroscopy (micro-FT-IR), transmission electron microscope (TEM), micro-area synchrotron radiation X-ray powder diffraction (μ-SRXRD) and fluorescence (μ-SRXRF). Both the PBs in tissues and separated from eight typical cases were investigated. POM and ESEM observation revealed the inside-out growth pattern of PBs. μ-SRXRD and micro-FT-IR results demonstrated the dominant mineral phase of PBs in ovarian serous cancer and teratoma was AB-type carbonate hydroxyapatite (Ca10[(PO4)6-x-y(CO3)x(HPO4)y][(OH)2-u(CO3)u] with 0 ≤ x,y,u ≤ 2). As observed by ESEM and TEM, the layer-rich PBs in teratoma were up to 70 μm and mainly consisted of 5 nm-wide, 5-12 nm-long columnar crystals; the PBs in ovarian serous cancer with a maximum diameter of 35 μm were composed of slightly longer columnar crystals and granulates with 20-100 nm in diameter. The selected area electron diffraction patterns showed dispersed polycrystalline diffraction rings with arching behavior of (002) diffraction, indicating the aggregated nanocrystals grew in the preferred orientation of (002) face. The EDX and μ-SRXRF results together indicated the existence of Na, Mg, Zn and Sr in PBs. These detailed mineralogical characteristics may help uncover the nature of the pathological PBs in ovary.

Psammoma bodies in two types of human ovarian tumours: a mineralogical study

NASA Astrophysics Data System (ADS)

Fanlu, Meng; Changqiu, Wang; Yan, Li; Anhuai, Lu; Fang, Mei; Jianying, Liu; Jingyun, Du; Yan, Zhang

2015-06-01

Psammoma body (PB) is a common form of calcification in pathological diagnosis and closely relevant to tumours. This paper focuses on the mineralogical characteristics of PBs in ovarian serous cancer and teratoma by using polarization microscope (POM), environmental scanning electron microscope (ESEM), micro-Fourier transform infrared spectroscopy (micro-FT-IR), transmission electron microscope (TEM), micro-area synchrotron radiation X-ray powder diffraction (μ-SRXRD) and fluorescence (μ-SRXRF). Both the PBs in tissues and separated from eight typical cases were investigated. POM and ESEM observation revealed the inside-out growth pattern of PBs. μ-SRXRD and micro-FT-IR results demonstrated the dominant mineral phase of PBs in ovarian serous cancer and teratoma was AB-type carbonate hydroxyapatite (Ca10[(PO4)6-x-y(CO3)x(HPO4 2-)y][(OH)2-u(CO3)u] with 0 ≤ x,y,u ≤ 2). As observed by ESEM and TEM, the layer-rich PBs in teratoma were up to 70 μm and mainly consisted of 5 nm-wide, 5-12 nm-long columnar crystals; the PBs in ovarian serous cancer with a maximum diameter of 35 μm were composed of slightly longer columnar crystals and granulates with 20-100 nm in diameter. The selected area electron diffraction patterns showed dispersed polycrystalline diffraction rings with arching behavior of (002) diffraction, indicating the aggregated nanocrystals grew in the preferred orientation of (002) face. The EDX and μ-SRXRF results together indicated the existence of Na, Mg, Zn and Sr in PBs. These detailed mineralogical characteristics may help uncover the nature of the pathological PBs in ovary.

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.

High-pressure Irreversible Amorphization of La1/3NbO3

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

I Halevy; A Hen; A Broide

2011-12-31

The crystallographic structure of La{sub 1/3}NbO{sub 3} perovskite was studied at high pressures using a diamond-anvil cell and synchrotron radiation. High-pressure energy dispersive (EDS) x-ray diffraction and high-pressure angle dispersive (ADS) x-ray diffraction revealed an irreversible amorphization at {approx}10 GPa. A large change in the bulk modulus accompanied the high-pressure amorphization.

Spatial distribution of crystalline corrosion products formed during corrosion of stainless steel in concrete

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

Serdar, Marijana; Meral, Cagla; Kunz, Martin

2015-05-15

The mineralogy and spatial distribution of nano-crystalline corrosion products that form in the steel/concrete interface were characterized using synchrotron X-ray micro-diffraction (μ-XRD). Two types of low-nickel high-chromium reinforcing steels embedded into mortar and exposed to NaCl solution were investigated. Corrosion in the samples was confirmed by electrochemical impedance spectroscopy (EIS). μ-XRD revealed that goethite (α-FeOOH) and akaganeite (β-FeOOH) are the main iron oxide–hydroxides formed during the chloride-induced corrosion of stainless steel in concrete. Goethite is formed closer to the surface of the steel due to the presence of chromium in the steel, while akaganeite is formed further away from themore » surface due to the presence of chloride ions. Detailed microstructural analysis is shown and discussed on one sample of each type of steel. - Highlights: • Synchrotron micro-diffraction used to map the distribution of crystalline phases. • Goethite and akaganeite are the main corrosion products during chloride induced corrosion in mortar. • Layers of goethite and akaganeite are negatively correlated. • EDS showed Cr present in corrosion products identified by SEM.« 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.

Structure of nanocrystalline calcium silicate hydrates: insights from X-ray diffraction, synchrotron X-ray absorption and nuclear magnetic resonance

PubMed Central

Grangeon, Sylvain; Claret, Francis; Roosz, Cédric; Sato, Tsutomu; Gaboreau, Stéphane; Linard, Yannick

2016-01-01

The structure of nanocrystalline calcium silicate hydrates (C–S–H) having Ca/Si ratios ranging between 0.57 ± 0.05 and 1.47 ± 0.04 was studied using an electron probe micro-analyser, powder X-ray diffraction, 29Si magic angle spinning NMR, and Fourier-transform infrared and synchrotron X-ray absorption spectroscopies. All samples can be described as nanocrystalline and defective tobermorite. At low Ca/Si ratio, the Si chains are defect free and the Si Q 3 and Q 2 environments account, respectively, for up to 40.2 ± 1.5% and 55.6 ± 3.0% of the total Si, with part of the Q 3 Si being attributable to remnants of the synthesis reactant. As the Ca/Si ratio increases up to 0.87 ± 0.02, the Si Q 3 environment decreases down to 0 and is preferentially replaced by the Q 2 environment, which reaches 87.9 ± 2.0%. At higher ratios, Q 2 decreases down to 32.0 ± 7.6% for Ca/Si = 1.38 ± 0.03 and is replaced by the Q 1 environment, which peaks at 68.1 ± 3.8%. The combination of X-ray diffraction and NMR allowed capturing the depolymerization of Si chains as well as a two-step variation in the layer-to-layer distance. This latter first increases from ∼11.3 Å (for samples having a Ca/Si ratio <∼0.6) up to 12.25 Å at Ca/Si = 0.87 ± 0.02, probably as a result of a weaker layer-to-layer connectivity, and then decreases down to 11 Å when the Ca/Si ratio reaches 1.38 ± 0.03. The decrease in layer-to-layer distance results from the incorporation of interlayer Ca that may form a Ca(OH)2-like structure, nanocrystalline and intermixed with C–S–H layers, at high Ca/Si ratios. PMID:27275135

X-Ray Crystallographic Studies on Acetylcholinesterase and on Its Interaction with Anticholinesterase Agents.

DTIC Science & Technology

1994-11-24

complexes with reversible ligands, including edrophonium, d-tubocurarine and huperzine A , diffracting to similar resolution. The X26c Laue beam line...The EMBL-DESY synchrotron facility at Hamburg was employed to collect a complete 2.3 A data set for a crystal of native Torpedo AChE, as well as for...at the NSLS synchrotron facility at Brookhaven National Laboratory (BNL) was used to obtain a Laue diffraction pattern for a crystal of native Torpedo

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

Human insulin polymorphism upon ligand binding and pH variation: the case of 4-ethylresorcinol.

PubMed

Fili, S; Valmas, A; Norrman, M; Schluckebier, G; Beckers, D; Degen, T; Wright, J; Fitch, A; Gozzo, F; Giannopoulou, A E; Karavassili, F; Margiolaki, I

2015-09-01

This study focuses on the effects of the organic ligand 4-ethylresorcinol on the crystal structure of human insulin using powder X-ray crystallography. For this purpose, systematic crystallization experiments have been conducted in the presence of the organic ligand and zinc ions within the pH range 4.50-8.20, while observing crystallization behaviour around the isoelectric point of insulin. High-throughput crystal screening was performed using a laboratory X-ray diffraction system. The most representative samples were selected for synchrotron X-ray diffraction measurements, which took place at the European Synchrotron Radiation Facility (ESRF) and the Swiss Light Source (SLS). Four different crystalline polymorphs have been identified. Among these, two new phases with monoclinic symmetry have been found, which are targets for the future development of microcrystalline insulin drugs.

Human insulin polymorphism upon ligand binding and pH variation: the case of 4-ethylresorcinol

PubMed Central

Fili, S.; Valmas, A.; Norrman, M.; Schluckebier, G.; Beckers, D.; Degen, T.; Wright, J.; Fitch, A.; Gozzo, F.; Giannopoulou, A. E.; Karavassili, F.; Margiolaki, I.

2015-01-01

This study focuses on the effects of the organic ligand 4-ethylresorcinol on the crystal structure of human insulin using powder X-ray crystallography. For this purpose, systematic crystallization experiments have been conducted in the presence of the organic ligand and zinc ions within the pH range 4.50–8.20, while observing crystallization behaviour around the isoelectric point of insulin. High-throughput crystal screening was performed using a laboratory X-ray diffraction system. The most representative samples were selected for synchrotron X-ray diffraction measurements, which took place at the European Synchrotron Radiation Facility (ESRF) and the Swiss Light Source (SLS). Four different crystalline polymorphs have been identified. Among these, two new phases with monoclinic symmetry have been found, which are targets for the future development of microcrystalline insulin drugs. PMID:26306195

Instrumentation on Multi-Scaled Scattering of Bio-Macromolecular Solutions

PubMed Central

Chu, Benjamin; Fang, Dufei; Mao, Yimin

2015-01-01

The design, construction and initial tests on a combined laser light scattering and synchrotron X-ray scattering instrument can cover studies of length scales from atomic sizes in Angstroms to microns and dynamics from microseconds to seconds are presented. In addition to static light scattering (SLS), dynamic light scattering (DLS), small angle X-ray scattering (SAXS) and wide angle X-ray diffraction (WAXD), the light scattering instrument is being developed to carry out studies in mildly turbid solutions, in the presence of multiple scattering. Three-dimensional photon cross correlation function (3D-PCCF) measurements have been introduced to couple with synchrotron X-ray scattering to study the structure, size and dynamics of macromolecules in solution. PMID:25946340

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

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

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.

Crystal structure and density of helium to 232 kbar

NASA Technical Reports Server (NTRS)

Mao, H. K.; Wu, Y.; Jephcoat, A. P.; Hemley, R. J.; Bell, P. M.; Bassett, W. A.

1988-01-01

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

Diffraction and Transmission Synchrotron Imaging at the German Light Source ANKA--Potential Industrial Applications

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

Rack, Alexander; Weitkamp, Timm; European Synchrotron Radiation Facility, BP 220, F-38043 Grenoble Cedex

2009-03-10

Diffraction and transmission synchrotron imaging methods have proven to be highly suitable for investigations in materials research and non-destructive evaluation. The high flux and spatial coherence of X-rays from modern synchrotron light sources allows one to work using high resolution and different contrast modalities. This article gives a short overview of different transmission and diffraction imaging methods with high potential for industrial applications, now available for commercial access via the German light source ANKA (Forschungszentrum Karlsruhe) and its new department ANKA Commercial Service (ANKA COS, http://www.anka-cos.de)

Live small-animal X-ray lung velocimetry and lung micro-tomography at the Australian Synchrotron Imaging and Medical Beamline.

PubMed

Murrie, Rhiannon P; Morgan, Kaye S; Maksimenko, Anton; Fouras, Andreas; Paganin, David M; Hall, Chris; Siu, Karen K W; Parsons, David W; Donnelley, Martin

2015-07-01

The high flux and coherence produced at long synchrotron beamlines makes them well suited to performing phase-contrast X-ray imaging of the airways and lungs of live small animals. Here, findings of the first live-animal imaging on the Imaging and Medical Beamline (IMBL) at the Australian Synchrotron are reported, demonstrating the feasibility of performing dynamic lung motion measurement and high-resolution micro-tomography. Live anaesthetized mice were imaged using 30 keV monochromatic X-rays at a range of sample-to-detector propagation distances. A frame rate of 100 frames s(-1) allowed lung motion to be determined using X-ray velocimetry. A separate group of humanely killed mice and rats were imaged by computed tomography at high resolution. Images were reconstructed and rendered to demonstrate the capacity for detailed, user-directed display of relevant respiratory anatomy. The ability to perform X-ray velocimetry on live mice at the IMBL was successfully demonstrated. High-quality renderings of the head and lungs visualized both large structures and fine details of the nasal and respiratory anatomy. The effect of sample-to-detector propagation distance on contrast and resolution was also investigated, demonstrating that soft tissue contrast increases, and resolution decreases, with increasing propagation distance. This new capability to perform live-animal imaging and high-resolution micro-tomography at the IMBL enhances the capability for investigation of respiratory diseases and the acceleration of treatment development in Australia.

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

PREFACE: 22nd International Congress on X-Ray Optics and Microanalysis

NASA Astrophysics Data System (ADS)

Falkenberg, Gerald; Schroer, Christian G.

2014-04-01

ICXOM22 The 22nd edition of the International Congress on X-ray Optics and Microanalysis (ICXOM 22) was held from 2-6 September 2013, in Hamburg, Germany. The congress was organized by scientists from DESY in collaboration with TU Dresden and Helmholtz-Zentrum Geesthacht, who also formed the scientific advisory board. The congress was hosted in the historical lecture hall building of the University of Hamburg located in the city center. ICXOM22 was attended by about 210 registered participants, including 67 students, and was open for listeners. The attendance was split between 26 countries (Germany 120, rest of Europe 57, America 20, Asia 8, Australia 6). The ICXOM series is a forum for the discussion of new developments in instrumentation, methods and applications in the fields of micro- and nano-analysis by means of X-ray beams. Following the trend of the last 10 years, the conference focusses more and more on synchrotron radiation rather than X-ray laboratory sources. Besides micro-beam X-ray fluorescence and absorption spectroscopy, different methods based on diffraction and full-field imaging were covered. Newly introduced to the ICXOM series was scanning coherent X-ray diffraction imaging, which was shown to evolve into a mature method for the imaging of nanostructures, defects and strain fields. New developments on fast X-ray detectors were discussed (Lambda, Maia) and advances in X-ray optics — like the generation of a sub 5nm point focus by Multilayer Zone plates — were presented. Talks on micro- and nano-analysis applications were distributed in special sessions on bio-imaging, Earth and environmental sciences, and Cultural heritage. The congress featured nine keynote and ten plenary talks, 56 talks in 14 parallel sessions and about 120 posters in three afternoon sessions. Seventeen commercial exhibitors exposed related X-ray instrumentation products, and two luncheon seminars on detector electronics were given. This allowed us to keep the student fees low and to distribute eight student travel grants. The Wednesday was devoted to an outing to DESY with guided tours to PETRA III and FLASH experiments and to the European XFEL construction site. A lecture was given by Henry Chapman introducing to structural imaging at X-ray free-electron lasers. Talks highlighting the current status and future of nanoanalysis at the leading synchrotron facilities APS (J Maser), ESRF (P Cloetens) and SPRing8 (Ishikawa) were given in the DESY auditorium offering other DESY scientists the opportunity to follow the talks. Participants A higher quality version of this image is available in supplementary data Further information about ICXOM22, including a detailed program and electronic abstract book, can be found on the congress website www.icxom22.de. We thank all the participants of ICXOM22, everybody who helped in the organization and are looking forward to hearing about further progress during ICXOM23, which will be organized by Brookhaven National Laboratory in Uptown, New York. Gerald Falkenberg ICXOM22 conference chair Christian Schroer ICXOM22 co-chair

Resonance energy shifts during nuclear Bragg diffraction of x rays

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

Arthur, J.; Brown, G.S.; Brown, D.E.

1989-10-09

We have observed dramatic changes in the time distribution of synchrotron x rays resonantly scattered from {sup 57}Fe nuclei in a crystal of yttrium iron garnet, which depend on the deviation angle of the incident radiation from the Bragg angle. These changes are caused by small shifts in the effective energies of the hyperfine-split nuclear resonances, an effect of dynamical diffraction for the coherently excited nuclei in the crystal. The very high brightness of the synchro- tron x-ray source allows this effect to be observed in a 15-min measurement.

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

Synchrotron-radiation X-ray diffraction evidence of the emergence of ferroelectricity in LiTaO3 by ordering of a disordered Li ion in the polar direction

NASA Astrophysics Data System (ADS)

Zhang, Zhi-Gang; Abe, Tomohiro; Moriyoshi, Chikako; Tanaka, Hiroshi; Kuroiwa, Yoshihiro

2018-07-01

Synchrotron-radiation X-ray diffraction studies as a function of temperature reveal the structural origin of the spontaneous polarization and related lattice strains in stoichiometric LiTaO3. Electron charge density distribution maps visualized by the maximum entropy method clearly demonstrate that ordering of the disordered Li ion in the polar direction accompanied by deformation of the oxygen octahedra lead to the ferroelectric phase transition. The ionic polarization attributed to the ionic displacements is dominant in the polar structure. The structural change occurs continuously at the phase transition temperature, which suggests a second-order phase transition.

Determination of elemental distribution in green micro-algae using synchrotron radiation nano X-ray fluorescence (SR-nXRF) and electron microscopy techniques--subcellular localization and quantitative imaging of silver and cobalt uptake by Coccomyxa actinabiotis.

PubMed

Leonardo, T; Farhi, E; Boisson, A-M; Vial, J; Cloetens, P; Bohic, S; Rivasseau, C

2014-02-01

The newly discovered unicellular micro-alga Coccomyxa actinabiotis proves to be highly radio-tolerant and strongly concentrates radionuclides, as well as large amounts of toxic metals. This study helps in the understanding of the mechanisms involved in the accumulation and detoxification of silver and cobalt. Elemental distribution inside Coccomyxa actinabiotis cells was determined using synchrotron nano X-ray fluorescence spectroscopy at the ID22 nano fluorescence imaging beamline of the European Synchrotron Radiation Facility. The high resolution and high sensitivity of this technique enabled the assessment of elemental associations and exclusions in subcellular micro-algae compartments. A quantitative treatment of the scans was implemented to yield absolute concentrations of each endogenous and exogenous element with a spatial resolution of 100 nm and compared to the macroscopic content in cobalt and silver determined using inductively coupled plasma-mass spectrometry. The nano X-ray fluorescence imaging was complemented by transmission electron microscopy coupled to X-ray microanalysis (TEM-EDS), yielding differential silver distribution in the cell wall, cytosol, nucleus, chloroplast and mitochondria with unique resolution. The analysis of endogenous elements in control cells revealed that iron had a unique distribution; zinc, potassium, manganese, molybdenum, and phosphate had their maxima co-localized in the same area; and sulfur, copper and chlorine were almost homogeneously distributed among the whole cell. The subcellular distribution and quantification of cobalt and silver in micro-alga, assessed after controlled exposure to various concentrations, revealed that exogenous metals were mainly sequestered inside the cell rather than on mucilage or the cell wall, with preferential compartmentalization. Cobalt was homogeneously distributed outside of the chloroplast. Silver was localized in the cytosol at low concentration and in the whole cell excluding the nucleus at high concentration. Exposure to low concentrations of cobalt or silver did not alter the localization nor the concentration of endogenous elements within the cells. To our knowledge, this is the first report on element co-localization and segregation at the sub-cellular level in micro-algae by means of synchrotron nano X-ray fluorescence spectroscopy.

Applications of a pnCCD detector coupled to columnar structure CsI(Tl) scintillator system in ultra high energy X-ray Laue diffraction

NASA Astrophysics Data System (ADS)

Shokr, M.; Schlosser, D.; Abboud, A.; Algashi, A.; Tosson, A.; Conka, T.; Hartmann, R.; Klaus, M.; Genzel, C.; Strüder, L.; Pietsch, U.

2017-12-01

Most charge coupled devices (CCDs) are made of silicon (Si) with typical active layer thicknesses of several microns. In case of a pnCCD detector the sensitive Si thickness is 450 μm. However, for silicon based detectors the quantum efficiency for hard X-rays drops significantly for photon energies above 10 keV . This drawback can be overcome by combining a pixelated silicon-based detector system with a columnar scintillator. Here we report on the characterization of a low noise, fully depleted 128×128 pixels pnCCD detector with 75×75 μm2 pixel size coupled to a 700 μm thick columnar CsI(Tl) scintillator in the photon range between 1 keV to 130 keV . The excellent performance of the detection system in the hard X-ray range is demonstrated in a Laue type X-ray diffraction experiment performed at EDDI beamline of the BESSY II synchrotron taken at a set of several GaAs single crystals irradiated by white synchrotron radiation. With the columnar structure of the scintillator, the position resolution of the whole system reaches a value of less than one pixel. Using the presented detector system and considering the functional relation between indirect and direct photon events Laue diffraction peaks with X-ray energies up to 120 keV were efficiently detected. As one of possible applications of the combined CsI-pnCCD system we demonstrate that the accuracy of X-ray structure factors extracted from Laue diffraction peaks can be significantly improved in hard X-ray range using the combined CsI(Tl)-pnCCD system compared to a bare pnCCD.

Synchrotron Powder X-ray Diffraction Study of the Structure and Dehydration Behavior of Sepiolite

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

Post,J.; Bish, D.; Heaney, P.

2007-01-01

Rietveld refinements using synchrotron powder X-ray diffraction data were used to study the crystal structure and dehydration behavior of sepiolite from Durango, Mexico. The room-temperature (RT) sepiolite structure in air compares well with previous models but reveals an additional zeolitic H{sub 2}O site. The RT structure under vacuum retained only {approx}1/8 of the zeolitic H{sub 2}O and the volume decreased by 1.3%. Real-time, temperature-resolved synchrotron powder X-ray diffraction data and Rietveld refinements were used to investigate the behavior of the sepiolite structure from 300 to 925 K. Rietveld refinements revealed that most of the zeolitic H{sub 2}O is lost bymore » {approx}390 K, accompanied by a decrease in the a and c unit-cell parameters. Above {approx}600 K the sepiolite structure folds as one-half of the crystallographically bound H{sub 2}O is lost. Rietveld refinements of the 'anhydrous' sepiolite structure reveal that, in general, unit-cell parameters a and b and volume steadily decrease with increasing temperature; there is an obvious change in slope at {approx}820 K suggesting a phase transformation coinciding with the loss of the remaining bound H{sub 2}O molecule.« less

Single-drop optimization of protein crystallization.

PubMed

Meyer, Arne; Dierks, Karsten; Hilterhaus, Dierk; Klupsch, Thomas; Mühlig, Peter; Kleesiek, Jens; Schöpflin, Robert; Einspahr, Howard; Hilgenfeld, Rolf; Betzel, Christian

2012-08-01

A completely new crystal-growth device has been developed that permits charting a course across the phase diagram to produce crystalline samples optimized for diffraction experiments. The utility of the device is demonstrated for the production of crystals for the traditional X-ray diffraction data-collection experiment, of microcrystals optimal for data-collection experiments at a modern microbeam insertion-device synchrotron beamline and of nanocrystals required for data collection on an X-ray laser beamline.

Status of the Nanoscopium Scanning Hard X-ray Nanoprobe Beamline of Synchrotron Soleil

NASA Astrophysics Data System (ADS)

Somogyi, A.; Kewish, C. M.; Ribbens, M.; Moreno, T.; Polack, F.; Baranton, G.; Desjardins, K.; Samama, J. P.

2013-10-01

The Nanoscopium 155 m-long scanning hard X-ray nanoprobe beamline of Synchrotron Soleil (St Aubin, France) is dedicated to quantitative multi-modal 2D/3D imaging. The beamline aims to reach down to 30 nm spatial resolution in the 5-20 keV energy range. Two experimental stations working in consecutive operation mode will be dedicated to coherent diffractive imaging and scanning X-ray nanoprobe techniques. The beamline is in the construction phase, the first user experiments are expected in 2014. The main characteristics of the beamline and an overview of its status are given in this paper.

Towards protein-crystal centering using second-harmonic generation (SHG) microscopy

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

Kissick, David J.; Dettmar, Christopher M.; Becker, Michael

2013-05-01

The potential of second-harmonic generation (SHG) microscopy for automated crystal centering to guide synchrotron X-ray diffraction of protein crystals has been explored. The potential of second-harmonic generation (SHG) microscopy for automated crystal centering to guide synchrotron X-ray diffraction of protein crystals was explored. These studies included (i) comparison of microcrystal positions in cryoloops as determined by SHG imaging and by X-ray diffraction rastering and (ii) X-ray structure determinations of selected proteins to investigate the potential for laser-induced damage from SHG imaging. In studies using β{sub 2} adrenergic receptor membrane-protein crystals prepared in lipidic mesophase, the crystal locations identified by SHGmore » images obtained in transmission mode were found to correlate well with the crystal locations identified by raster scanning using an X-ray minibeam. SHG imaging was found to provide about 2 µm spatial resolution and shorter image-acquisition times. The general insensitivity of SHG images to optical scatter enabled the reliable identification of microcrystals within opaque cryocooled lipidic mesophases that were not identified by conventional bright-field imaging. The potential impact of extended exposure of protein crystals to five times a typical imaging dose from an ultrafast laser source was also assessed. Measurements of myoglobin and thaumatin crystals resulted in no statistically significant differences between structures obtained from diffraction data acquired from exposed and unexposed regions of single crystals. Practical constraints for integrating SHG imaging into an active beamline for routine automated crystal centering are discussed.« less

Theoretical calculation of coherent Laue-case conversion between x-rays and ALPs for an x-ray light-shining-through-a-wall experiment

NASA Astrophysics Data System (ADS)

Yamaji, T.; Yamazaki, T.; Tamasaku, K.; Namba, T.

2017-12-01

Single crystals have high atomic electric fields as much as 1 011 V /m , which correspond to magnetic fields of ˜103 T . These fields can be utilized to convert x-rays into axionlike particles (ALPs) coherently similar to x-ray diffraction. In this paper, we perform the first theoretical calculation of the Laue-case conversion in crystals based on the Darwin dynamical theory of x-ray diffraction. The calculation shows that the Laue-case conversion has longer interaction length than the Bragg case, and that ALPs in the keV range can be resonantly converted by tuning an incident angle of x-rays. ALPs with mass up to O (10 keV ) can be searched by light-shining-through-a-wall (LSW) experiments at synchrotron x-ray facilities.

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

Rodriguez, Jose A.; Ivanova, Magdalena I.; Sawaya, Michael R.

We report that the protein α-synuclein is the main component of Lewy bodies, the neuron-associated aggregates seen in Parkinson disease and other neurodegenerative pathologies. An 11-residue segment, which we term NACore, appears to be responsible for amyloid formation and cytotoxicity of human α-synuclein. Here we describe crystals of NACore that have dimensions smaller than the wavelength of visible light and thus are invisible by optical microscopy. As the crystals are thousands of times too small for structure determination by synchrotron X-ray diffraction, we use micro-electron diffraction to determine the structure at atomic resolution. The 1.4 Å resolution structure demonstrates thatmore » this method can determine previously unknown protein structures and here yields, to our knowledge, the highest resolution achieved by any cryo-electron microscopy method to date. The structure exhibits protofibrils built of pairs of face-to-face β-sheets. X-ray fibre diffraction patterns show the similarity of NACore to toxic fibrils of full-length α-synuclein. Finally, the NACore structure, together with that of a second segment, inspires a model for most of the ordered portion of the toxic, full-length α-synuclein fibril, presenting opportunities for the design of inhibitors of α-synuclein fibrils.« less

Time-resolved measurements of supersonic fuel sprays using synchrotron X-rays.

PubMed

Powell, C F; Yue, Y; Poola, R; Wang, J

2000-11-01

A time-resolved radiographic technique has been developed for probing the fuel distribution close to the nozzle of a high-pressure single-hole diesel injector. The measurement was made using X-ray absorption of monochromatic synchrotron-generated radiation, allowing quantitative determination of the fuel distribution in this optically impenetrable region with a time resolution of better than 1 micros. These quantitative measurements constitute the most detailed near-nozzle study of a fuel spray to date.

Explosive vessel for coupling dynamic experiments to the X-ray beam at the Advanced Photon Source

NASA Astrophysics Data System (ADS)

Owens, Charles; Sanchez, Nathaniel; Sorensen, Christian; Jensen, Brian

2017-06-01

Recent experiments at the Advanced Photon Source have been successful in coupling gun systems to the synchrotron to take advantage of the advanced X-ray diagnostics available including X-ray diffraction and X-ray phase contrast imaging (PCI) to examine matter at extreme conditions. There are many experiments that require explosive loading capabilities, e.g. detonator and initiator dynamics, small angle X-ray scattering (SAXS), ejecta formation, and explosively driven flyer experiments. The current work highlights a new explosive vessel that was designed specifically for use at a synchrotron facility with requirements to confine up to 15 grams of explosives (TNT equivalent), couple the vessel to the X-ray beam line, and reliably position samples remotely. A description of the system and capability will be provided along with the results from qualification testing to bring the system into service (LA-UR-17-21381).

GAPD: a GPU-accelerated atom-based polychromatic diffraction simulation code.

PubMed

E, J C; Wang, L; Chen, S; Zhang, Y Y; Luo, S N

2018-03-01

GAPD, a graphics-processing-unit (GPU)-accelerated atom-based polychromatic diffraction simulation code for direct, kinematics-based, simulations of X-ray/electron diffraction of large-scale atomic systems with mono-/polychromatic beams and arbitrary plane detector geometries, is presented. This code implements GPU parallel computation via both real- and reciprocal-space decompositions. With GAPD, direct simulations are performed of the reciprocal lattice node of ultralarge systems (∼5 billion atoms) and diffraction patterns of single-crystal and polycrystalline configurations with mono- and polychromatic X-ray beams (including synchrotron undulator sources), and validation, benchmark and application cases are presented.

Experimental Approaches for Solution X-Ray Scattering and Fiber Diffraction

PubMed Central

Irving, T. C.

2008-01-01

X-ray scattering and diffraction from non-crystalline systems have gained renewed interest in recent years, as focus shifts from the structural chemistry information gained by high-resolution studies to the context of structural physiology at larger length scales. Such techniques permit the study of isolated macromolecules as well as highly organized macromolecular assemblies as a whole under near-physiological conditions. Time-resolved approaches, made possible by advanced synchrotron instrumentation, add a critical dimension to many of these investigations. This article reviews experimental approaches in non-crystalline x-ray scattering and diffraction that may be used to illuminate important scientific questions such as protein/nucleic acid folding and structure-function relationships in large macromolecular assemblies. PMID:18801437

Purification, crystallization and preliminary X-ray diffraction studies of N-acetylglucosamine-phosphate mutase from Candida albicans

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

Nishitani, Yuichi; Maruyama, Daisuke; Nonaka, Tsuyoshi

2006-04-01

Preliminary X-ray diffraction studies on N-acetylglucosamine-phosphate mutase from C. albicans are reported. N-acetylglucosamine-phosphate mutase (AGM1) is an essential enzyme in the synthesis of UDP-N-acetylglucosamine (UDP-GlcNAc) in eukaryotes and belongs to the α-d-phosphohexomutase superfamily. AGM1 from Candida albicans (CaAGM1) was purified and crystallized by the sitting-drop vapour-diffusion method. The crystals obtained belong to the primitive monoclinic space group P2{sub 1}, with unit-cell parameters a = 60.2, b = 130.2, c = 78.0 Å, β = 106.7°. The crystals diffract X-rays to beyond 1.8 Å resolution using synchrotron radiation.

Submicron x-ray diffraction and its applications to problems in materials and environmental science

NASA Astrophysics Data System (ADS)

Tamura, N.; Celestre, R. S.; MacDowell, A. A.; Padmore, H. A.; Spolenak, R.; Valek, B. C.; Meier Chang, N.; Manceau, A.; Patel, J. R.

2002-03-01

The availability of high brilliance third generation synchrotron sources together with progress in achromatic focusing optics allows us to add submicron spatial resolution to the conventional century-old x-ray diffraction technique. The new capabilities include the possibility to map in situ, grain orientations, crystalline phase distribution, and full strain/stress tensors at a very local level, by combining white and monochromatic x-ray microbeam diffraction. This is particularly relevant for high technology industry where the understanding of material properties at a microstructural level becomes increasingly important. After describing the latest advances in the submicron x-ray diffraction techniques at the Advanced Light Source, we will give some examples of its application in material science for the measurement of strain/stress in metallic thin films and interconnects. Its use in the field of environmental science will also be discussed.

Amorphous boron gasket in diamond anvil cell research

NASA Astrophysics Data System (ADS)

Lin, Jung-Fu; Shu, Jinfu; Mao, Ho-kwang; Hemley, Russell J.; Shen, Guoyin

2003-11-01

Recent advances in high-pressure diamond anvil cell experiments include high-energy synchrotron x-ray techniques as well as new cell designs and gasketing procedures. The success of high-pressure experiments usually depends on a well-prepared sample, in which the gasket plays an important role. Various gasket materials such as diamond, beryllium, rhenium, and stainless steel have been used. Here we introduce amorphous boron as another gasket material in high-pressure diamond anvil cell experiments. We have applied the boron gasket for laser-heating x-ray diffraction, radial x-ray diffraction, nuclear resonant inelastic x-ray scattering, and inelastic x-ray scattering. The high shear strength of the amorphous boron maximizes the thickness of the sample chamber and increases the pressure homogeneity, improving the quality of high-pressure data. Use of amorphous boron avoids unwanted x-ray diffraction peaks and reduces the absorption of incident and x rays exiting the gasket material. The high quality of the diffraction patterns makes it possible to refine the cell parameters with powder x-ray diffraction data under high pressure and high temperature. The reactivity of boron prevents its use at high temperatures, however. When heated, boron may also react with the specimen to produce unwanted phases. The relatively porous boron starting material at ambient conditions also poses some challenges for sample preparation.

In-situ determination of metallic variation and multi-association in single particles by combining synchrotron microprobe, sequential chemical extraction and multivariate statistical analysis.

PubMed

Zhu, Yu-Min; Zhang, Hua; Fan, Shi-Suo; Wang, Si-Jia; Xia, Yi; Shao, Li-Ming; He, Pin-Jing

2014-07-15

Due to the heterogeneity of metal distribution, it is challenging to identify the speciation, source and fate of metals in solid samples at micro scales. To overcome these challenges single particles of air pollution control residues were detected in situ by synchrotron microprobe after each step of chemical extraction and analyzed by multivariate statistical analysis. Results showed that Pb, Cu and Zn co-existed as acid soluble fractions during chemical extraction, regardless of their individual distribution as chlorides or oxides in the raw particles. Besides the forms of Fe2O3, MnO2 and FeCr2O4, Fe, Mn, Cr and Ni were closely associated with each other, mainly as reducible fractions. In addition, the two groups of metals had interrelations with the Si-containing insoluble matrix. The binding could not be directly detected by micro-X-ray diffraction (μ-XRD) and XRD, suggesting their partial existence as amorphous forms or in the solid solution. The combined method on single particles can effectively determine metallic multi-associations and various extraction behaviors that could not be identified by XRD, μ-XRD or X-ray absorption spectroscopy. The results are useful for further source identification and migration tracing of heavy metals. Copyright © 2014 Elsevier B.V. All rights reserved.

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

Sun, Cheng-Jun, E-mail: cjsun@aps.anl.gov; Brewe, Dale L.; Heald, Steve M.

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 absorptionmore » near edge structure for Pr{sub 0.67}Sr{sub 0.33}MnO{sub 3} 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.« less

Monochromator for continuous spectrum x-ray radiation

DOEpatents

Staudenmann, J.L.; Liedl, G.L.

1983-12-02

A monochromator for use with synchrotron x-ray radiation comprises two diffraction means which can be rotated independently and independent means for translationally moving one diffraction means with respect to the other. The independence of the rotational and translational motions allows Bragg angles from 3.5/sup 0/ to 86.5/sup 0/, and facilitates precise and high-resolution monochromatization over a wide energy range. The diffraction means are removably mounted so as to be readily interchangeable, which allows the monochromator to be used for both non-dispersive and low dispersive.

Monochromator for continuous spectrum x-ray radiation

DOEpatents

Staudenmann, Jean-Louis; Liedl, Gerald L.

1987-07-07

A monochromator for use with synchrotron x-ray radiation comprises two diffraction means which can be rotated independently and independent means for translationally moving one diffraction means with respect to the other. The independence of the rotational and translational motions allows Bragg angles from 3.5.degree. to 86.5.degree., and facilitates precise and high-resolution monochromatization over a wide energy range. The diffraction means are removably mounted so as to be readily interchangeable, which allows the monochromator to be used for both non-dispersive and low dispersive work.

Microanalysis of iron oxidation state in iron oxides using X Ray Absorption Near Edge Structure (XANES)

NASA Technical Reports Server (NTRS)

Sutton, S. R.; Delaney, J.; Bajt, S.; Rivers, M. L.; Smith, J. V.

1993-01-01

An exploratory application of x ray absorption near edge structure (XANES) analysis using the synchrotron x ray microprobe was undertaken to obtain Fe XANES spectra on individual sub-millimeter grains in conventional polished sections. The experiments concentrated on determinations of Fe valence in a suite of iron oxide minerals for which independent estimates of the iron speciation could be made by electron microprobe analysis and x ray diffraction.

Mapping the spatial and temporal progression of human dental enamel biomineralization using synchrotron X-ray diffraction.

PubMed

Simmons, Lisa M; Montgomery, Janet; Beaumont, Julia; Davis, Graham R; Al-Jawad, Maisoon

2013-11-01

The complex biological, physicochemical process of human dental enamel formation begins in utero and for most teeth takes several years to complete. Lost enamel tissue cannot regenerate, therefore a better understanding of the spatial and temporal progression of mineralization of this tissue is needed in order to design improved in vivo mineral growth processes for regenerative dentistry and allow the possibility to grow a synthetic whole or partial tooth. Human dental enamel samples across a range of developmental stages available through archaeological collections have been used to explore the spatial and temporal progression of enamel biomineralization. Position sensitive synchrotron X-ray diffraction was used to quantify spatial and temporal variations in crystallite organization, lattice parameters and crystallite thickness at three different stages in enamel maturation. In addition X-ray microtomography was used to study mineral content distributions. An inverse correlation was found between the spatial variation in mineral content and the distribution of crystallite organization and thickness as a function of time during enamel maturation. Combined X-ray microtomography and synchrotron X-ray diffraction results show that as enamel matures the mineral content increases and the mineral density distribution becomes more homogeneous. Starting concurrently but proceeding at a slower rate, the enamel crystallites become more oriented and larger; and the crystallite organization becomes spatially more complex and heterogeneous. During the mineralization of human dental enamel, the rate of mineral formation and mineral organization are not identical. Whilst the processes start simultaneously, full mineral content is achieved earlier, and crystallite organization is slower and continues for longer. These findings provide detailed insights into mineral development in human dental enamel which can inform synthetic biomimetic approaches for the benefit of clinical dentistry. Copyright © 2013 Elsevier Ltd. All rights reserved.

Novel micro-reactor flow cell for investigation of model catalysts using in situ grazing-incidence X-ray scattering

PubMed Central

Kehres, Jan; Pedersen, Thomas; Masini, Federico; Andreasen, Jens Wenzel; Nielsen, Martin Meedom; Diaz, Ana; Nielsen, Jane Hvolbæk; Hansen, Ole

2016-01-01

The design, fabrication and performance of a novel and highly sensitive micro-reactor device for performing in situ grazing-incidence X-ray scattering experiments of model catalyst systems is presented. The design of the reaction chamber, etched in silicon on insulator (SIO), permits grazing-incidence small-angle X-ray scattering (GISAXS) in transmission through 10 µm-thick entrance and exit windows by using micro-focused beams. An additional thinning of the Pyrex glass reactor lid allows simultaneous acquisition of the grazing-incidence wide-angle X-ray scattering (GIWAXS). In situ experiments at synchrotron facilities are performed utilizing the micro-reactor and a designed transportable gas feed and analysis system. The feasibility of simultaneous in situ GISAXS/GIWAXS experiments in the novel micro-reactor flow cell was confirmed with CO oxidation over mass-selected Ru nanoparticles. PMID:26917133

A laboratory based system for laue micro x-ray diffraction.

PubMed

Lynch, P A; Stevenson, A W; Liang, D; Parry, D; Wilkins, S; Tamura, N

2007-02-01

A laboratory diffraction system capable of illuminating individual grains in a polycrystalline matrix is described. Using a microfocus x-ray source equipped with a tungsten anode and prefigured monocapillary optic, a micro-x-ray diffraction system with a 10 microm beam was developed. The beam profile generated by the ellipsoidal capillary was determined using the "knife edge" approach. Measurement of the capillary performance, indicated a beam divergence of 14 mrad and a useable energy bandpass from 5.5 to 19 keV. Utilizing the polychromatic nature of the incident x-ray beam and application of the Laue indexing software package X-Ray Micro-Diffraction Analysis Software, the orientation and deviatoric strain of single grains in a polycrystalline material can be studied. To highlight the system potential the grain orientation and strain distribution of individual grains in a polycrystalline magnesium alloy (Mg 0.2 wt % Nd) was mapped before and after tensile loading. A basal (0002) orientation was identified in the as-rolled annealed alloy; after tensile loading some grains were observed to undergo an orientation change of 30 degrees with respect to (0002). The applied uniaxial load was measured as an increase in the deviatoric tensile strain parallel to the load axis.

Cation ordering/disordering kinetics in Ba3CoNb2O9: An in situ study using synchrotron x-ray powder diffraction

NASA Astrophysics Data System (ADS)

Mallinson, P. M.; Claridge, J. B.; Rosseinsky, M. J.; Ibberson, R. M.; Wright, J. P.; Fitch, A. N.; Price, T.; Iddles, D. M.

2007-11-01

In situ synchrotron x-ray powder diffraction has been used to study the kinetics of cation ordering and disordering in the microwave dielectric electroceramic Ba3CoNb2O9 with a time resolution of 15s. The method enables the order/disorder temperature (To /d) in this material of 1430°C to be directly observed. The changes in the rate and degree of cation ordering and in the growth of ordered domains between samples ordered from standard precursor material and then subsequently reordered following an annealing period above To /d show that small changes in precursor order state and phase assemblage strongly influence the final domain size.

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.

Observation of Threading Dislocations in Ammonothermal Gallium Nitride Single Crystal Using Synchrotron X-ray Topography

NASA Astrophysics Data System (ADS)

Yao, Y.; Ishikawa, Y.; Sugawara, Y.; Takahashi, Y.; Hirano, K.

2018-04-01

Synchrotron monochromatic-beam x-ray topography observation has been performed on high-quality ammonothermal gallium nitride single crystal to evaluate threading dislocations (TD) in a nondestructive manner. Asymmetric diffractions with six equivalent g-vectors of 11-26, in addition to a symmetric diffraction with g = 0008, were applied to determine the Burgers vectors (b) of dislocations. It was found that pure edge-type TDs with \\varvec b = < {11 - 20} > /3 did not exist in the sample. A dominant proportion of TDs were of mixed type with \\varvec b = < {11 - 20} > /3 + < {0001} > , i.e., so-called c + a dislocations. Pure 1c screw dislocations with \\varvec b = < {0001} > and TDs with c-component larger than 1c were also observed.

In Situ X-ray Diffraction Studies of Li(sub x)Mn(sub 2)O(sub 4) Cathode Materials by Synchrotron X-ray Radiation

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

Yang, X. Q.; Sun, X.; Lee, S. J.

In Situ x-ray diffraction studies on Li{sub x}Mn{sub 2}O{sub 4} spinel cathode materials during charge-discharge cycles were carried out by using a synchrotron as x-ray source. Lithium rich (x = 1.03-1.06) spinel materials obtained from two different sources were studied. Three cubic phases with different lattice constants were observed during charge-discharge cycles in all the samples when a Sufficiently low charge-discharge rate (C/10) was used. There are two regions of two-phase coexistence between these three phases, indicating that both phase transitions are first order. The separation of the Bragg peaks representing these three phases varies from sample to sample andmore » also depends on the charge-discharge rate. These results show that the de-intercalation of lithium in lithium-rich spinel cathode materials proceeds through a series of phase transitions from a lithium-rich phase to a lithium-poor phase and finally to a {lambda}-MnO{sub 2} like cubic phase, rather than through a continuous lattice constant contraction in a single phase.« less

In vitro synchrotron-based radiography of micro-gap formation at the implant-abutment interface of two-piece dental implants.

PubMed

Rack, A; Rack, T; Stiller, M; Riesemeier, H; Zabler, S; Nelson, K

2010-03-01

Micro-gap formation at the implant-abutment interface of two-piece dental implants was investigated in vitro using high-resolution radiography in combination with hard X-ray synchrotron radiation. Images were taken with the specimen under different mechanical loads of up to 100 N. The aim of this investigation was to prove the existence of micro-gaps for implants with conical connections as well as to study the mechanical behavior of the mating zone of conical implants during loading. Synchrotron-based radiography in comparison with classical laboratory radiography yields high spatial resolution in combination with high contrast even when exploiting micro-sized features in highly attenuating objects. The first illustration of a micro-gap which was previously indistinguishable by laboratory methods underlines that the complex micro-mechanical behavior of implants requires further in vitro investigations where synchrotron-based micro-imaging is one of the prerequisites.

Crystallization and preliminary X-ray diffraction analysis of a novel Arg49 phospholipase A{sub 2} homologue from Zhaoermia mangshanensis venom

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

Murakami, Mário T.; Center for Applied Toxinology, CAT-CEPID, São Paulo, SP; Advanced Center for Genomics and Proteomics, UNESP-State University of São Paulo, São José do Rio Preto 15054-000

2007-07-01

A single crystal of zhaoermiatoxin with maximum dimensions of 0.2 × 0.2 × 0.5 mm was used for X-ray diffraction data collection to a resolution of 2.05 Å using synchrotron radiation and the diffraction pattern was indexed in the hexagonal space group P6{sub 4}, with unit-cell parameters a = 72.9, b = 72.9, c = 93.9 Å. Zhaoermiatoxin, an Arg49 phospholipase A{sub 2} homologue from Zhaoermia mangshanensis (formerly Trimeresurus mangshanensis, Ermia mangshanensis) venom is a novel member of the PLA{sub 2}-homologue family that possesses an arginine residue at position 49, probably arising from a secondary Lys49→Arg substitution that does notmore » alter the catalytic inactivity towards phospholipids. Like other Lys49 PLA{sub 2} homologues, zhaoermiatoxin induces oedema and strong myonecrosis without detectable PLA{sub 2} catalytic activity. A single crystal with maximum dimensions of 0.2 × 0.2 × 0.5 mm was used for X-ray diffraction data collection to a resolution of 2.05 Å using synchrotron radiation and the diffraction pattern was indexed in the hexagonal space group P6{sub 4}, with unit-cell parameters a = 72.9, b = 72.9, c = 93.9 Å.« less

Application of Synchrotron Microprobe Methods to Solid-Phase Speciation of Metals and Metalloids in House Dust

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

S Walker; H Jamieson; P Rasmussen

2011-12-31

Determination of the source and form of metals in house dust is important to those working to understand human and particularly childhood exposure to metals in residential environments. We report the development of a synchrotron microprobe technique for characterization of multiple metal hosts in house dust. We have applied X-ray fluorescence for chemical characterization and X-ray diffraction for crystal structure identification using microfocused synchrotron X-rays at a less than 10 {micro}m spot size. The technique has been evaluated by application to archived house dust samples containing elevated concentrations of Pb, Zn, and Ba in bedroom dust, and Pb and Asmore » in living room dust. The technique was also applied to a sample of soil from the corresponding garden to identify linkages between indoor and outdoor sources of metals. Paint pigments including white lead (hydrocerussite) and lithopone (wurtzite and barite) are the primary source of Pb, Zn, and Ba in bedroom dust, probably related to renovation activity in the home at the time of sampling. The much lower Pb content in the living room dust shows a relationship to the exterior soil and no specific evidence of Pb and Zn from the bedroom paint pigments. The technique was also successful at confirming the presence of chromated copper arsenate treated wood as a source of As in the living room dust. The results of the study have confirmed the utility of this approach in identifying specific metal forms within the dust.« less

Review: Serial Femtosecond Crystallography: A Revolution in Structural Biology

PubMed Central

Martin-Garcia, Jose M.; Conrad, Chelsie E.; Coe, Jesse; Roy-Chowdhury, Shatabdi; Fromme, Petra

2016-01-01

Macromolecular crystallography at synchrotron sources has proven to be the most influential method within structural biology, producing thousands of structures since its inception. While its utility has been instrumental in progressing our knowledge of structures of molecules, it suffers from limitations such as the need for large, well-diffracting crystals, and radiation damage that can hamper native structural determination. The recent advent of X-ray free electron lasers (XFELs) and their implementation in the emerging field of serial femtosecond crystallography (SFX) has given rise to a remarkable expansion upon existing crystallographic constraints, allowing structural biologists access to previously restricted scientific territory. SFX relies on exceptionally brilliant, micro-focused X-ray pulses, which are femtoseconds in duration, to probe nano/micrometer sized crystals in a serial fashion. This results in data sets comprised of individual snapshots, each capturing Bragg diffraction of single crystals in random orientations prior to their subsequent destruction. Thus structural elucidation while avoiding radiation damage, even at room temperature, can now be achieved. This emerging field has cultivated new methods for nanocrystallogenesis, sample delivery, and data processing. Opportunities and challenges within SFX are reviewed herein. PMID:27143509

Serial femtosecond crystallography: A revolution in structural biology.

PubMed

Martin-Garcia, Jose M; Conrad, Chelsie E; Coe, Jesse; Roy-Chowdhury, Shatabdi; Fromme, Petra

2016-07-15

Macromolecular crystallography at synchrotron sources has proven to be the most influential method within structural biology, producing thousands of structures since its inception. While its utility has been instrumental in progressing our knowledge of structures of molecules, it suffers from limitations such as the need for large, well-diffracting crystals, and radiation damage that can hamper native structural determination. The recent advent of X-ray free electron lasers (XFELs) and their implementation in the emerging field of serial femtosecond crystallography (SFX) has given rise to a remarkable expansion upon existing crystallographic constraints, allowing structural biologists access to previously restricted scientific territory. SFX relies on exceptionally brilliant, micro-focused X-ray pulses, which are femtoseconds in duration, to probe nano/micrometer sized crystals in a serial fashion. This results in data sets comprised of individual snapshots, each capturing Bragg diffraction of single crystals in random orientations prior to their subsequent destruction. Thus structural elucidation while avoiding radiation damage, even at room temperature, can now be achieved. This emerging field has cultivated new methods for nanocrystallogenesis, sample delivery, and data processing. Opportunities and challenges within SFX are reviewed herein. Published by Elsevier Inc.

Femtosecond X-ray coherent diffraction of aligned amyloid fibrils on low background graphene.

PubMed

Seuring, Carolin; Ayyer, Kartik; Filippaki, Eleftheria; Barthelmess, Miriam; Longchamp, Jean-Nicolas; Ringler, Philippe; Pardini, Tommaso; Wojtas, David H; Coleman, Matthew A; Dörner, Katerina; Fuglerud, Silje; Hammarin, Greger; Habenstein, Birgit; Langkilde, Annette E; Loquet, Antoine; Meents, Alke; Riek, Roland; Stahlberg, Henning; Boutet, Sébastien; Hunter, Mark S; Koglin, Jason; Liang, Mengning; Ginn, Helen M; Millane, Rick P; Frank, Matthias; Barty, Anton; Chapman, Henry N

2018-05-09

Here we present a new approach to diffraction imaging of amyloid fibrils, combining a free-standing graphene support and single nanofocused X-ray pulses of femtosecond duration from an X-ray free-electron laser. Due to the very low background scattering from the graphene support and mutual alignment of filaments, diffraction from tobacco mosaic virus (TMV) filaments and amyloid protofibrils is obtained to 2.7 Å and 2.4 Å resolution in single diffraction patterns, respectively. Some TMV diffraction patterns exhibit asymmetry that indicates the presence of a limited number of axial rotations in the XFEL focus. Signal-to-noise levels from individual diffraction patterns are enhanced using computational alignment and merging, giving patterns that are superior to those obtainable from synchrotron radiation sources. We anticipate that our approach will be a starting point for further investigations into unsolved structures of filaments and other weakly scattering objects.

Micro-X-Ray Fluorescence, Micro-X-Ray Absorption Spectroscopy, and Micro-X-Ray Diffraction Investigation of Lead Speciation after the Addition of Different Phosphorus Amendments to a Smelter-Contaminated Soil

EPA Science Inventory

The stabilization of Pb on additions of P to contaminated soils and mine spoil materials has been well documented. It is clear from the literature that different P sources result in different efficacies of Pb stabilization in the same contaminated material. We hypothesized that...

Hard X-ray irradiation of cosmic silicate analogs: structural evolution and astrophysical implications

NASA Astrophysics Data System (ADS)

Gavilan, L.; Jäger, C.; Simionovici, A.; Lemaire, J. L.; Sabri, T.; Foy, E.; Yagoubi, S.; Henning, T.; Salomon, D.; Martinez-Criado, G.

2016-03-01

Context. Protoplanetary disks, interstellar clouds, and active galactic nuclei contain X-ray-dominated regions. X-rays interact with the dust and gas present in such environments. While a few laboratory X-ray irradiation experiments have been performed on ices, X-ray irradiation experiments on bare cosmic dust analogs have been scarce up to now. Aims: Our goal is to study the effects of hard X-rays on cosmic dust analogs via in situ X-ray diffraction. By using a hard X-ray synchrotron nanobeam, we seek to simulate cumulative X-ray exposure on dust grains during their lifetime in these astrophysical environments and provide an upper limit on the effect of hard X-rays on dust grain structure. Methods: We prepared enstatite (MgSiO3) nanograins, which are analogs to cosmic silicates, via the melting-quenching technique. These amorphous grains were then annealed to obtain polycrystalline grains. These were characterized via scanning electron microscopy (SEM) and high-resolution transmission electron microscopy (HRTEM) before irradiation. Powder samples were prepared in X-ray transparent substrates and were irradiated with hard X-rays nanobeams (29.4 keV) provided by beamline ID16B of the European Synchrotron Radiation Facility (Grenoble). X-ray diffraction images were recorded in transmission mode, and the ensuing diffractograms were analyzed as a function of the total X-ray exposure time. Results: We detected the amorphization of polycrystalline silicates embedded in an organic matrix after an accumulated X-ray exposure of 6.4 × 1027 eV cm-2. Pure crystalline silicate grains (without resin) do not exhibit amorphization. None of the amorphous silicate samples (pure and embedded in resin) underwent crystallization. We analyze the evolution of the polycrystalline sample embedded in an organic matrix as a function of X-ray exposure. Conclusions: Loss of diffraction peak intensity, peak broadening, and the disappearance of discrete spots and arcs reveal the amorphization of the resin embedded (originally polycrystalline) silicate sample. We explore the astrophysical implications of this laboratory result as an upper limit to the effect of X-rays on the structure of cosmic silicates.

Speckle-based portable device for in-situ metrology of x-ray mirrors at Diamond Light Source

NASA Astrophysics Data System (ADS)

Wang, Hongchang; Kashyap, Yogesh; Zhou, Tunhe; Sawhney, Kawal

2017-09-01

For modern synchrotron light sources, the push toward diffraction-limited and coherence-preserved beams demands accurate metrology on X-ray optics. Moreover, it is important to perform in-situ characterization and optimization of X-ray mirrors since their ultimate performance is critically dependent on the working conditions. Therefore, it is highly desirable to develop a portable metrology device, which can be easily implemented on a range of beamlines for in-situ metrology. An X-ray speckle-based portable device for in-situ metrology of synchrotron X-ray mirrors has been developed at Diamond Light Source. Ultra-high angular sensitivity is achieved by scanning the speckle generator in the X-ray beam. In addition to the compact setup and ease of implementation, a user-friendly graphical user interface has been developed to ensure that characterization and alignment of X-ray mirrors is simple and fast. The functionality and feasibility of this device is presented with representative examples.

Anisotropic pyrochemical microetching of poly(tetrafluoroethylene) initiated by synchrotron radiation-induced scission of molecule bonds

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

Yamaguchi, Akinobu, E-mail: yamaguti@lasti.u-hyogo.ac.jp, E-mail: utsumi@lasti.u-hyogo.ac.jp; Kido, Hideki; Utsumi, Yuichi, E-mail: yamaguti@lasti.u-hyogo.ac.jp, E-mail: utsumi@lasti.u-hyogo.ac.jp

2016-02-01

We developed a process for micromachining polytetrafluoroethylene (PTFE): anisotropic pyrochemical microetching induced by synchrotron X-ray irradiation. X-ray irradiation was performed at room temperature. Upon heating, the irradiated PTFE substrates exhibited high-precision features. Both the X-ray diffraction peak and Raman signal from the irradiated areas of the substrate decreased with increasing irradiation dose. The etching mechanism is speculated as follows: X-ray irradiation caused chain scission, which decreased the number-average degree of polymerization. The melting temperature of irradiated PTFE decreased as the polymer chain length decreased, enabling the treated regions to melt at a lower temperature. The anisotropic pyrochemical etching process enabledmore » the fabrication of PTFE microstructures with higher precision than simultaneously heating and irradiating the sample.« less

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

Hunter, Mark S.; Yoon, Chun Hong; DeMirci, Hasan

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

Confocal depth-resolved fluorescence micro-X-ray absorption spectroscopy for the study of cultural heritage materials: a new mobile endstation at the Beijing Synchrotron Radiation Facility

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

Chen, Guang; Chu, Shengqi; Sun, Tianxi

A confocal fluorescence endstation for depth-resolved micro-X-ray absorption spectroscopy is described. A polycapillary half-lens defines the incident beam path and a second polycapillary half-lens at 90° defines the probe sample volume. An automatic alignment program based on an evolutionary algorithm is employed to make the alignment procedure efficient. This depth-resolved system was examined on a general X-ray absorption spectroscopy (XAS) beamline at the Beijing Synchrotron Radiation Facility. Sacrificial red glaze (AD 1368–1644) china was studied to show the capability of the instrument. As a mobile endstation to be applied on multiple beamlines, the confocal system can improve the function andmore » flexibility of general XAS beamlines, and extend their capabilities to a wider user community.« less

Operation of the Australian Store.Synchrotron for macromolecular crystallography

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

Meyer, Grischa R.; Aragão, David; Mudie, Nathan J.

2014-10-01

The Store.Synchrotron service, a fully functional, cloud computing-based solution to raw X-ray data archiving and dissemination at the Australian Synchrotron, is described. The Store.Synchrotron service, a fully functional, cloud computing-based solution to raw X-ray data archiving and dissemination at the Australian Synchrotron, is described. The service automatically receives and archives raw diffraction data, related metadata and preliminary results of automated data-processing workflows. Data are able to be shared with collaborators and opened to the public. In the nine months since its deployment in August 2013, the service has handled over 22.4 TB of raw data (∼1.7 million diffraction images). Severalmore » real examples from the Australian crystallographic community are described that illustrate the advantages of the approach, which include real-time online data access and fully redundant, secure storage. Discoveries in biological sciences increasingly require multidisciplinary approaches. With this in mind, Store.Synchrotron has been developed as a component within a greater service that can combine data from other instruments at the Australian Synchrotron, as well as instruments at the Australian neutron source ANSTO. It is therefore envisaged that this will serve as a model implementation of raw data archiving and dissemination within the structural biology research community.« less

Geochemical and mineralogical controls on metal(loid) mobility in the oxide zone of the Prairie Creek Deposit, NWT

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

Stavinga, Drew; Jamieson, Heather; Layton-Matthews, Daniel

2017-02-01

Prairie Creek is an unmined high grade Zn-Pb-Ag deposit in the southern Mackenzie Mountains of the Northwest Territories, located in a 320 km2 enclave surrounded by the Nahanni National Park reserve. The upper portion of the quartz-carbonate-sulphide vein mineralization has undergone extensive oxidation, forming high grade zones, rich in smithsonite (ZnCO3) and cerussite (PbCO3). This weathered zone represents a significant resource and a potential component of mine waste material. This study is focused on characterizing the geochemical and mineralogical controls on metal(loid) mobility under mine waste conditions, with particular attention to the metal carbonates as a potential source of tracemore » elements to the environment. Analyses were conducted using a combination of microanalytical techniques (electron microprobe, scanning electron microscopy with automated mineralogy, laser-ablation inductively-coupled mass spectrometry, and synchrotron-based element mapping, micro-X-ray diffraction and micro-X-ray absorbance). The elements of interest included Zn, Pb, Ag, As, Cd, Cu, Hg, Sb and Se.« less

Growth and characterization of epitaxially stabilized ceria(001) nanostructures on Ru(0001)

DOE PAGES

Flege, Jan Ingo; Hocker, Jan; Kaemena, Bjorn; ...

2016-05-03

We have studied (001) surface terminated cerium oxide nanoparticles grown on a ruthenium substrate using physical vapor deposition. Their morphology, shape, crystal structure, and chemical state are determined by low-energy electron microscopy and micro-diffraction, scanning probe microscopy, and synchrotron-based X-ray absorption spectroscopy. Square islands are identified as CeO 2 nanocrystals exhibiting a (001) oriented top facet of varying size; they have a height of about 7 to 10 nm and a side length between about 50 and 500 nm, and are terminated with a p(2 × 2) surface reconstruction. Micro-illumination electron diffraction reveals the existence of a coincidence lattice atmore » the interface to the ruthenium substrate. The orientation of the side facets of the rod-like particles is identified as (111); the square particles are most likely of cuboidal shape, exhibiting (100) oriented side facets. Lastly, the square and needle-like islands are predominantly found at step bunches and may be grown exclusively at temperatures exceeding 1000 °C.« less

Combining operando synchrotron X-ray tomographic microscopy and scanning X-ray diffraction to study lithium ion batteries

PubMed Central

Pietsch, Patrick; Hess, Michael; Ludwig, Wolfgang; Eller, Jens; Wood, Vanessa

2016-01-01

We present an operando study of a lithium ion battery combining scanning X-ray diffraction (SXRD) and synchrotron radiation X-ray tomographic microscopy (SRXTM) simultaneously for the first time. This combination of techniques facilitates the investigation of dynamic processes in lithium ion batteries containing amorphous and/or weakly attenuating active materials. While amorphous materials pose a challenge for diffraction techniques, weakly attenuating material systems pose a challenge for attenuation-contrast tomography. Furthermore, combining SXRD and SRXTM can be used to correlate processes occurring at the atomic level in the crystal lattices of the active materials with those at the scale of electrode microstructure. To demonstrate the benefits of this approach, we investigate a silicon powder electrode in lithium metal half-cell configuration. Combining SXRD and SRXTM, we are able to (i) quantify the dissolution of the metallic lithium electrode and the expansion of the silicon electrode, (ii) better understand the formation of the Li15Si4 phase, and (iii) non-invasively probe kinetic limitations within the silicon electrode. A simple model based on the 1D diffusion equation allows us to qualitatively understand the observed kinetics and demonstrates why high-capacity electrodes are more prone to inhomogeneous lithiation reactions. PMID:27324109

Combining operando synchrotron X-ray tomographic microscopy and scanning X-ray diffraction to study lithium ion batteries

NASA Astrophysics Data System (ADS)

Pietsch, Patrick; Hess, Michael; Ludwig, Wolfgang; Eller, Jens; Wood, Vanessa

2016-06-01

We present an operando study of a lithium ion battery combining scanning X-ray diffraction (SXRD) and synchrotron radiation X-ray tomographic microscopy (SRXTM) simultaneously for the first time. This combination of techniques facilitates the investigation of dynamic processes in lithium ion batteries containing amorphous and/or weakly attenuating active materials. While amorphous materials pose a challenge for diffraction techniques, weakly attenuating material systems pose a challenge for attenuation-contrast tomography. Furthermore, combining SXRD and SRXTM can be used to correlate processes occurring at the atomic level in the crystal lattices of the active materials with those at the scale of electrode microstructure. To demonstrate the benefits of this approach, we investigate a silicon powder electrode in lithium metal half-cell configuration. Combining SXRD and SRXTM, we are able to (i) quantify the dissolution of the metallic lithium electrode and the expansion of the silicon electrode, (ii) better understand the formation of the Li15Si4 phase, and (iii) non-invasively probe kinetic limitations within the silicon electrode. A simple model based on the 1D diffusion equation allows us to qualitatively understand the observed kinetics and demonstrates why high-capacity electrodes are more prone to inhomogeneous lithiation reactions.

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.

Synchrotron micro-scale measurement of metal distributions in Phragmites australis and Typha latifolia root tissue from an urban brownfield site

DOE PAGES

Feng, Huan; Qian, Yu; Gallagher, Frank J.; ...

2015-11-01

Liberty State Park in New Jersey, USA, is a “brownfield” site containing various levels of contaminants. To investigate metal uptake and distributions in plants on the brownfield site, Phragmites australis and Typha latifolia were collected in Liberty State Park during the growing season (May–September) in 2011 at two sites with the high and low metal loads, respectively. The objective of this study was to understand the metal (Fe, Mn, Cu, Pb and Zn) concentration and spatial distributions in P. australis and T. latifolia root systems with micro-meter scale resolution using synchrotron X-ray microfluorescence (μXRF) and synchrotron X-ray computed microtomography (μCMT)more » techniques. The root structure measurement by synchrotron μCMT showed that high X-ray attenuation substance appeared in the epidermis. Synchrotron μXRF measurement showed that metal concentrations and distributions in the root cross-section between epidermis and vascular tissue were statistically different. Significant correlations were found between metals (Cu, Mn, Pb and Zn) and Fe in the epidermis, implying that metals were scavenged by Fe oxides. The results from this study suggest that the expression of metal transport and accumulation within the root systems may be element specific. The information derived from this study can improve our current knowledge of the wetland plant ecological function in brownfield remediation.« less

X-ray Fluorescence Holography: Principles, Apparatus, and Applications

NASA Astrophysics Data System (ADS)

Hayashi, Kouichi; Korecki, Pawel

2018-06-01

X-ray fluorescence holography (XFH) is an atomic structure determination technique that combines the capabilities of X-ray diffraction and X-ray fluorescence spectroscopy. It provides a unique means of gaining fully three-dimensional information about the local atomic structure and lattice site positions of selected elements inside compound samples. In this work, we discuss experimental and theoretical aspects that are essential for the efficient recording and analysis of X-ray fluorescence holograms and review the most recent advances in XFH. We describe experiments performed with brilliant synchrotron radiation as well as with tabletop setups that employ conventional X-ray tubes.

Effect of thermomechanical processing on the microstructure and retained austenite stability during in situ tensile testing using synchrotron x-ray diffraction of NbMoAI TRIP steel.

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

Pereloma, E.; Zhang, L.; Liss, K.-D.

2011-06-01

In this work we compare and contrast the stability of retained austenite during tensile testing of Nb-Mo-Al transformation-induced plasticity steel subjected to different thermomechanical processing schedules. The obtained microstructures were characterised using optical metallography, transmission electron microscopy and X-ray diffraction. The transformation of retained austenite to martensite under tensile loading was observed by in-situ high energy X-ray diffraction at 1ID / APS. It has been shown that the variations in the microstructure of the steel, such as volume fractions of present phases, their morphology and dimensions, play a critical role in the strain-induced transition of retained austenite to martensite.

Spider Silks-Biomimetics Beyond Silk Fibers: Hydrogels, films & Adhesives from Aqueous Recombinant Spider Silk dopes: A Synchrotron X-Ray Nano-Structural Study

NASA Astrophysics Data System (ADS)

Sampath, Sujatha; Jones, Justin; Harris, Thomas; Lewis, Randolph

2015-03-01

With a combination of high strength and extensibility, spider silk's (SS) mechanical properties surpass those of any man made fiber. The superior properties are due to the primary protein composition and the complex hierarchical structural organization from nanoscale to macroscopic length scales. Considerable progress has been made to synthetically mimic the production of fibers based on SS proteins. We present synchrotron x-ray micro diffraction (SyXRD) results on new fibers and gels (hydrogels, lyogels) from recombinant SS protein water-soluble dopes. Novelty in these materials is two-fold: water based rather than widely used HFIP acid synthesis, makes them safe in medical applications (replacement for tendons & ligaments). Secondly, hydrogels morphology render them as excellent carriers for targeted drug delivery biomedical applications. SyXRD results reveal semi-crystalline structure with ordered beta-sheets and relatively high degree of axial orientation in the fibers, making them the closest yet to natural spider silks. SyXRD on the gels elucidate the structural transformations during the self-recovery process through mechanical removal and addition of water. Studies correlating the observed structural changes to mechanical properties are underway.

In-situ characterization of highly reversible phase transformation by synchrotron X-ray Laue microdiffraction

DOE PAGES

Chen, Xian; Tamura, Nobumichi; MacDowell, Alastair; ...

2016-05-23

The alloy Cu 25 Au 30 Zn 45 undergoes a huge first-order phase transformation (6% strain) and shows a high reversibility under thermal cycling and an unusual martensitc microstructure in sharp contrast to its nearby compositions. We discovered this alloy by systematically tuning the composition so that its lattice parameters satisfy the cofactor conditions (i.e., the kinematic conditions of compatibility between phases). It was conjectured that satisfaction of these conditions is responsible for the enhanced reversibility as well as the observed unusual fluid-like microstructure during transformation, but so far, there has been no direct evidence confirming that these observed microstructuresmore » are those predicted by the cofactor conditions. In order to verify this hypothesis, we use synchrotron X-ray Laue microdiffraction to measure the orientations and structural parameters of variants and phases near the austenite/martensite interface. The areas consisting of both austenite and multi-variants of martensite are scanned by microLaue diffraction. The cofactor conditions have been examined from the kinematic relation of lattice vectors across the interface. The continuity condition of the interface is precisely verified from the correspondent lattice vectors between two phases.« less

Rietveld Refinement on X-Ray Diffraction Patterns of Bioapatite in Human Fetal Bones

PubMed Central

Meneghini, Carlo; Dalconi, Maria Chiara; Nuzzo, Stefania; Mobilio, Settimio; Wenk, Rudy H.

2003-01-01

Bioapatite, the main constituent of mineralized tissue in mammalian bones, is a calcium-phosphate-based mineral that is similar in structure and composition to hydroxyapatite. In this work, the crystallographic structure of bioapatite in human fetuses was investigated by synchrotron radiation x-ray diffraction (XRD) and microdiffraction (μ-XRD) techniques. Rietveld refinement analyses of XRD and μ-XRD data allow for quantitative probing of the structural modifications of bioapatite as functions of the mineralization process and gestational age. PMID:12609904

Evaluating scintillator performance in time-resolved hard X-ray studies at synchrotron light sources.

PubMed

Rutherford, Michael E; Chapman, David J; White, Thomas G; Drakopoulos, Michael; Rack, Alexander; Eakins, Daniel E

2016-05-01

The short pulse duration, small effective source size and high flux of synchrotron radiation is ideally suited for probing a wide range of transient deformation processes in materials under extreme conditions. In this paper, the challenges of high-resolution time-resolved indirect X-ray detection are reviewed in the context of dynamic synchrotron experiments. In particular, the discussion is targeted at two-dimensional integrating detector methods, such as those focused on dynamic radiography and diffraction experiments. The response of a scintillator to periodic synchrotron X-ray excitation is modelled and validated against experimental data collected at the Diamond Light Source (DLS) and European Synchrotron Radiation Facility (ESRF). An upper bound on the dynamic range accessible in a time-resolved experiment for a given bunch separation is calculated for a range of scintillators. New bunch structures are suggested for DLS and ESRF using the highest-performing commercially available crystal LYSO:Ce, allowing time-resolved experiments with an interframe time of 189 ns and a maximum dynamic range of 98 (6.6 bits).

Evaluating scintillator performance in time-resolved hard X-ray studies at synchrotron light sources

PubMed Central

Rutherford, Michael E.; Chapman, David J.; White, Thomas G.; Drakopoulos, Michael; Rack, Alexander; Eakins, Daniel E.

2016-01-01

The short pulse duration, small effective source size and high flux of synchrotron radiation is ideally suited for probing a wide range of transient deformation processes in materials under extreme conditions. In this paper, the challenges of high-resolution time-resolved indirect X-ray detection are reviewed in the context of dynamic synchrotron experiments. In particular, the discussion is targeted at two-dimensional integrating detector methods, such as those focused on dynamic radiography and diffraction experiments. The response of a scintillator to periodic synchrotron X-ray excitation is modelled and validated against experimental data collected at the Diamond Light Source (DLS) and European Synchrotron Radiation Facility (ESRF). An upper bound on the dynamic range accessible in a time-resolved experiment for a given bunch separation is calculated for a range of scintillators. New bunch structures are suggested for DLS and ESRF using the highest-performing commercially available crystal LYSO:Ce, allowing time-resolved experiments with an interframe time of 189 ns and a maximum dynamic range of 98 (6.6 bits). PMID:27140147

Ice Recrystallization in a Solution of a Cryoprotector and Its Inhibition by a Protein: Synchrotron X-Ray Diffraction Study.

PubMed

Zakharov, Boris; Fisyuk, Alexander; Fitch, Andy; Watier, Yves; Kostyuchenko, Anastasia; Varshney, Dushyant; Sztucki, Michael; Boldyreva, Elena; Shalaev, Evgenyi

2016-07-01

Ice formation and recrystallization is a key phenomenon in freezing and freeze-drying of pharmaceuticals and biopharmaceuticals. In this investigation, high-resolution synchrotron X-ray diffraction is used to quantify the extent of disorder of ice crystals in binary aqueous solutions of a cryoprotectant (sorbitol) and a protein, bovine serum albumin. Ice crystals in more dilute (10 wt%) solutions have lower level of microstrain and larger crystal domain size than these in more concentrated (40 wt%) solutions. Warming the sorbitol-water mixtures from 100 to 228 K resulted in partial ice melting, with simultaneous reduction in the microstrain and increase in crystallite size, that is, recrystallization. In contrast to sorbitol solutions, ice crystals in the BSA solutions preserved both the microstrain and smaller crystallite size on partial melting, demonstrating that BSA inhibits ice recrystallization. The results are consistent with BSA partitioning into quasi-liquid layer on ice crystals but not with a direct protein-ice interaction and protein sorption on ice surface. The study shows for the first time that a common (i.e., not-antifreeze) protein can have a major impact on ice recrystallization and also presents synchrotron X-ray diffraction as a unique tool for quantification of crystallinity and disorder in frozen aqueous systems. Copyright © 2016 American Pharmacists Association®. Published by Elsevier Inc. All rights reserved.

Melting point suppression in new lanthanoid(III) ionic liquids by trapping of kinetic polymorphs: an in situ synchrotron powder diffraction study.

PubMed

Chesman, Anthony S R; Yang, Mei; Mallick, Bert; Ross, Tamsyn M; Gass, Ian A; Deacon, Glen B; Batten, Stuart R; Mudring, Anja-Verena

2012-01-04

The complexes (N(4444))(3)[Ln(dcnm)(6)] (Ln = La-Nd, Sm; N(4444) = tetrabutylammonium) display a decrease in the melting point upon fast cooling from a melt, which is shown by in situ synchrotron based X-ray powder diffraction to be due to the formation of a second, less thermodynamically stable, polymorph. This journal is © The Royal Society of Chemistry 2012

High-resolution x-ray imaging for microbiology at the Advanced Photon Source

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

Lai, B.; Kemner, K. M.; Maser, J.

1999-11-02

Exciting new applications of high-resolution x-ray imaging have emerged recently due to major advances in high-brilliance synchrotrons sources and high-performance zone plate optics. Imaging with submicron resolution is now routine with hard x-rays: the authors have demonstrated 150 run in the 6--10 keV range with x-ray microscopes at the Advanced Photon Source (APS), a third-generation synchrotrons radiation facility. This has fueled interest in using x-ray imaging in applications ranging from the biomedical, environmental, and materials science fields to the microelectronics industry. One important application they have pursued at the APS is a study of the microbiology of bacteria and theirmore » associated extracellular material (biofilms) using fluorescence microanalysis. No microscopy techniques were previously available with sufficient resolution to study live bacteria ({approx}1 {micro}m x 4 {micro}m in size) and biofilms in their natural hydrated state with better than part-per-million elemental sensitivity and the capability of determining g chemical speciation. In vivo x-ray imaging minimizes artifacts due to sample fixation, drying, and staining. This provides key insights into the transport of metal contaminants by bacteria in the environment and potential new designs for remediation and sequestration strategies.« less

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.

Sharp chemical interface in epitaxial Fe{sub 3}O{sub 4} thin films

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

Gálvez, S.; Rubio-Zuazo, J., E-mail: rubio@esrf.fr; Salas-Colera, E.

Chemically sharp interface was obtained on single phase single oriented Fe{sub 3}O{sub 4} (001) thin film (7 nm) grown on NiO (001) substrate using oxygen assisted molecular beam epitaxy. Refinement of the atomic structure, stoichiometry, and oxygen vacancies were determined by soft and hard x-ray photoelectron spectroscopy, low energy electron diffraction and synchrotron based X-ray reflectivity, and X-ray diffraction. Our results demonstrate an epitaxial growth of the magnetite layer, perfect iron stoichiometry, absence of oxygen vacancies, and the existence of an intermixing free interface. Consistent magnetic and electrical characterizations are also shown.

Synchrotron X-ray topography of electronic materials.

PubMed

Tuomi, T

2002-05-01

Large-area transmission, transmission section, large-area back-reflection, back-reflection section and grazing-incidence topography are the geometries used when recording high-resolution X-ray diffraction images with synchrotron radiation from a bending magnet, a wiggler or an undulator of an electron or a positron storage ring. Defect contrast can be kinematical, dynamical or orientational even in the topographs recorded on the same film at the same time. In this review article limited to static topography experiments, examples of defect studies on electronic materials cover the range from voids and precipitates in almost perfect float-zone and Czochralski silicon, dislocations in gallium arsenide grown by the liquid-encapsulated Czochralski technique, the vapour-pressure controlled Czochralski technique and the vertical-gradient freeze technique, stacking faults and micropipes in silicon carbide to misfit dislocations in epitaxic heterostructures. It is shown how synchrotron X-ray topographs of epitaxic laterally overgrown gallium arsenide layer structures are successfully explained by orientational contrast.

Local x-ray structure analysis of optically manipulated biological micro-objects

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

Cojoc, Dan; Ferrari, Enrico; Santucci, Silvia C.

2010-12-13

X-ray diffraction using micro- and nanofocused beams is well suited for nanostructure analysis at different sites of a biological micro-object. To conduct in vitro studies without mechanical contact, we developed object manipulation by optical tweezers in a microfluidic cell. Here we report x-ray microdiffraction analysis of a micro-object optically trapped in three dimensions. We revealed the nanostructure of a single starch granule at different points and investigated local radiation damage induced by repeated x-ray exposures at the same position, demonstrating high stability and full control of the granule orientation by multiple optical traps.

CARNAÚBA: The Coherent X-Ray Nanoprobe Beamline for the Brazilian Synchrotron SIRIUS/LNLS

NASA Astrophysics Data System (ADS)

Tolentino, Hélio C. N.; Soares, Márcio M.; Perez, Carlos A.; Vicentin, Flávio C.; Abdala, Dalton B.; Galante, Douglas; Teixeira, Verônica de C.; de Araújo, Douglas H. C.; Westfahl, Harry, Jr.

2017-06-01

The CARNAÚBA beamline is the tender-to-hard X-ray (2 - 15 keV) scanning nanoprobe planned for the 4th generation storage ring SIRIUS at the LNLS. CARNAÚBA uses an undulator source with vertical linear polarization in a low-beta straight section and grazing incidence-focusing mirrors to create a nanoprobe at 143 m from the source. The beamline optic is based on KB mirrors and provides high brilliance at an achromatic focal spot down to the diffraction limit diameter of ˜30 nm with a working distance of ˜6 cm. These characteristics are crucial for studying nanometric samples in experiments involving complex stages and environments. The CARNAÚBA beamline aims to perform raster scans using x-ray fluorescence, x-ray absorption spectroscopy, x-ray diffraction and coherent x-ray imaging techniques. Computed tomography will extend these methods to three dimensions.

Initiation and growth kinetics of solidification cracking during welding of steel

PubMed Central

Aucott, L.; Huang, D.; Dong, H. B.; Wen, S. W.; Marsden, J. A.; Rack, A.; Cocks, A. C. F.

2017-01-01

Solidification cracking is a key phenomenon associated with defect formation during welding. To elucidate the failure mechanisms, solidification cracking during arc welding of steel are investigated in situ with high-speed, high-energy synchrotron X-ray radiography. Damage initiates at relatively low true strain of about 3.1% in the form of micro-cavities at the weld subsurface where peak volumetric strain and triaxiality are localised. The initial micro-cavities, with sizes from 10 × 10−6 m to 27 × 10−6 m, are mostly formed in isolation as revealed by synchrotron X-ray micro-tomography. The growth of micro-cavities is driven by increasing strain induced to the solidifying steel. Cavities grow through coalescence of micro-cavities to form micro-cracks first and then through the propagation of micro-cracks. Cracks propagate from the core of the weld towards the free surface along the solidifying grain boundaries at a speed of 2–3 × 10−3 m s−1. PMID:28074852

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.

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.

Main functions, recent updates, and applications of Synchrotron Radiation Workshop code

NASA Astrophysics Data System (ADS)

Chubar, Oleg; Rakitin, Maksim; Chen-Wiegart, Yu-Chen Karen; Chu, Yong S.; Fluerasu, Andrei; Hidas, Dean; Wiegart, Lutz

2017-08-01

The paper presents an overview of the main functions and new application examples of the "Synchrotron Radiation Workshop" (SRW) code. SRW supports high-accuracy calculations of different types of synchrotron radiation, and simulations of propagation of fully-coherent radiation wavefronts, partially-coherent radiation from a finite-emittance electron beam of a storage ring source, and time-/frequency-dependent radiation pulses of a free-electron laser, through X-ray optical elements of a beamline. An extended library of physical-optics "propagators" for different types of reflective, refractive and diffractive X-ray optics with its typical imperfections, implemented in SRW, enable simulation of practically any X-ray beamline in a modern light source facility. The high accuracy of calculation methods used in SRW allows for multiple applications of this code, not only in the area of development of instruments and beamlines for new light source facilities, but also in areas such as electron beam diagnostics, commissioning and performance benchmarking of insertion devices and individual X-ray optical elements of beamlines. Applications of SRW in these areas, facilitating development and advanced commissioning of beamlines at the National Synchrotron Light Source II (NSLS-II), are described.

The power of in situ pulsed laser deposition synchrotron characterization for the detection of domain formation during growth of Ba0.5Sr0.5TiO3 on MgO.

PubMed

Bauer, Sondes; Lazarev, Sergey; Molinari, Alan; Breitenstein, Andreas; Leufke, Philipp; Kruk, Robert; Hahn, Horst; Baumbach, Tilo

2014-03-01

A highly sophisticated pulsed laser deposition (PLD) chamber has recently been installed at the NANO beamline at the synchrotron facility ANKA (Karlsruhe, Germany), which allows for comprehensive studies on the PLD growth process of dielectric, ferroelectric and ferromagnetic thin films in epitaxial oxide heterostructures or even multilayer systems by combining in situ reflective high-energy diffraction with the in situ synchrotron high-resolution X-ray diffraction and surface diffraction methods. The modularity of the in situ PLD chamber offers the opportunity to explore the microstructure of the grown thin films as a function of the substrate temperature, gas pressure, laser fluence and target-substrate separation distance. Ba0.5Sr0.5TiO3 grown on MgO represents the first system that is grown in this in situ PLD chamber and studied by in situ X-ray reflectivity, in situ two-dimensional reciprocal space mapping of symmetric X-ray diffraction and acquisition of time-resolved diffraction profiles during the ablation process. In situ PLD synchrotron investigation has revealed the occurrence of structural distortion as well as domain formation and misfit dislocation which all depend strongly on the film thickness. The microstructure transformation has been accurately detected with a time resolution of 1 s. The acquisition of two-dimensional reciprocal space maps during the PLD growth has the advantage of simultaneously monitoring the changes of the crystalline structure as well as the formation of defects. The stability of the morphology during the PLD growth is demonstrated to be remarkably affected by the film thickness. A critical thickness for the domain formation in Ba0.5Sr0.5TiO3 grown on MgO could be determined from the acquisition of time-resolved diffraction profiles during the PLD growth. A splitting of the diffraction peak into two distinguishable peaks has revealed a morphology change due to modification of the internal strain during growth.

Recent progress in X-ray optics at the ESRF

NASA Astrophysics Data System (ADS)

Freund, A.

2003-03-01

It is the task of x-ray optics to adapt the raw beam generated by modern sources such as synchrotron storage rings to a great variety of experimental requirements in terms of intensity, spot size, polarization and other parameters. The very high quality of synchrotron radiation (source size of a few microns and beam divergence of a few micro-radians) and the extreme x-ray flux (power of several hundred Watts in a few square mm) make this task quite difficult. In particular the heat load aspect is very important in the conditioning process of the brute x-ray power. Cryogenically cooled silicon crystals and water-cooled diamond crystals can presently fulfil this task, but limits will soon be reached and new schemes and materials must be envisioned. A major tendency of instrument improvement has a ways been to concentrate more photons into a smaller spot utilizing a whole variety of focusing devices such as Fresnel zone plates, refractive lenses and Systems based on bent surfaces, for example Kirkpatrick-Baez Systems. Apart from the resistance of the sample, the ultimate limits are determined by the source size and strength on one side, by materials properties, cooling, mounting and bending schemes on the other side, and fundamentally by the diffraction process. There is also the important aspect of coherence that can be both a nuisance and a blessing for the experiments, in particular for imaging techniques. Its conservation puts additional constraints on the quality of the optical elements. A review of recent progress in this field is given.

CMT for transport in porous media

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

Schwartz, L.

This session is comprised of an outline of uses for x-ray microtomography in the field of petroleum geology. Calculations, diagrams, and color photomicrographs depict the many applications of synchrotron x-ray microtomograpy in determining transport properties and fluid flow characteristics of reservoir rocks, micro-porosity in carbonates, and aspects of multi-phase transport.

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®.

Step-by-step fabrication of a highly oriented crystalline three-dimensional pillared-layer-type metal-organic framework thin film confirmed by synchrotron X-ray diffraction.

PubMed

Otsubo, Kazuya; Haraguchi, Tomoyuki; Sakata, Osami; Fujiwara, Akihiko; Kitagawa, Hiroshi

2012-06-13

Fabrication of a crystalline ordered thin film based on the porous metal-organic frameworks (MOFs) is one of the practical applications of the future functional nanomaterials. Here, we report the creation of a highly oriented three-dimensional (3-D) porous pillared-layer-type MOF thin film on a metal substrate using a step-by-step approach based on liquid-phase epitaxy. Synchrotron X-ray diffraction (XRD) study clearly indicates that the thin film is crystalline and its orientation is highly controlled in both horizontal and vertical directions relative to the substrate. This report provides the first confirmation of details of not only the crystallinity but also the orientation of 3-D MOF thin film using synchrotron XRD. Moreover, we also demonstrate its guest adsorption/desorption behavior by using in situ XRD measurements. The results presented here would promise useful insights for fabrication of MOF-based nanodevices in the future.

Structure determination of an integral membrane protein at room temperature from crystals in situ

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

Axford, Danny; Foadi, James; Imperial College London, London SW7 2AZ

2015-05-14

The X-ray structure determination of an integral membrane protein using synchrotron diffraction data measured in situ at room temperature is demonstrated. The structure determination of an integral membrane protein using synchrotron X-ray diffraction data collected at room temperature directly in vapour-diffusion crystallization plates (in situ) is demonstrated. Exposing the crystals in situ eliminates manual sample handling and, since it is performed at room temperature, removes the complication of cryoprotection and potential structural anomalies induced by sample cryocooling. Essential to the method is the ability to limit radiation damage by recording a small amount of data per sample from many samplesmore » and subsequently assembling the resulting data sets using specialized software. The validity of this procedure is established by the structure determination of Haemophilus influenza TehA at 2.3 Å resolution. The method presented offers an effective protocol for the fast and efficient determination of membrane-protein structures at room temperature using third-generation synchrotron beamlines.« 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

Zinc speciation in proximity to phosphate application points in a lead/zinc smelter-contaminated soil.

PubMed

Baker, Lucas R; Pierzynski, Gary M; Hettiarachchi, Ganga M; Scheckel, Kirk G; Newville, Matthew

2012-01-01

The use of P to immobilize Pb in contaminated soils has been well documented. However, the influence of P on Zn speciation in soils has not been extensively examined, and these two metals often occur as co-contaminants. We hypothesized that additions of P to a Pb/Zn-contaminated soil would induce Zn phosphate mineral formation and fluid P sources would be more effective than granular P amendments. A combination of different synchrotron-based techniques, namely, spatially resolved micro-X-ray fluorescence (μ-XRF), micro-extended X-ray absorption fine structure spectroscopy (μ-EXAFS), and micro-X-ray diffraction (μ-XRD), were used to speciate Zn at two incubation times in the proximity of application points (0 to 4 mm) for fluid and granular P amendments in a Pb/Zn smelter-contaminated soil. Phosphate rock (PR), triple super phosphate (TSP), monoammonium phosphate (MAP), and fluid ammonium polyphosphate induced Zn phosphate formation. Ammonium polyphosphate was more effective at greater distances (up to 3.7 mm) from the point of P application. Phosphoric acid increased the presence of soluble Zn species because of increased acidity. Soluble Zn has implications with respect to Zn bioavailability, which may negatively impact vegetation and other sensitive organisms. Although additions of P immobilize Pb, this practice needs close monitoring due to potential increases in Zn solubility in a Pb/Zn smelter-contaminated soil. Copyright © by the American Society of Agronomy, Crop Science Society of America, and Soil Science Society of America, Inc.

High spatial resolution grain orientation and strain mapping in thin films using polychromatic submicron x-ray diffraction

NASA Astrophysics Data System (ADS)

Tamura, N.; MacDowell, A. A.; Celestre, R. S.; Padmore, H. A.; Valek, B.; Bravman, J. C.; Spolenak, R.; Brown, W. L.; Marieb, T.; Fujimoto, H.; Batterman, B. W.; Patel, J. R.

2002-05-01

The availability of high brilliance synchrotron sources, coupled with recent progress in achromatic focusing optics and large area two-dimensional detector technology, has allowed us to develop an x-ray synchrotron technique that is capable of mapping orientation and strain/stress in polycrystalline thin films with submicron spatial resolution. To demonstrate the capabilities of this instrument, we have employed it to study the microstructure of aluminum thin film structures at the granular and subgranular levels. Due to the relatively low absorption of x-rays in materials, this technique can be used to study passivated samples, an important advantage over most electron probes given the very different mechanical behavior of buried and unpassivated materials.

High-energy synchrotron x-ray techniques for studying irradiated materials

DOE PAGES

Park, Jun-Sang; Zhang, Xuan; Sharma, Hemant; ...

2015-03-20

High performance materials that can withstand radiation, heat, multiaxial stresses, and corrosive environment are necessary for the deployment of advanced nuclear energy systems. Nondestructive in situ experimental techniques utilizing high energy x-rays from synchrotron sources can be an attractive set of tools for engineers and scientists to investigate the structure–processing–property relationship systematically at smaller length scales and help build better material models. In this paper, two unique and interconnected experimental techniques, namely, simultaneous small-angle/wide-angle x-ray scattering (SAXS/WAXS) and far-field high-energy diffraction microscopy (FF-HEDM) are presented. Finally, the changes in material state as Fe-based alloys are heated to high temperatures ormore » subject to irradiation are examined using these techniques.« less

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

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

Shen, Guoyin; Mao, Ho Kwang

2016-11-22

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. Thesemore » 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.« less

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.

Structure of the toxic core of α-synuclein from invisible crystals

DOE PAGES

Rodriguez, Jose A.; Ivanova, Magdalena I.; Sawaya, Michael R.; ...

2015-09-09

We report that the protein α-synuclein is the main component of Lewy bodies, the neuron-associated aggregates seen in Parkinson disease and other neurodegenerative pathologies. An 11-residue segment, which we term NACore, appears to be responsible for amyloid formation and cytotoxicity of human α-synuclein. Here we describe crystals of NACore that have dimensions smaller than the wavelength of visible light and thus are invisible by optical microscopy. As the crystals are thousands of times too small for structure determination by synchrotron X-ray diffraction, we use micro-electron diffraction to determine the structure at atomic resolution. The 1.4 Å resolution structure demonstrates thatmore » this method can determine previously unknown protein structures and here yields, to our knowledge, the highest resolution achieved by any cryo-electron microscopy method to date. The structure exhibits protofibrils built of pairs of face-to-face β-sheets. X-ray fibre diffraction patterns show the similarity of NACore to toxic fibrils of full-length α-synuclein. Finally, the NACore structure, together with that of a second segment, inspires a model for most of the ordered portion of the toxic, full-length α-synuclein fibril, presenting opportunities for the design of inhibitors of α-synuclein fibrils.« less

Synchrotron Powder X-ray Diffraction Study of the Structure and Dehydration Behavior of Sepiolite

NASA Astrophysics Data System (ADS)

Post, J. E.; Bish, D. L.; Heaney, P. J.

2006-05-01

Sepiolite is a hydrous Mg-silicate clay mineral with fibrous morphology that typically occurs as fine-grained, poorly crystalline masses. It occurs in a wide variety of geological environments and has been mined for centuries because of its many uses, e.g. in the pharmaceutical, fertilizer, and pesticide industries. Its versatile functionality derives from the large surface area and microporosity that are characteristic of the material. In recent years, sepiolite has received considerable attention with regard to the adsorption of organics, for use as a support for catalysts, as a molecular sieve, and as an inorganic membrane for ultrafiltration. Because of its fine-grained and poorly crystalline nature, it has not been possible to study sepiolite's crystal structure using single-crystal X-ray diffraction methods, and consequently many details of the structure are still not well known. In this study, Rietveld refinements using synchrotron powder X-ray diffraction data were used to investigate the crystal structure and dehydration behavior of sepiolite from Durango, Mexico. The room- temperature (RT) sepiolite structure in air compares well with previous models but reveals an additional zeolitic water site. The RT structure under vacuum retained only ~1/8 of the zeolitic water and the volume decreased 1.3%. Real-time, temperature-resolved synchrotron powder X-ray diffraction data and Rietveld refinements were used to investigate the behavior of the sepiolite structure from 300 to 925 K. Rietveld refinements revealed that most of the zeolitic water is lost by ~390 K, accompanied by a decrease in the a and c unit-cell parameters. Above ~600 K the sepiolite structure folds as one-half of the crystallographically bound water is lost. Rietveld refinements of the "anhydrous" sepiolite structure reveal that, in general, unit-cell parameters a, b, â and volume steadily decrease with increasing temperature; there is an obvious change in slope at ~820 K suggesting a phase transformation coinciding with the loss of the remaining bound water molecule. These temperature-resolved real-time powder X-ray diffraction studies provide the first comprehensive description of the sepiolite structure and the complex changes it undergoes as it dehydrates. Additional heating and cooling in situ powder X-ray diffraction experiments are underway in order to investigate the relative stabilities and rehydration behaviors of the partially-hydrated sepiolite phases. The results of these studies should provide a more robust model for predicting and modifying the properties and applications of this critical industrial material and environmentally important mineral.

Study of gold nanoparticle synthesis by synchrotron x-ray diffraction and fluorescence

NASA Astrophysics Data System (ADS)

Yan, Zhongying; Wang, Xiao; Yu, Le; Moeendarbari, Sina; Hao, Yaowu; Cai, Zhonghou; Cheng, Xuemei

Gold nanoparticles have a wide range of potential applications, including therapeutic agent delivery, catalysis, and electronics. Recently a new process of hollow nanoparticle synthesis was reported, the mechanism of which was hypothesized to involve electroless deposition around electrochemically evolved hydrogen bubbles. However, the growth mechanism still needs experimental evidence. We report investigation of this synthesis process using synchrotron x-ray diffraction and fluorescence measurements performed at beamline 2-ID-D of the Advanced Photon Source (APS). A series of gold nanoparticle samples with different synthesis time (50-1200 seconds) were deposited using a mixture electrolyte solution of Na3Au(SO3)2 and H4N2NiO6S2 on anodic aluminum oxide (AAO) membranes. The 2D mapping of fluorescence intensity and comparison of x-ray diffraction peaks of the samples have provided valuable information on the growth mechanism. Work at Bryn Mawr College and University of Texas at Arlington is supported by NSF Grants (1207085 and 1207377) and use of the APS at Argonne National Laboratory is supported by the U. S. Department of Energy under Contract No. DE-AC02-06CH11357.

Radiation-induced melting in coherent X-ray diffractive imaging at the nanoscale

PubMed Central

Ponomarenko, O.; Nikulin, A. Y.; Moser, H. O.; Yang, P.; Sakata, O.

2011-01-01

Coherent X-ray diffraction techniques play an increasingly significant role in the imaging of nanoscale structures, ranging from metallic and semiconductor to biological objects. In material science, X-rays are usually considered to be of a low-destructive nature, but under certain conditions they can cause significant radiation damage and heat loading on the samples. The qualitative literature data concerning the tolerance of nanostructured samples to synchrotron radiation in coherent diffraction imaging experiments are scarce. In this work the experimental evidence of a complete destruction of polymer and gold nanosamples by the synchrotron beam is reported in the case of imaging at 1–10 nm spatial resolution. Numerical simulations based on a heat-transfer model demonstrate the high sensitivity of temperature distribution in samples to macroscopic experimental parameters such as the conduction properties of materials, radiation heat transfer and convection. However, for realistic experimental conditions the calculated rates of temperature rise alone cannot explain the melting transitions observed in the nanosamples. Comparison of these results with the literature data allows a specific scenario of the sample destruction in each particular case to be presented, and a strategy for damage reduction to be proposed. PMID:21685675

Integrated nonlinear optical imaging microscope for on-axis crystal detection and centering at a synchrotron beamline

PubMed Central

Madden, Jeremy T.; Toth, Scott J.; Dettmar, Christopher M.; Newman, Justin A.; Oglesbee, Robert A.; Hedderich, Hartmut G.; Everly, R. Michael; Becker, Michael; Ronau, Judith A.; Buchanan, Susan K.; Cherezov, Vadim; Morrow, Marie E.; Xu, Shenglan; Ferguson, Dale; Makarov, Oleg; Das, Chittaranjan; Fischetti, Robert; Simpson, Garth J.

2013-01-01

Nonlinear optical (NLO) instrumentation has been integrated with synchrotron X-ray diffraction (XRD) for combined single-platform analysis, initially targeting applications for automated crystal centering. Second-harmonic-generation microscopy and two-photon-excited ultraviolet fluorescence microscopy were evaluated for crystal detection and assessed by X-ray raster scanning. Two optical designs were constructed and characterized; one positioned downstream of the sample and one integrated into the upstream optical path of the diffractometer. Both instruments enabled protein crystal identification with integration times between 80 and 150 µs per pixel, representing a ∼103–104-fold reduction in the per-pixel exposure time relative to X-ray raster scanning. Quantitative centering and analysis of phenylalanine hydroxylase from Chromobacterium violaceum cPAH, Trichinella spiralis deubiquitinating enzyme TsUCH37, human κ-opioid receptor complex kOR-T4L produced in lipidic cubic phase (LCP), intimin prepared in LCP, and α-cellulose samples were performed by collecting multiple NLO images. The crystalline samples were characterized by single-crystal diffraction patterns, while α-cellulose was characterized by fiber diffraction. Good agreement was observed between the sample positions identified by NLO and XRD raster measurements for all samples studied. PMID:23765294

Sub-500  nm hard x ray focusing by compound long kinoform lenses.

PubMed

Liao, Keliang; Liu, Jing; Liang, Hao; Wu, Xuehui; Zhang, Kai; Yuan, Qingxi; Yi, Futing; Sheng, Weifan

2016-01-01

The focusing performance of polymethyl methacrylate compound long kinoform lenses with 70 μm aperture and 19.5 mm focal length was characterized with 8 keV x rays using the knife-edge scan method at the 4W1A transmission x-ray microscope beamline of Beijing Synchrotron Radiation Facility. The experiment result shows a best FWHM focus size of 440 nm with 31% diffraction efficiency.

Origin of Pressure-induced Superconducting Phase in K xFe 2-ySe 2 studied by Synchrotron X-ray Diffraction and Spectroscopy

DOE PAGES

Yamamoto, Yoshiya; Yamaoka, Hitoshi; Tanaka, Masashi; ...

2016-08-08

Pressure dependence of the electronic and crystal structures of K xFe 2–ySe 2, which has pressure-induced two superconducting domes of SC I and SC II, was investigated by x-ray emission spectroscopy and diffraction. X-ray diffraction data show that compressibility along the c-axis changes around 12 GPa, where a new superconducting phase of SC II appears. This suggests a possible tetragonal to collapsed tetragonal phase transition. X-ray emission spectroscopy data also shows the change in the electronic structure around 12 GPa. These results can be explained by the scenario that the two SC domes under pressure originate from the change ofmore » Fermi surface topology. Lastly, our results here show the pronounced increase of the density of states near the Fermi surface under pressure with a structural phase transition, which can help address our fundamental understanding for the appearance of the SC II phase.« less

Large-area soft x-ray projection lithography using multilayer mirrors structured by RIE

NASA Astrophysics Data System (ADS)

Rahn, Steffen; Kloidt, Andreas; Kleineberg, Ulf; Schmiedeskamp, Bernt; Kadel, Klaus; Schomburg, Werner K.; Hormes, F. J.; Heinzmann, Ulrich

1993-01-01

SXPL (soft X-ray projection lithography) is one of the most promising applications of X-ray reflecting optics using multilayer mirrors. Within our collaboration, such multilayer mirrors were fabricated, characterized, laterally structured and then used as reflection masks in a projecting lithography procedure. Mo/Si-multilayer mirrors were produced by electron beam evaporation in UHV under thermal treatment with an in-situ X-ray controlled thickness in the region of 2d equals 14 nm. The reflectivities measured at normal incidence reached up to 54%. Various surface analysis techniques have been applied in order to characterize and optimize the X-ray mirrors. The multilayers were patterned by reactive ion etching (RIE) with CF(subscript 4), using a photoresist as the etch mask, thus producing X-ray reflection masks. The masks were tested in the synchrotron radiation laboratory of the electron accelerator ELSA at the Physikalisches Institut of Bonn University. A double crystal X-ray monochromator was modified so as to allow about 0.5 cm(superscript 2) of the reflection mask to be illuminated by white synchrotron radiation. The reflected patterns were projected (with an energy of 100 eV) onto the resist (Hoechst AZ PF 514), which was mounted at an average distance of about 7 mm. In the first test-experiments, structure sizes down to 8 micrometers were nicely reproduced over the whole of the exposed area. Smaller structures were distorted by Fresnel-diffraction. The theoretically calculated diffraction images agree very well with the observed images.

National Synchrotron Light Source annual report 1991

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

Hulbert, S.L.; Lazarz, N.M.

1992-04-01

This report discusses the following research conducted at NSLS: atomic and molecular science; energy dispersive diffraction; lithography, microscopy and tomography; nuclear physics; UV photoemission and surface science; x-ray absorption spectroscopy; x-ray scattering and crystallography; x-ray topography; workshop on surface structure; workshop on electronic and chemical phenomena at surfaces; workshop on imaging; UV FEL machine reviews; VUV machine operations; VUV beamline operations; VUV storage ring parameters; x-ray machine operations; x-ray beamline operations; x-ray storage ring parameters; superconducting x-ray lithography source; SXLS storage ring parameters; the accelerator test facility; proposed UV-FEL user facility at the NSLS; global orbit feedback systems; and NSLSmore » computer system.« less

Refractive optics to compensate x-ray mirror shape-errors

NASA Astrophysics Data System (ADS)

Laundy, David; Sawhney, Kawal; Dhamgaye, Vishal; Pape, Ian

2017-08-01

Elliptically profiled mirrors operating at glancing angle are frequently used at X-ray synchrotron sources to focus X-rays into sub-micrometer sized spots. Mirror figure error, defined as the height difference function between the actual mirror surface and the ideal elliptical profile, causes a perturbation of the X-ray wavefront for X- rays reflecting from the mirror. This perturbation, when propagated to the focal plane results in an increase in the size of the focused beam. At Diamond Light Source we are developing refractive optics that can be used to locally cancel out the wavefront distortion caused by figure error from nano-focusing elliptical mirrors. These optics could be used to correct existing optical components on synchrotron radiation beamlines in order to give focused X-ray beam sizes approaching the theoretical diffraction limit. We present our latest results showing measurement of the X-ray wavefront error after reflection from X-ray mirrors and the translation of the measured wavefront into a design for refractive optical elements for correction of the X-ray wavefront. We show measurement of the focused beam with and without the corrective optics inserted showing reduction in the size of the focus resulting from the correction to the wavefront.

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.

Tracking calcification in tissue-engineered bone using synchrotron micro-FTIR and SEM.

PubMed

Deegan, Anthony J; Cinque, Gianfelice; Wehbe, Katia; Konduru, Sandeep; Yang, Ying

2015-02-01

One novel tissue engineering approach to mimic in vivo bone formation is the use of aggregate or micromass cultures. Various qualitative and quantitative techniques, such as histochemical staining, protein assay kits and RT-PCR, have been used previously on cellular aggregate studies to investigate how these intricate arrangements lead to mature bone tissue. However, these techniques struggle to reveal spatial and temporal distribution of proliferation and mineralization simultaneously. Synchrotron-based Fourier transform infrared microspectroscopy (micro-FTIR) offers a unique insight at the molecular scale by coupling high IR sensitivity to organic matter with the high spatial resolution allowed by diffraction limited SR microbeam. This study is set to investigate the effects of culture duration and aggregate size on the dynamics and spatial distribution of calcification in engineered bone aggregates by a combination of micro-FTIR and scanning electron microscopy (SEM)/energy-dispersive X-ray spectroscopy (EDX). A murine bone cell line has been used, and small/large bone aggregates have been induced using different chemically treated culture substrates. Our findings suggest that bone cell aggregate culturing can greatly increase levels of mineralization over short culture periods. The size of the aggregates influences mineralisation rates with larger aggregates mineralizing at a faster rate than their smaller counterparts. The micro-FTIR mapping has demonstrated that mineralization in the larger aggregates initiated from the periphery and spread to the centre, whilst the smaller aggregates have more minerals in the centre at the early stage and deposited more in the periphery after further culturing, implying that aggregate size influences calcification distribution and development over time. SEM/EDX data correlates well with the micro-FTIR results for the total mineral content. Thus, synchrotron-based micro-FTIR can accurately track mineralization process/mechanism in the engineered bone.

Real-time phase-contrast x-ray imaging: a new technique for the study of animal form and function

PubMed Central

Socha, John J; Westneat, Mark W; Harrison, Jon F; Waters, James S; Lee, Wah-Keat

2007-01-01

Background Despite advances in imaging techniques, real-time visualization of the structure and dynamics of tissues and organs inside small living animals has remained elusive. Recently, we have been using synchrotron x-rays to visualize the internal anatomy of millimeter-sized opaque, living animals. This technique takes advantage of partially-coherent x-rays and diffraction to enable clear visualization of internal soft tissue not viewable via conventional absorption radiography. However, because higher quality images require greater x-ray fluxes, there exists an inherent tradeoff between image quality and tissue damage. Results We evaluated the tradeoff between image quality and harm to the animal by determining the impact of targeted synchrotron x-rays on insect physiology, behavior and survival. Using 25 keV x-rays at a flux density of 80 μW/mm-2, high quality video-rate images can be obtained without major detrimental effects on the insects for multiple minutes, a duration sufficient for many physiological studies. At this setting, insects do not heat up. Additionally, we demonstrate the range of uses of synchrotron phase-contrast imaging by showing high-resolution images of internal anatomy and observations of labeled food movement during ingestion and digestion. Conclusion Synchrotron x-ray phase contrast imaging has the potential to revolutionize the study of physiology and internal biomechanics in small animals. This is the only generally applicable technique that has the necessary spatial and temporal resolutions, penetrating power, and sensitivity to soft tissue that is required to visualize the internal physiology of living animals on the scale from millimeters to microns. PMID:17331247

Characterization of ion-induced radiation effects in nuclear materials using synchrotron x-ray techniques

DOE PAGES

Lang, Maik; Tracy, Cameron L.; Palomares, Raul I.; ...

2015-05-01

Recent efforts to characterize the nanoscale structural and chemical modifications induced by energetic ion irradiation in nuclear materials have greatly benefited from the application of synchrotron-based x-ray diffraction (XRD) and x-ray absorption spectroscopy (XAS) techniques. Key to the study of actinide-bearing materials has been the use of small sample volumes, which are particularly advantageous, as the small quantities minimize the level of radiation exposure at the ion-beam and synchrotron user facility. This approach utilizes energetic heavy ions (energy range: 100 MeV–3 GeV) that pass completely through the sample thickness and deposit an almost constant energy per unit length along theirmore » trajectory. High energy x-rays (25–65 keV) from intense synchrotron light sources are then used in transmission geometry to analyze ion-induced structural and chemical modifications throughout the ion tracks. We describe in detail the experimental approach for utilizing synchrotron radiation (SR) to study the radiation response of a range of nuclear materials (e.g., ThO 2 and Gd 2Ti xZr 2–xO 7). Also addressed is the use of high-pressure techniques, such as the heatable diamond anvil cell, as a new means to expose irradiated materials to well-controlled high-temperature (up to 1000 °C) and/or high-pressure (up to 50 GPa) conditions. Furthermore, this is particularly useful for characterizing the annealing kinetics of irradiation-induced material modifications.« less

Effective increase in beam emittance by phase-space expansion using asymmetric Bragg diffraction.

PubMed

Chu, Chia-Hung; Tang, Mau-Tsu; Chang, Shih-Lin

2015-08-24

We propose an innovative method to extend the utilization of the phase space downstream of a synchrotron light source for X-ray transmission microscopy. Based on the dynamical theory of X-ray diffraction, asymmetrically cut perfect crystals are applied to reshape the position-angle-wavelength space of the light source, by which the usable phase space of the source can be magnified by over one hundred times, thereby "phase-space-matching" the source with the objective lens of the microscope. The method's validity is confirmed using SHADOW code simulations, and aberration through an optical lens such as a Fresnel zone plate is examined via matrix optics for nano-resolution X-ray images.

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.

In cellulo serial crystallography of alcohol oxidase crystals inside yeast cells

DOE PAGES

Jakobi, Arjen J.; Passon, Daniel M.; Knoops, Kevin; ...

2016-03-01

The possibility of using femtosecond pulses from an X-ray free-electron laser to collect diffraction data from protein crystals formed in their native cellular organelle has been explored. X-ray diffraction of submicrometre-sized alcohol oxidase crystals formed in peroxisomes within cells of genetically modified variants of the methylotrophic yeast Hansenula polymorpha is reported and characterized. Furthermore, the observations are supported by synchrotron radiation-based powder diffraction data and electron microscopy. Based on these findings, the concept of in cellulo serial crystallography on protein targets imported into yeast peroxisomes without the need for protein purification as a requirement for subsequent crystallization is outlined.

In cellulo serial crystallography of alcohol oxidase crystals inside yeast cells

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

Jakobi, Arjen J.; Passon, Daniel M.; Knoops, Kevin

The possibility of using femtosecond pulses from an X-ray free-electron laser to collect diffraction data from protein crystals formed in their native cellular organelle has been explored. X-ray diffraction of submicrometre-sized alcohol oxidase crystals formed in peroxisomes within cells of genetically modified variants of the methylotrophic yeast Hansenula polymorpha is reported and characterized. Furthermore, the observations are supported by synchrotron radiation-based powder diffraction data and electron microscopy. Based on these findings, the concept of in cellulo serial crystallography on protein targets imported into yeast peroxisomes without the need for protein purification as a requirement for subsequent crystallization is outlined.

In cellulo serial crystallography of alcohol oxidase crystals inside yeast cells

PubMed Central

Jakobi, Arjen J.; Passon, Daniel M.; Knoops, Kèvin; Stellato, Francesco; Liang, Mengning; White, Thomas A.; Seine, Thomas; Messerschmidt, Marc; Chapman, Henry N.; Wilmanns, Matthias

2016-01-01

The possibility of using femtosecond pulses from an X-ray free-electron laser to collect diffraction data from protein crystals formed in their native cellular organelle has been explored. X-ray diffraction of submicrometre-sized alcohol oxidase crystals formed in peroxisomes within cells of genetically modified variants of the methylotrophic yeast Hansenula polymorpha is reported and characterized. The observations are supported by synchrotron radiation-based powder diffraction data and electron microscopy. Based on these findings, the concept of in cellulo serial crystallography on protein targets imported into yeast peroxisomes without the need for protein purification as a requirement for subsequent crystallization is outlined. PMID:27006771

A sparsity-based iterative algorithm for reconstruction of micro-CT images from highly undersampled projection datasets obtained with a synchrotron X-ray source

NASA Astrophysics Data System (ADS)

Melli, S. Ali; Wahid, Khan A.; Babyn, Paul; Cooper, David M. L.; Gopi, Varun P.

2016-12-01

Synchrotron X-ray Micro Computed Tomography (Micro-CT) is an imaging technique which is increasingly used for non-invasive in vivo preclinical imaging. However, it often requires a large number of projections from many different angles to reconstruct high-quality images leading to significantly high radiation doses and long scan times. To utilize this imaging technique further for in vivo imaging, we need to design reconstruction algorithms that reduce the radiation dose and scan time without reduction of reconstructed image quality. This research is focused on using a combination of gradient-based Douglas-Rachford splitting and discrete wavelet packet shrinkage image denoising methods to design an algorithm for reconstruction of large-scale reduced-view synchrotron Micro-CT images with acceptable quality metrics. These quality metrics are computed by comparing the reconstructed images with a high-dose reference image reconstructed from 1800 equally spaced projections spanning 180°. Visual and quantitative-based performance assessment of a synthetic head phantom and a femoral cortical bone sample imaged in the biomedical imaging and therapy bending magnet beamline at the Canadian Light Source demonstrates that the proposed algorithm is superior to the existing reconstruction algorithms. Using the proposed reconstruction algorithm to reduce the number of projections in synchrotron Micro-CT is an effective way to reduce the overall radiation dose and scan time which improves in vivo imaging protocols.

Electrochemical reactions in fluoride-ion batteries: mechanistic insights from pair distribution function analysis

DOE PAGES

Grenier, Antonin; Porras-Gutierrez, Ana-Gabriela; Groult, Henri; ...

2017-07-05

Detailed analysis of electrochemical reactions occurring in rechargeable Fluoride-Ion Batteries (FIBs) is provided by means of synchrotron X-ray diffraction (XRD) and Pair Distribution Function (PDF) analysis.

Local lattice distortion in NiCoCr, FeCoNiCr and FeCoNiCrMn concentrated alloys investigated by synchrotron X-ray diffraction

DOE PAGES

Tong, Yang; Jin, Ke; Bei, Hongbin; ...

2018-05-26

Severe lattice distortion is presumptively considered as a core effect of high-entropy alloys, but quantitative measurements are still missing. Here, we demonstrate that the lattice distortion in high-entropy alloys can be quantitatively analyzed based on pair distribution function obtained from synchrotron X-ray diffraction. By applying this method to equiatomic NiCoCr, FeCoNiCr and FeCoNiCrMn concentrated alloys, we found that the local lattice distortion in the NiCoCr (0.23%) and FeCoNiCrMn (0.24%) alloys are comparable while negligible in the FeCoNiCr alloy (0.04%). Furthermore, the origin of local lattice distortion in the NiCoCr and FeCoNiCrMn concentrated alloys was discussed.

Local lattice distortion in NiCoCr, FeCoNiCr and FeCoNiCrMn concentrated alloys investigated by synchrotron X-ray diffraction

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

Tong, Yang; Jin, Ke; Bei, Hongbin

Severe lattice distortion is presumptively considered as a core effect of high-entropy alloys, but quantitative measurements are still missing. Here, we demonstrate that the lattice distortion in high-entropy alloys can be quantitatively analyzed based on pair distribution function obtained from synchrotron X-ray diffraction. By applying this method to equiatomic NiCoCr, FeCoNiCr and FeCoNiCrMn concentrated alloys, we found that the local lattice distortion in the NiCoCr (0.23%) and FeCoNiCrMn (0.24%) alloys are comparable while negligible in the FeCoNiCr alloy (0.04%). Furthermore, the origin of local lattice distortion in the NiCoCr and FeCoNiCrMn concentrated alloys was discussed.

Phase formation and strain relaxation of Ga2O3 on c-plane and a-plane sapphire substrates as studied by synchrotron-based x-ray diffraction

NASA Astrophysics Data System (ADS)

Cheng, Zongzhe; Hanke, Michael; Vogt, Patrick; Bierwagen, Oliver; Trampert, Achim

2017-10-01

Heteroepitaxial Ga2O3 was deposited on c-plane and a-plane oriented sapphire by plasma-assisted molecular beam epitaxy and probed by ex-situ and in-situ synchrotron-based x-ray diffraction. The investigation on c-plane sapphire determined a critical thickness of around 33 Å, at which the monoclinic β-phase forms on top of the hexagonal α-phase. A 143 Å thick single phase α-Ga2O3 was observed on a-plane sapphire, much thicker than the α-Ga2O3 on c-plane sapphire. The α-Ga2O3 relaxed very fast in the first 30 Å in both out-of-plane and in-plane directions as measured by the in-situ study.

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.

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

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

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

Lyubimov, Artem Y.; Stanford University, Stanford, CA 94305; Stanford University, Stanford, CA 94305

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

Multiscale measurements on temperature-dependent deformation of a textured magnesium alloy with synchrotron x-ray imaging and diffraction

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

Lu, L.; Bie, B. X.; Li, Q. H.

2017-06-01

In situ synchrotron x-ray imaging and diffraction are used to investigate deformation of a rolled magnesium alloy under uniaxial compression at room and elevated temperatures along two different directions. The loading axis (LA) is either perpendicular or parallel to the normal direction, and these two cases are referred to as LA⊥ and LAk loading, respectively. Multiscale measurements including stressestrain curves (macroscale), strain fields (mesoscale), and diffraction patterns (microscale) are obtained simultaneously. Due to initial texture, f1012g extension twinning is predominant in the LA⊥ loading, while dislocation motion prevails in the LAk loading. With increasing temperature, fewer f1012g extension twins aremore » activated in the LA⊥ samples, giving rise to reduced strain homogenization, while pyramidal slip becomes readily activated, leading to more homogeneous deformation for the LAk loading. The difference in the strain hardening rates is attributed to that in strain field homogenization for these two loading directions« less

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.

Trichomes of Tobacco Excrete Zinc as Zinc-Substituted Calcium Carbonate and Other Zinc-Containing Compounds1[W

PubMed Central

Sarret, Géraldine; Harada, Emiko; Choi, Yong-Eui; Isaure, Marie-Pierre; Geoffroy, Nicolas; Fakra, Sirine; Marcus, Matthew A.; Birschwilks, Mandy; Clemens, Stephan; Manceau, Alain

2006-01-01

Tobacco (Nicotiana tabacum L. cv Xanthi) plants were exposed to toxic levels of zinc (Zn). Zn exposure resulted in toxicity signs in plants, and these damages were partly reduced by a calcium (Ca) supplement. Confocal imaging of intracellular Zn using Zinquin showed that Zn was preferentially accumulated in trichomes. Exposure to Zn and Zn + Ca increased the trichome density and induced the production of Ca/Zn mineral grains on the head cells of trichomes. These grains were aggregates of submicrometer-sized crystals and poorly crystalline material and contained Ca as major element, along with subordinate amounts of Zn, manganese, potassium, chlorine, phosphorus, silicon, and magnesium. Micro x-ray diffraction revealed that the large majority of the grains were composed essentially of metal-substituted calcite (CaCO3). CaCO3 polymorphs (aragonite and vaterite) and CaC2O4 (Ca oxalate) mono- and dihydrate also were identified, either as an admixture to calcite or in separate grains. Some grains did not diffract, although they contained Ca, suggesting the presence of amorphous form of Ca. The presence of Zn-substituted calcite was confirmed by Zn K-edge micro-extended x-ray absorption fine structure spectroscopy. Zn bound to organic compounds and Zn-containing silica and phosphate were also identified by this technique. The proportion of Zn-substituted calcite relative to the other species increased with Ca exposure. The production of Zn-containing biogenic calcite and other Zn compounds through the trichomes is a novel mechanism involved in Zn detoxification. This study illustrates the potential of laterally resolved x-ray synchrotron radiation techniques to study biomineralization and metal homeostasis processes in plants. PMID:16731580

X-ray diffraction and X-ray K absorption near edge studies of copper (II) complexes with amino acids

NASA Astrophysics Data System (ADS)

Sharma, P. K.; Mishra, Ashutosh; Malviya, Varsha; Kame, Rashmi; Malviya, P. K.

2017-05-01

Synthesis of copper (II) complexes [CuL1L2X].nH2O, where n=1, 2,3 (X=Cl,Br,NO3) (L1is 2,2’-bipyridine and L2 is L-tyrosine) by the chemical root method. The XRD data for the samples have been recorded. EXAFS spectra have also been recorded at the K-edge of Cu using the dispersive beam line BL-8 at 2.5 Gev Indus-2 Synchrotron radiation source at RRCAT, Indore, India. XRD and EXAFS data have been analysed using the computer software. X-ray diffraction studies of all complexes indicate their crystalline nature. Lattice parameter, bond length, particle size have been determined from XRD data.

Crystal Structure of 17α-Dihydroequilin, C18H22O2, from Synchrotron Powder Diffraction Data and Density Functional Theory

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

Kaduk, James; Gindhart, Amy; Blanton, Thomas

The crystal structure of 17α-dihydroequilin has been solved and refined using synchrotron X-ray powder diffraction data, and optimized using density functional techniques. 17α-dihydroequilin crystallizes in space group P212121 (#19) with a = 6.76849(1) Å, b = 8.96849(1) Å, c = 23.39031(5) Å, V = 1419.915(3) Å3, and Z = 4. Both hydroxyl groups form hydrogen bonds to each other, resulting in zig-zag chains along the b-axis. The powder diffraction pattern has been submitted to ICDD for inclusion in the Powder Diffraction File™ as the entry 00-066-1608.

An Investigation on the Persistence of Uranium Hydride during Storage of Simulant Nuclear Waste Packages.

PubMed

Stitt, C A; Harker, N J; Hallam, K R; Paraskevoulakos, C; Banos, A; Rennie, S; Jowsey, J; Scott, T B

2015-01-01

Synchrotron X-rays have been used to study the oxidation of uranium and uranium hydride when encapsulated in grout and stored in de-ionised water for 10 months. Periodic synchrotron X-ray tomography and X-ray powder diffraction have allowed measurement and identification of the arising corrosion products and the rates of corrosion. The oxidation rates of the uranium metal and uranium hydride were slower than empirically derived rates previously reported for each reactant in an anoxic water system, but without encapsulation in grout. This was attributed to the grout acting as a physical barrier limiting the access of oxidising species to the uranium surface. Uranium hydride was observed to persist throughout the 10 month storage period and industrial consequences of this observed persistence are discussed.

An Investigation on the Persistence of Uranium Hydride during Storage of Simulant Nuclear Waste Packages

PubMed Central

Harker, N. J.; Hallam, K. R.; Paraskevoulakos, C.; Banos, A.; Rennie, S.; Jowsey, J.

2015-01-01

Synchrotron X-rays have been used to study the oxidation of uranium and uranium hydride when encapsulated in grout and stored in de-ionised water for 10 months. Periodic synchrotron X-ray tomography and X-ray powder diffraction have allowed measurement and identification of the arising corrosion products and the rates of corrosion. The oxidation rates of the uranium metal and uranium hydride were slower than empirically derived rates previously reported for each reactant in an anoxic water system, but without encapsulation in grout. This was attributed to the grout acting as a physical barrier limiting the access of oxidising species to the uranium surface. Uranium hydride was observed to persist throughout the 10 month storage period and industrial consequences of this observed persistence are discussed. PMID:26176551

Thermal Stress Behavior of Micro- and Nano-Size Aluminum Films

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

Hanabusa, T.; Kusaka, K.; Nishida, M.

2008-03-17

In-situ observation of thermal stresses in thin films deposited on silicon substrate was made by X-ray and synchrotron radiation. Specimens prepared in this experiment were micro- and nano-size thin aluminum films with and without passivation film. The thickness of the film was 1 micrometer for micro-size films and 10, 20 and 50 nanometer for nano-size films. The stress measurement in micro-size films was made by X-ray radiation whereas the measurement of nano-size films was made by synchrotron radiation. Residual stress measurement revealed tensile stresses in all as-deposited films. Thermal stresses were measured in a series of heating- and cooling-stage. Thermalmore » stress behavior of micro-size films revealed hysteresis loop during a heating and cooling process. The width of a hysteresis loop was larger in passivated film that unpassivated film. No hysteresis loops were observed in nano-size films with SiO{sub 2} passivation. Strengthning mechanism in thin films was discussed on a passivation film and a film thickness.« less

Crystallization and preliminary X-ray diffraction study of recombinant ribokinase from Thermus Species 2.9

NASA Astrophysics Data System (ADS)

Abramchik, Yu. A.; Timofeev, V. I.; Muravieva, T. I.; Esipov, R. S.; Kuranova, I. P.

2016-11-01

Ribokinase from a thermophilic strain of Thermus species 2.9 belonging to the carbohydrate ribokinase family (EC 2.7.1.15) was isolated, purified, and crystallized. The crystallization conditions were found by the vapor-diffusion technique and were then optimized to apply the capillary counter-diffusion technique. The X-ray diffraction data set was collected from the crystals, which were grown by the counter-diffusion technique, at the SPring-8 synchrotron radiation facility to 2.87 Å resolution. The crystals belong to sp. gr. P1211 and have the following unit-cell parameters: a = 81.613 Å, b = 156.132 Å, c = 87.714 Å, α = γ = 90°, β = 103.819°. The X-ray diffraction data set is suitable for determining the three-dimensional structure of the protein by the molecular-replacement method.

Room-temperature serial crystallography using a kinetically optimized microfluidic device for protein crystallization and on-chip X-ray diffraction

PubMed Central

Heymann, Michael; Opthalage, Achini; Wierman, Jennifer L.; Akella, Sathish; Szebenyi, Doletha M. E.; Gruner, Sol M.; Fraden, Seth

2014-01-01

An emulsion-based serial crystallographic technology has been developed, in which nanolitre-sized droplets of protein solution are encapsulated in oil and stabilized by surfactant. Once the first crystal in a drop is nucleated, the small volume generates a negative feedback mechanism that lowers the supersaturation. This mechanism is exploited to produce one crystal per drop. Diffraction data are measured, one crystal at a time, from a series of room-temperature crystals stored on an X-ray semi-transparent microfluidic chip, and a 93% complete data set is obtained by merging single diffraction frames taken from different unoriented crystals. As proof of concept, the structure of glucose isomerase was solved to 2.1 Å, demonstrating the feasibility of high-throughput serial X-ray crystallography using synchrotron radiation. PMID:25295176

Energy-dispersive X-ray emission spectroscopy using an X-ray free-electron laser in a shot-by-shot mode

DOE PAGES

Alonso-Mori, Roberto; Kern, Jan; Gildea, Richard J.; ...

2012-11-05

The ultrabright femtosecond X-ray pulses provided by X-ray free-electron lasers open capabilities for studying the structure and dynamics of a wide variety of systems beyond what is possible with synchrotron sources. Recently, this “probe-before-destroy” approach has been demonstrated for atomic structure determination by serial X-ray diffraction of microcrystals. There has been the question whether a similar approach can be extended to probe the local electronic structure by X-ray spectroscopy. To address this, we have carried out femtosecond X-ray emission spectroscopy (XES) at the Linac Coherent Light Source using redox-active Mn complexes. XES probes the charge and spin states as wellmore » as the ligand environment, critical for understanding the functional role of redox-active metal sites. Kβ 1,3 XES spectra of Mn II and Mn 2 III,IV complexes at room temperature were collected using a wavelength dispersive spectrometer and femtosecond X-ray pulses with an individual dose of up to >100 MGy. The spectra were found in agreement with undamaged spectra collected at low dose using synchrotron radiation. Our results demonstrate that the intact electronic structure of redox active transition metal compounds in different oxidation states can be characterized with this shot-by-shot method. This opens the door for studying the chemical dynamics of metal catalytic sites by following reactions under functional conditions. Furthermore, the technique can be combined with X-ray diffraction to simultaneously obtain the geometric structure of the overall protein and the local chemistry of active metal sites and is expected to prove valuable for understanding the mechanism of important metalloproteins, such as photosystem II.« less

Energy-dispersive X-ray emission spectroscopy using an X-ray free-electron laser in a shot-by-shot mode

PubMed Central

Alonso-Mori, Roberto; Kern, Jan; Gildea, Richard J.; Sokaras, Dimosthenis; Weng, Tsu-Chien; Lassalle-Kaiser, Benedikt; Tran, Rosalie; Hattne, Johan; Laksmono, Hartawan; Hellmich, Julia; Glöckner, Carina; Echols, Nathaniel; Sierra, Raymond G.; Schafer, Donald W.; Sellberg, Jonas; Kenney, Christopher; Herbst, Ryan; Pines, Jack; Hart, Philip; Herrmann, Sven; Grosse-Kunstleve, Ralf W.; Latimer, Matthew J.; Fry, Alan R.; Messerschmidt, Marc M.; Miahnahri, Alan; Seibert, M. Marvin; Zwart, Petrus H.; White, William E.; Adams, Paul D.; Bogan, Michael J.; Boutet, Sébastien; Williams, Garth J.; Zouni, Athina; Messinger, Johannes; Glatzel, Pieter; Sauter, Nicholas K.; Yachandra, Vittal K.; Yano, Junko; Bergmann, Uwe

2012-01-01

The ultrabright femtosecond X-ray pulses provided by X-ray free-electron lasers open capabilities for studying the structure and dynamics of a wide variety of systems beyond what is possible with synchrotron sources. Recently, this “probe-before-destroy” approach has been demonstrated for atomic structure determination by serial X-ray diffraction of microcrystals. There has been the question whether a similar approach can be extended to probe the local electronic structure by X-ray spectroscopy. To address this, we have carried out femtosecond X-ray emission spectroscopy (XES) at the Linac Coherent Light Source using redox-active Mn complexes. XES probes the charge and spin states as well as the ligand environment, critical for understanding the functional role of redox-active metal sites. Kβ1,3 XES spectra of MnII and Mn2III,IV complexes at room temperature were collected using a wavelength dispersive spectrometer and femtosecond X-ray pulses with an individual dose of up to >100 MGy. The spectra were found in agreement with undamaged spectra collected at low dose using synchrotron radiation. Our results demonstrate that the intact electronic structure of redox active transition metal compounds in different oxidation states can be characterized with this shot-by-shot method. This opens the door for studying the chemical dynamics of metal catalytic sites by following reactions under functional conditions. The technique can be combined with X-ray diffraction to simultaneously obtain the geometric structure of the overall protein and the local chemistry of active metal sites and is expected to prove valuable for understanding the mechanism of important metalloproteins, such as photosystem II. PMID:23129631

Near Edge X-Ray Absorption and X-Ray Photoelectron Diffraction Studies of the Structural Environment of Ge-Si Systems

NASA Astrophysics Data System (ADS)

Castrucci, P.; Gunnella, R.; Pinto, N.; Bernardini, R.; de Crescenzi, M.; Sacchi, M.

Near edge X-ray absorption spectroscopy (XAS), X-ray photoelectron diffraction (XPD) and Auger electron diffraction (AED) are powerful techniques for the qualitative study of the structural and electronic properties of several systems. The recent development of a multiple scattering approach to simulating experimental spectra opened a friendly way to the study of structural environments of solids and surfaces. This article reviews recent X-ray absorption experiments using synchrotron radiation which were performed at Ge L edges and core level electron diffraction measurements obtained using a traditional X-ray source from Ge core levels for ultrathin Ge films deposited on silicon substrates. Thermodynamics and surface reconstruction have been found to play a crucial role in the first stages of Ge growth on Si(001) and Si(111) surfaces. Both techniques show the occurrence of intermixing processes even for room-temperature-grown Ge/Si(001) samples and give a straightforward measurement of the overlayer tetragonal distortion. The effects of Sb as a surfactant on the Ge/Si(001) interface have also been investigated. In this case, evidence of layer-by-layer growth of the fully strained Ge overlayer with a reduced intermixing is obtained when one monolayer of Sb is predeposited on the surface.

Surface and interface analysis of nanomaterials at microfocus beamline (BL-16) of Indus-2

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

Das, Gangadhar, E-mail: rnrrsgangadhar@gmail.com; Tiwari, M. K., E-mail: mktiwati@rrcat.gov.in; Homi Bhabha National Institute, RRCAT

2016-05-06

Analysis of chemical nature and electronic structure at the interface of a thin film medium is important in many technological applications as well as to understand overall efficiency of a thin film device. Synchrotron radiation based x-ray spectroscopy is a promising technique to study interface nature of the nanomaterials with atomic resolutions. A combined x-ray reflectivity and grazing incidence x-ray fluorescence measurement facility has been recently constructed at the BL-16 microfocus beamline of Indus-2 synchrotron facility to accomplish surface-interface microstructural characterization of thin layered materials. It is also possible to analyze contaminates or adsorbed ad-atoms on the surface of themore » thin nanostructure materials. The BL-16 beamline also provides an attractive platform to perform a variety of analytical research activities especially in the field of micro x-ray fluorescence and ultra-trace elements analysis using Synchrotron radiation. We describe various salient features of the BL-16 reflectometer experimental station and the detailed description of its capabilities through the measured results, obtained for various thin layered nanomaterials.« less

Mg(1 + x)Ir(1 - x) (x = 0, 0.037 and 0.054), a binary intermetallic compound with a new orthorhombic structure type determined from powder and single-crystal X-ray diffraction.

PubMed

Cerný, Radovan; Renaudin, Guillaume; Favre-Nicolin, Vincent; Hlukhyy, Viktor; Pöttgen, Rainer

2004-06-01

The new binary compound Mg(1 + x)Ir(1 - x) (x = 0-0.054) was prepared by melting the elements in the Mg:Ir ratio 2:3 in a sealed tantalum tube under an argon atmosphere in an induction furnace (single crystals) or by annealing cold-pressed pellets of the starting composition Mg:Ir 1:1 in an autoclave under an argon atmosphere (powder sample). The structure was independently solved from high-resolution synchrotron powder and single-crystal X-ray data: Pearson symbol oC304, space group Cmca, lattice parameters from synchrotron powder data a = 18.46948 (6), b = 16.17450 (5), c = 16.82131 (5) A. Mg(1 + x)Ir(1 - x) is a topologically close-packed phase, containing 13 Ir and 12 Mg atoms in the asymmetric unit, and has a narrow homogeneity range. Nearly all the atoms have Frank-Kasper-related coordination polyhedra, with the exception of two Ir atoms, and this compound contains the shortest Ir-Ir distances ever observed. The solution of a rather complex crystal structure from powder diffraction, which was fully confirmed by the single-crystal method, shows the power of powder diffraction in combination with the high-resolution data and the global optimization method.

An experimental system for high temperature X-ray diffraction studies with in situ mechanical loading

PubMed Central

Oswald, Benjamin B.; Schuren, Jay C.; Pagan, Darren C.; Miller, Matthew P.

2013-01-01

An experimental system with in situ thermomechanical loading has been developed to enable high energy synchrotron x-ray diffraction studies of crystalline materials. The system applies and maintains loads of up to 2250 N in uniaxial tension or compression at a frequency of up to 100 Hz. The furnace heats the specimen uniformly up to a maximum temperature of 1200 °C in a variety of atmospheres (oxidizing, inert, reducing) that, combined with in situ mechanical loading, can be used to mimic processing and operating conditions of engineering components. The loaded specimen is reoriented with respect to the incident beam of x-rays using two rotational axes to increase the number of crystal orientations interrogated. The system was used at the Cornell High Energy Synchrotron Source to conduct experiments on single crystal silicon and polycrystalline Low Solvus High Refractory nickel-based superalloy. The data from these experiments provide new insights into how stresses evolve at the crystal scale during thermomechanical loading and complement the development of high-fidelity material models. PMID:23556825

Negative thermal expansion and magnetoelastic coupling in the breathing pyrochlore lattice material LiGaCr4S8

NASA Astrophysics Data System (ADS)

Pokharel, G.; May, A. F.; Parker, D. S.; Calder, S.; Ehlers, G.; Huq, A.; Kimber, S. A. J.; Arachchige, H. Suriya; Poudel, L.; McGuire, M. A.; Mandrus, D.; Christianson, A. D.

2018-04-01

The physical properties of the spinel LiGaCr4S8 have been studied with neutron diffraction, x-ray diffraction, magnetic susceptibility, and heat capacity measurements. The neutron diffraction and synchrotron x-ray diffraction data reveal negative thermal expansion (NTE) below 111(4) K. The magnetic susceptibility deviates from Curie-Weiss behavior with the onset of NTE. At low temperature a broad peak in the magnetic susceptibility at 10.3(3) K is accompanied by the return of normal thermal expansion. First-principles calculations find a strong coupling between the lattice and the simulated magnetic ground state. These results indicate strong magnetoelastic coupling in LiGaCr4S8 .

New high- and low-temperature apparatus for synchrotron polycrystalline X-ray diffraction.

PubMed

Tang, C C; Bushnell-Wye, G; Cernik, R J

1998-05-01

A high-temperature furnace with an induction heater coil and a cryogenic system based on closed-cycle refrigeration have been assembled to enhance the non-ambient powder diffraction facilities at the Synchrotron Radiation Source, Daresbury Laboratory. The commissioning of the high- and low-temperature devices on the high-resolution powder diffractometer of Station 2.3 is described. The combined temperature range provided by the furnace/cryostat is 10-1500 K. Results from Fe and NH(4)Br powder samples are presented to demonstrate the operation of the apparatus. The developments presented in this paper are applicable to a wide range of other experiments and diffraction geometries.

Complete elliptical ring geometry provides energy and instrument calibration for synchrotron-based two-dimensional X-ray diffraction

PubMed Central

Hart, Michael L.; Drakopoulos, Michael; Reinhard, Christina; Connolley, Thomas

2013-01-01

A complete calibration method to characterize a static planar two-dimensional detector for use in X-ray diffraction at an arbitrary wavelength is described. This method is based upon geometry describing the point of intersection between a cone’s axis and its elliptical conic section. This point of intersection is neither the ellipse centre nor one of the ellipse focal points, but some other point which lies in between. The presented solution is closed form, algebraic and non-iterative in its application, and gives values for the X-ray beam energy, the sample-to-detector distance, the location of the beam centre on the detector surface and the detector tilt relative to the incident beam. Previous techniques have tended to require prior knowledge of either the X-ray beam energy or the sample-to-detector distance, whilst other techniques have been iterative. The new calibration procedure is performed by collecting diffraction data, in the form of diffraction rings from a powder standard, at known displacements of the detector along the beam path. PMID:24068840

A Curved Image-Plate Detector System for High-Resolution Synchrotron X-ray Diffraction

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

Sarin, P.; Haggerty, R; Yoon, W

2009-01-01

The developed curved image plate (CIP) is a one-dimensional detector which simultaneously records high-resolution X-ray diffraction (XRD) patterns over a 38.7 2{theta} range. In addition, an on-site reader enables rapid extraction, transfer and storage of X-ray intensity information in {le}30 s, and further qualifies this detector to study kinetic processes in materials science. The CIP detector can detect and store X-ray intensity information linearly proportional to the incident photon flux over a dynamical range of about five orders of magnitude. The linearity and uniformity of the CIP detector response is not compromised in the unsaturated regions of the image plate,more » regardless of saturation in another region. The speed of XRD data acquisition together with excellent resolution afforded by the CIP detector is unique and opens up wide possibilities in materials research accessible through X-ray diffraction. This article presents details of the basic features, operation and performance of the CIP detector along with some examples of applications, including high-temperature XRD.« less

National Synchrotron Light Source annual report 1991. Volume 1, October 1, 1990--September 30, 1991

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

Hulbert, S.L.; Lazarz, N.M.

1992-04-01

This report discusses the following research conducted at NSLS: atomic and molecular science; energy dispersive diffraction; lithography, microscopy and tomography; nuclear physics; UV photoemission and surface science; x-ray absorption spectroscopy; x-ray scattering and crystallography; x-ray topography; workshop on surface structure; workshop on electronic and chemical phenomena at surfaces; workshop on imaging; UV FEL machine reviews; VUV machine operations; VUV beamline operations; VUV storage ring parameters; x-ray machine operations; x-ray beamline operations; x-ray storage ring parameters; superconducting x-ray lithography source; SXLS storage ring parameters; the accelerator test facility; proposed UV-FEL user facility at the NSLS; global orbit feedback systems; and NSLSmore » computer system.« less

MICRO SCALE INVESTIGATIONS TO UNDERSTAND BINDING MECHANISMS OF METALS IN BIOSOLIDS USING SYNCHROTRON BASED X-RAY FLUORESCENCE AND X-RAY ABSORPTION SPECTROSCOPIES

EPA Science Inventory

The environmental impact of metals in biosolids to plants, animals and the human food chain has been studied for decades. From the related literature, it can be concluded that, by addition of biosolids to soil, the overall chemical reactivity in the soil system is altered beyond ...

Elemental mapping of biofortified wheat grains using micro X-ray fluorescence

NASA Astrophysics Data System (ADS)

Ramos, I.; Pataco, I. M.; Mourinho, M. P.; Lidon, F.; Reboredo, F.; Pessoa, M. F.; Carvalho, M. L.; Santos, J. P.; Guerra, M.

2016-06-01

Micro X-ray fluorescence has been used to obtain elemental maps of biofortified wheat grains. Two varieties of wheat were used in the study, Triticum aestivum L. and Triticum durum desf. Two treatments, with different nutrient concentration, were applied to the plants during the whole plant growth cycle. From the obtained elemental maps it was possible to extract information regarding the plant's physiological processes under the biofortification procedures. Both macro and micronutrients were mapped, providing useful insight into the posterior food processing mechanisms of this biofortified staple food. We have also shown that these kind of studies can now be performed with laboratory benchtop apparatus, rather than using synchrotron radiation, increasing the overall attractiveness of micro X-ray fluorescence in the study of highly heterogeneous biological samples.

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

Zhang, Baozhuo; Young, Marcus L.

Many technological applications of austenitic shape memory alloys (SMAs) involve cyclical mechanical loading and unloading in order to take advantage of pseudoelasticity. In this paper, we investigated the effect of mechanical bending of pseudoelastic NiTi SMA wires using high-energy synchrotron radiation X-ray diffraction (SR-XRD). Differential scanning calorimetry was performed to identify the phase transformation temperatures. Scanning electron microscopy images show that micro-cracks in compressive regions of the wire propagate with increasing bend angle, while tensile regions tend not to exhibit crack propagation. SR-XRD patterns were analyzed to study the phase transformation and investigate micromechanical properties. By observing the various diffraction peaks such as the austenite (200) and the martensite (more » $${\\bar 1}12$$), ($${\\bar 1}03$$), ($${\\bar 1}11$$), and (101) planes, intensities and residual strain values exhibit strong anisotropy, depending upon whether the sample is in compression or tension during bending.« less

Origin of Pressure-induced Superconducting Phase in KxFe2-ySe2 studied by Synchrotron X-ray Diffraction and Spectroscopy

NASA Astrophysics Data System (ADS)

Yamamoto, Yoshiya; Yamaoka, Hitoshi; Tanaka, Masashi; Okazaki, Hiroyuki; Ozaki, Toshinori; Takano, Yoshihiko; Lin, Jung-Fu; Fujita, Hidenori; Kagayama, Tomoko; Shimizu, Katsuya; Hiraoka, Nozomu; Ishii, Hirofumi; Liao, Yen-Fa; Tsuei, Ku-Ding; Mizuki, Jun'Ichiro

2016-08-01

Pressure dependence of the electronic and crystal structures of KxFe2-ySe2, which has pressure-induced two superconducting domes of SC I and SC II, was investigated by x-ray emission spectroscopy and diffraction. X-ray diffraction data show that compressibility along the c-axis changes around 12 GPa, where a new superconducting phase of SC II appears. This suggests a possible tetragonal to collapsed tetragonal phase transition. X-ray emission spectroscopy data also shows the change in the electronic structure around 12 GPa. These results can be explained by the scenario that the two SC domes under pressure originate from the change of Fermi surface topology. Our results here show the pronounced increase of the density of states near the Fermi surface under pressure with a structural phase transition, which can help address our fundamental understanding for the appearance of the SC II phase.

Comparison of diffraction-enhanced computed tomography and monochromatic synchrotron radiation computed tomography of human trabecular bone.

PubMed

Connor, D M; Hallen, H D; Lalush, D S; Sumner, D R; Zhong, Z

2009-10-21

Diffraction-enhanced imaging (DEI) is an x-ray-based medical imaging modality that, when used in tomography mode (DECT), can generate a three-dimensional map of both the apparent absorption coefficient and the out-of-plane gradient of the index of refraction of the sample. DECT is known to have contrast gains over monochromatic synchrotron radiation CT (SRCT) for soft tissue structures. The goal of this experiment was to compare contrast-to-noise ratio (CNR) and resolution in images of human trabecular bone acquired using SRCT with images acquired using DECT. All images were acquired at the National Synchrotron Light Source (Upton, NY, USA) at beamline X15 A at an x-ray energy of 40 keV and the silicon [3 3 3] reflection. SRCT, apparent absorption DECT and refraction DECT slice images of the trabecular bone were created. The apparent absorption DECT images have significantly higher spatial resolution and CNR than the corresponding SRCT images. Thus, DECT will prove to be a useful tool for imaging applications in which high contrast and high spatial resolution are required for both soft tissue features and bone.

Development of at-wavelength metrology for x-ray optics at the ALS

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

Yashchuk, Valeriy V.; Goldberg, Kenneth A.; Yuan, Sheng

2010-07-09

The comprehensive realization of the exciting advantages of new third- and forth-generation synchrotron radiation light sources requires concomitant development of reflecting and diffractive x-ray optics capable of micro- and nano-focusing, brightness preservation, and super high resolution. The fabrication, tuning, and alignment of the optics are impossible without adequate metrology instrumentation, methods, and techniques. While the accuracy of ex situ optical metrology at the Advanced Light Source (ALS) has reached a state-of-the-art level, wavefront control on beamlines is often limited by environmental and systematic alignment factors, and inadequate in situ feedback. At ALS beamline 5.3.1, we are developing broadly applicable, high-accuracy,more » in situ, at-wavelength wavefront measurement techniques to surpass 100-nrad slope measurement accuracy for Kirkpatrick-Baez (KB) mirrors. The at-wavelength methodology we are developing relies on a series of tests with increasing accuracy and sensitivity. Geometric Hartmann tests, performed with a scanning illuminated sub-aperture determine the wavefront slope across the full mirror aperture. Shearing interferometry techniques use coherent illumination and provide higher sensitivity wavefront measurements. Combining these techniques with high precision optical metrology and experimental methods will enable us to provide in situ setting and alignment of bendable x-ray optics to realize diffraction-limited, sub 50 nm focusing at beamlines. We describe here details of the metrology beamline endstation, the x-ray beam diagnostic system, and original experimental techniques that have already allowed us to precisely set a bendable KB mirror to achieve a focused spot size of 150 nm.« less

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.

About microcracking due to leaching in cementitious composites: X-ray microtomography description and numerical approach

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

Rougelot, Thomas; Burlion, Nicolas, E-mail: nicolas.burlion@polytech-lille.f; Bernard, Dominique

2010-02-15

Chemical shock of cement based materials leads to significant degradation of their physical properties. A typical scenario is a calcium leaching due to water (water with very low pH compared with that of pore fluid). The main objective of this paper is to evaluate the evolution of microstructure induced by leaching of a cementitious composite using synchrotron X-ray micro tomography, mainly from an experimental point of view. In this particular case, it was possible to identify cracking induced by leaching. After a description of the degradation mechanism and the X-ray synchrotron microtomographic analysis, numerical simulations are performed in order tomore » show that cracking is induced by an initial pre-stressing of the composite, coupled with decalcification shrinkage and dramatic decrease in tensile strength during leaching. X-ray microtomography analysis allowed to make evidence of an induced microcracking in cementitious material submitted to leaching.« less

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

In situ analysis of phase transformation in sol-gel cogelified nanopowder mixture of Al 2O 3 and TiO 2 using synchrotron X-ray radiation diffraction experiments

NASA Astrophysics Data System (ADS)

Jianu, A.; Stanciu, L.; Groza, J. R.; Lathe, Ch.; Burkel, E.

2003-01-01

Aluminium titanate (Al 2TiO 5) has been selected for study due to its high melting point and thermal shock resistance. In situ analysis of phase transformation and of transformation kinetics of sol-gel powder mixture of alumina and titania cogelified samples was performed using high-temperature synchrotron radiation X-ray diffraction experiments. The high reactivity and molecular mixing of sol-gel cogelified precursor powders contributed to the evolution of the reaction. The stability of the TiO 2-tetragonal structure (anatase) increases due to Al 2O 3 presence. The temperature of the aluminium titanate endothermic reaction decreases when heating rate increases. The results obtained by in situ analysis have been used to establish the sintering parameters in order to obtain fully transformed, dense aluminium titanate bulk ceramics.

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

Insights on the origin of the Tb5Ge4 magnetocaloric effect

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

Belo, J. H.; Barbosa, M. B.; Pires, A. L.

2017-05-01

In this report the magnetic, atomic structures and spin-lattice coupling have been thoroughly studied through high magnetic field magnetometry, Synchrotron X-ray diffraction under applied magnetic field and magnetostriction measurements in the Tb5Ge4 compounds. A field induced phase transition from an antiferromagnetic towards a ferromagnetic ordering was confirmed but with absence of structural transformation. This absence has been confirmed experimentally through synchrotron x-ray diffraction under applied field (up to 30 T). Moreover, this absence was explained via a thermodynamic free energy model: first principles calculations determined a large energy gap (ΔE=0.65 eV) between the two possible structures, O(I) and O(II). Frommore » magnetic and structural properties, a H-T phase diagram has been proposed for Tb5Ge4. Finally it was observed a large magnetostriction (up to 600 ppm) induced by ΔH=7 T.« less

Intergranular stress study of TC11 titanium alloy after laser shock peening by synchrotron-based high-energy X-ray diffraction

NASA Astrophysics Data System (ADS)

Su, R.; Li, L.; Wang, Y. D.; Nie, Z. H.; Ren, Y.; Zhou, X.; Wang, J.

2018-05-01

The distribution of residual lattice strain as a function of depth were carefully investigated by synchrotron-based high energy X-ray diffraction (HEXRD) in TC11 titanium alloy after laser shock peening (LSP). The results presented big compressive residual lattice strains at surface and subsurface, then tensile residual lattice strains in deeper region, and finally close to zero lattice strains in further deep interior with no plastic deformation thereafter. These evolutions in residual lattice strains were attributed to the balance of direct load effect from laser shock wave and the derivative restriction force effect from surrounding material. Significant intergranular stress was evidenced in the processed sample. The intergranular stress exhibited the largest value at surface, and rapidly decreased with depth increase. The magnitude of intergranular stress was proportional to the severity of the plastic deformation caused by LSP. Two shocks generated larger intergranular stress than one shock.

Shining a light on planetary processes using synchrotron techniques

NASA Astrophysics Data System (ADS)

Brand, H. E. A.; Kimpton, J. A.

2017-12-01

The Australian Synchrotron is a world-class national research facility that uses accelerator technology to produce X-rays and infrared for research. It is available for researchers from all institutions and disciplines. This contribution is intended to inform the community of the current capabilities at the facility using examples drawn from planetary research across the beamlines. Examples will include: formation of jarosite minerals with a view to Mars; studies of Micrometeorites; and large volume CT imaging of geological samples. A suite of new beamlines has been proposed for the growth of the facility and one of these, ADS, the Advanced Diffraction and Scattering beamline, is intended to be a high energy X-ray diffraction beamline capable of reaching extreme conditions and carrying out challenging in situ experiments. There is an opportunity to develop complex new sample environments which could be of relevance to shock metamorphic processes and this will form part of the discussion.

In situ synchrotron X-ray diffraction study of hydrides in Zircaloy-4 during thermomechanical cycling

DOE PAGES

Cinbiz, Mahmut N.; Koss, Donald A.; Motta, Arthur T.; ...

2017-02-20

The d-spacing evolution of both in-plane and out-of-plane hydrides has been studied using in situ synchrotron radiation X-ray diffraction during thermo-mechanical cycling of cold-worked stress-relieved Zircaloy-4. The structure of the hydride precipitates is such that the δ{111} d-spacing of the planes aligned with the hydride platelet face is greater than the d-spacing of the 111 planes aligned with the platelet edges. Upon heating from room temperature, the δ{111} planes aligned with hydride plate edges exhibit bi-linear thermally-induced expansion. In contrast, the d-spacing of the (111) plane aligned with the hydride plate face initially contracts upon heating. Furthermore, these experimental resultsmore » can be understood in terms of a reversal of stress state associated with precipitating or dissolving hydride platelets within the α-zirconium matrix.« less

Synchrotron x-ray diffraction studies of the structural properties of electrode materials in operating battery cells

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

Thurston, T.R.; Jisrawi, N.M.; Mukerjee, S.

Hard x rays from a synchrotron source were utilized in diffraction experiments which probed the bulk of electrode materials while they were operating {ital in} {ital situ} in battery cells. Two technologically relevant electrode materials were examined; an {ital AB}{sub 2}-type anode in a nickel{endash}metal{endash}hydride cell and a LiMn{sub 2}O{sub 4} cathode in a Li-ion {open_quote}{open_quote}rocking chair{close_quote}{close_quote} cell. Structural features such as lattice expansions and contractions, phase transitions, and the formation of multiple phases were easily observed as either hydrogen or lithium was electrochemically intercalated in and out of the electrode materials. The relevance of this technique for future studiesmore » of battery electrode materials is discussed. {copyright} {ital 1996 American Institute of Physics.}« less

Parts per Million Powder X-ray Diffraction

DOE PAGES

Newman, Justin A.; Schmitt, Paul D.; Toth, Scott J.; ...

2015-10-14

Here in this paper we demonstrate the use of second harmonic generation (SHG) microscopy-guided synchrotron powder X-ray diffraction (PXRD) for the detection of trace crystalline active pharmaceutical ingredients in a common polymer blend. The combined instrument is capable of detecting 100 ppm crystalline ritonavir in an amorphous hydroxypropyl methylcellulose matrix with a high signal-to-noise ratio (>5000). The high spatial resolution afforded by SHG microscopy allows for the use of a minibeam collimator to reduce the total volume of material probed by synchrotron PXRD. The reduction in probed volume results in reduced background from amorphous material. The ability to detect lowmore » crystalline loading has the potential to improve measurements in the formulation pipeline for pharmaceutical solid dispersions, for which even trace quantities of crystalline active ingredients can negatively impact the stability and bioavailability of the final drug product.« less

Polarization-resolved second-harmonic generation microscopy as a method to visualize protein-crystal domains

PubMed Central

DeWalt, Emma L.; Begue, Victoria J.; Ronau, Judith A.; Sullivan, Shane Z.; Das, Chittaranjan; Simpson, Garth J.

2013-01-01

Polarization-resolved second-harmonic generation (PR-SHG) microscopy is described and applied to identify the presence of multiple crystallographic domains within protein-crystal conglomerates, which was confirmed by synchrotron X-ray diffraction. Principal component analysis (PCA) of PR-SHG images resulted in principal component 2 (PC2) images with areas of contrasting negative and positive values for conglomerated crystals and PC2 images exhibiting uniformly positive or uniformly negative values for single crystals. Qualitative assessment of PC2 images allowed the identification of domains of different internal ordering within protein-crystal samples as well as differentiation between multi-domain conglomerated crystals and single crystals. PR-SHG assessments of crystalline domains were in good agreement with spatially resolved synchrotron X-ray diffraction measurements. These results have implications for improving the productive throughput of protein structure determination through early identification of multi-domain crystals. PMID:23275165

Improving aluminum particle reactivity by annealing and quenching treatments: Synchrotron X-ray diffraction analysis of strain

DOE PAGES

McCollum, Jena; Pantoya, Michelle L.; Tamura, Nobumichi

2015-11-06

In bulk material processing, annealing and quenching metals such as aluminum (Al) can improve mechanical properties. On a single particle level, affecting mechanical properties may also affect Al particle reactivity. Our study examines the effect of annealing and quenching on the strain of Al particles and the corresponding reactivity of aluminum and copper oxide (CuO) composites. Micron-sized Al particles were annealed and quenched according to treatments designed to affect Al mechanical properties. Furthermore, synchrotron X-ray diffraction (XRD) analysis of the particles reveals that thermal treatment increased the dilatational strain of the aluminum-core, alumina-shell particles. Flame propagation experiments also show thermalmore » treatments effect reactivity when combined with CuO. An effective annealing and quenching treatment for increasing aluminum reactivity was identified. Our results show that altering the mechanical properties of Al particles affects their reactivity.« less

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

Study of the mechanical behavior of the hydride blister/rim structure in Zircaloy-4 using in-situ synchrotron X-ray diffraction

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

Lin, Jun-li; Han, Xiaochun; Heuser, Brent J.

2016-04-01

High-energy synchrotron X-ray diffraction was utilized to study the mechanical response of the f.c.c delta hydride phase, the intermetallic precipitation with hexagonal C14 lave phase and the alpha-Zr phase in the Zircaloy-4 materials with a hydride rim/blister structure near one surface of the material during in-situ uniaxial tension experiment at 200 degrees C. The f.c.c delta was the only hydride phase observed in the rim/blister structure. The conventional Rietveld refinement was applied to measure the macro-strain equivalent response of the three phases. Two regions were delineated in the applied load versus lattice strain measurement: a linear elastic strain region andmore » region that exhibited load partitioning. Load partitioning was quantified by von Mises analysis. The three phases were observed to have similar elastic modulus at 200 degrees C.« less

Validating a Model for Welding Induced Residual Stress Using High-Energy X-ray Diffraction

NASA Astrophysics Data System (ADS)

Mach, J. C.; Budrow, C. J.; Pagan, D. C.; Ruff, J. P. C.; Park, J.-S.; Okasinski, J.; Beaudoin, A. J.; Miller, M. P.

2017-05-01

Integrated computational materials engineering (ICME) provides a pathway to advance performance in structures through the use of physically-based models to better understand how manufacturing processes influence product performance. As one particular challenge, consider that residual stresses induced in fabrication are pervasive and directly impact the life of structures. For ICME to be an effective strategy, it is essential that predictive capability be developed in conjunction with critical experiments. In the present work, simulation results from a multi-physics model for gas metal arc welding are evaluated through x-ray diffraction using synchrotron radiation. A test component was designed with intent to develop significant gradients in residual stress, be representative of real-world engineering application, yet remain tractable for finely spaced strain measurements with positioning equipment available at synchrotron facilities. The experimental validation lends confidence to model predictions, facilitating the explicit consideration of residual stress distribution in prediction of fatigue life.

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).

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.

Synchrotron-radiation phase-contrast imaging of human stomach and gastric cancer: in vitro studies.

PubMed

Tang, Lei; Li, Gang; Sun, Ying-Shi; Li, Jie; Zhang, Xiao-Peng

2012-05-01

The electron density resolution of synchrotron-radiation phase-contrast imaging (SR-PCI) is 1000 times higher than that of conventional X-ray absorption imaging in light elements, through which high-resolution X-ray imaging of biological soft tissue can be achieved. For biological soft tissue, SR-PCI can give better imaging contrast than conventional X-ray absorption imaging. In this study, human resected stomach and gastric cancer were investigated using in-line holography and diffraction enhanced imaging at beamline 4W1A of the Beijing Synchrotron Radiation Facility. It was possible to depict gastric pits, measuring 50-70 µm, gastric grooves and tiny blood vessels in the submucosa layer by SR-PCI. The fine structure of a cancerous ulcer was displayed clearly on imaging the mucosa. The delamination of the gastric wall and infiltration of cancer in the submucosa layer were also demonstrated on cross-sectional imaging. In conclusion, SR-PCI can demonstrate the subtle structures of stomach and gastric cancer that cannot be detected by conventional X-ray absorption imaging, which prompt the X-ray diagnosis of gastric disease to the level of the gastric pit, and has the potential to provide new methods for the imageology of gastric cancer.

Variable Magnification With Kirkpatrick-Baez Optics for Synchrotron X-Ray Microscopy

PubMed Central

Jach, Terrence; Bakulin, Alex S.; Durbin, Stephen M.; Pedulla, Joseph; Macrander, Albert

2006-01-01

We describe the distinction between the operation of a short focal length x-ray microscope forming a real image with a laboratory source (convergent illumination) and with a highly collimated intense beam from a synchrotron light source (Köhler illumination). We demonstrate the distinction with a Kirkpatrick-Baez microscope consisting of short focal length multilayer mirrors operating at an energy of 8 keV. In addition to realizing improvements in the resolution of the optics, the synchrotron radiation microscope is not limited to the usual single magnification at a fixed image plane. Higher magnification images are produced by projection in the limit of geometrical optics with a collimated beam. However, in distinction to the common method of placing the sample behind the optical source of a diverging beam, we describe the situation in which the sample is located in the collimated beam before the optical element. The ultimate limits of this magnification result from diffraction by the specimen and are determined by the sample position relative to the focal point of the optic. We present criteria by which the diffraction is minimized. PMID:27274930

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.

Purification, crystallization and preliminary crystallographic analysis of biotin protein ligase from Staphylococcus aureus.

PubMed

Pendini, Nicole R; Polyak, Steve W; Booker, Grant W; Wallace, John C; Wilce, Matthew C J

2008-06-01

Biotin protein ligase from Staphylococcus aureus catalyses the biotinylation of acetyl-CoA carboxylase and pyruvate carboxylase. Recombinant biotin protein ligase from S. aureus has been cloned, expressed and purified. Crystals were grown using the hanging-drop vapour-diffusion method using PEG 8000 as the precipitant at 295 K. X-ray diffraction data were collected to 2.3 A resolution from crystals using synchrotron X-ray radiation at 100 K. The diffraction was consistent with the tetragonal space group P4(2)2(1)2, with unit-cell parameters a = b = 93.665, c = 131.95.

X-ray induced chemical reaction revealed by in-situ X-ray diffraction and scanning X-ray microscopy in 15 nm resolution (Conference Presentation)

NASA Astrophysics Data System (ADS)

Ge, Mingyuan; Liu, Wenjun; Bock, David; De Andrade, Vincent; Yan, Hanfei; Huang, Xiaojing; Marschilok, Amy; Takeuchi, Esther; Xin, Huolin; Chu, Yong S.

2016-09-01

The detection sensitivity of synchrotron-based X-ray techniques has been largely improved due to the ever increasing source brightness, which have significantly advanced ex-situ and in-situ research for energy materials, such as lithium-ion batteries. However, the strong beam-matter interaction arisen from the high beam flux can significantly modify the material structure. The parasitic beam-induced effect inevitably interferes with the intrinsic material property, which brings difficulties in interpreting experimental results, and therefore requires comprehensive evaluation. Here we present a quantitative in-situ study of the beam-effect on one electrode material Ag2VO2PO4 using four different X-ray probes with different radiation dose rate. The material system we reported exhibits interesting and reversible radiation-induced thermal and chemical reactions, which was further evaluated under electron microscopy to illustrate the underlying mechanism. The work we presented here will provide a guideline in using synchrotron X-rays to distinguish the materials' intrinsic behavior from extrinsic structure changed induced by X-rays, especially in the case of in-situ and operando study where the materials are under external field of either temperature or electric field.

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.

Nanox: a miniature mechanical stress rig designed for near-field X-ray diffraction imaging techniques.

PubMed

Gueninchault, N; Proudhon, H; Ludwig, W

2016-11-01

Multi-modal characterization of polycrystalline materials by combined use of three-dimensional (3D) X-ray diffraction and imaging techniques may be considered as the 3D equivalent of surface studies in the electron microscope combining diffraction and other imaging modalities. Since acquisition times at synchrotron sources are nowadays compatible with four-dimensional (time lapse) studies, suitable mechanical testing devices are needed which enable switching between these different imaging modalities over the course of a mechanical test. Here a specifically designed tensile device, fulfilling severe space constraints and permitting to switch between X-ray (holo)tomography, diffraction contrast tomography and topotomography, is presented. As a proof of concept the 3D characterization of an Al-Li alloy multicrystal by means of diffraction contrast tomography is presented, followed by repeated topotomography characterization of one selected grain at increasing levels of deformation. Signatures of slip bands and sudden lattice rotations inside the grain have been shown by means of in situ topography carried out during the load ramps, and diffraction spot peak broadening has been monitored throughout the experiment.

Nanox: a miniature mechanical stress rig designed for near-field X-ray diffraction imaging techniques

PubMed Central

Gueninchault, N.; Proudhon, H.; Ludwig, W.

2016-01-01

Multi-modal characterization of polycrystalline materials by combined use of three-dimensional (3D) X-ray diffraction and imaging techniques may be considered as the 3D equivalent of surface studies in the electron microscope combining diffraction and other imaging modalities. Since acquisition times at synchrotron sources are nowadays compatible with four-dimensional (time lapse) studies, suitable mechanical testing devices are needed which enable switching between these different imaging modalities over the course of a mechanical test. Here a specifically designed tensile device, fulfilling severe space constraints and permitting to switch between X-ray (holo)tomography, diffraction contrast tomography and topotomography, is presented. As a proof of concept the 3D characterization of an Al–Li alloy multicrystal by means of diffraction contrast tomography is presented, followed by repeated topotomography characterization of one selected grain at increasing levels of deformation. Signatures of slip bands and sudden lattice rotations inside the grain have been shown by means of in situ topography carried out during the load ramps, and diffraction spot peak broadening has been monitored throughout the experiment. PMID:27787253

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

Shayduk, Roman; Vonk, Vedran; Strempfer, Jörg

We report on the quantitative determination of the transient surface temperature of Pt(110) upon nanosecond laser pulse heating. We find excellent agreement between heat transport theory and the experimentally determined transient surface temperature as obtained from time-resolved X-ray diffraction on timescales from hundred nanoseconds to milliseconds. Exact knowledge of the surface temperature's temporal evolution after laser excitation is crucial for future pump-probe experiments at synchrotron storage rings and X-ray free electron lasers.

Penetration Depth and Defect Image Contrast Formation in Grazing-Incidence X-ray Topography of 4H-SiC Wafers

NASA Astrophysics Data System (ADS)

Yang, Yu; Guo, Jianqiu; Goue, Ouloide Yannick; Kim, Jun Gyu; Raghothamachar, Balaji; Dudley, Michael; Chung, Gill; Sanchez, Edward; Manning, Ian

2018-02-01

Synchrotron x-ray topography in grazing-incidence geometry is useful for discerning defects at different depths below the crystal surface, particularly for 4H-SiC epitaxial wafers. However, the penetration depths measured from x-ray topographs are much larger than theoretical values. To interpret this discrepancy, we have simulated the topographic contrast of dislocations based on two of the most basic contrast formation mechanisms, viz. orientation and kinematical contrast. Orientation contrast considers merely displacement fields associated with dislocations, while kinematical contrast considers also diffraction volume, defined as the effective misorientation around dislocations and the rocking curve width for given diffraction vector. Ray-tracing simulation was carried out to visualize dislocation contrast for both models, taking into account photoelectric absorption of the x-ray beam inside the crystal. The results show that orientation contrast plays the key role in determining both the contrast and x-ray penetration depth for different types of dislocation.

Study of the specific features of single-crystal boron microstructure

NASA Astrophysics Data System (ADS)

Blagov, A. E.; Vasil'ev, A. L.; Dmitriev, V. P.; Ivanova, A. G.; Kulikov, A. G.; Marchenkov, N. V.; Popov, P. A.; Presnyakov, M. Yu.; Prosekov, P. A.; Pisarevskii, Yu. V.; Targonskii, A. V.; Chernaya, T. S.; Chernyshov, D. Yu.

2017-09-01

A complex study of the structure of β-boron single crystal grown by the floating-zone method, with sizes significantly exceeding the analogs known in the literature, has been performed. The study includes X-ray diffraction analysis and X-ray diffractometry (measurement of pole figures and rocking curves), performed on both laboratory and synchrotron sources; atomic-resolution scanning transmission electron microscopy with spherical aberration correction; and energy-dispersive microanalysis. X-ray diffraction analysis using synchrotron radiation has been used to refine the β-boron structure and find impurity Si atoms. The relative variations in the unit-cell parameters a and c for the crystal bulk are found to be δ a/ a ≈ 0.4 and δ c/ c ≈ 0.1%. X-ray diffractometry has revealed that the single-crystal growth axis coincides with the [2\\bar 2013] crystallographic axis and makes an angle of 21.12° with the [0001] threefold axis. Electron microscopy data have confirmed that the sample under study is a β-boron crystal, which may contain 0.3-0.4 at % Si as an impurity. Planar defects (stacking faults and dislocations) are found. The results of additional measurements of the temperature dependence of the thermal conductivity of the crystal in the range of 50-300 K are indicative of its high structural quality.

LPE grown LSO:Tb scintillator films for high-resolution X-ray imaging applications at synchrotron light sources

NASA Astrophysics Data System (ADS)

Cecilia, A.; Rack, A.; Douissard, P.-A.; Martin, T.; Dos Santos Rolo, T.; Vagovič, P.; Hamann, E.; van de Kamp, T.; Riedel, A.; Fiederle, M.; Baumbach, T.

2011-08-01

Within the project ScinTAX of the 6th framework program (FP6) of the European Commission (SCINTAX—STRP 033 427) we have developed a new thin single crystal scintillator for high-resolution X-ray imaging. The scintillator is based on a Tb-doped Lu2SiO5 (LSO) film epitaxially grown on an adapted substrate. The high density, effective atomic number and light yield of the scintillating LSO significantly improves the efficiency of the X-ray imaging detectors currently used in synchrotron micro-imaging applications. In this work we present the characterization of the scintillating LSO films in terms of their spatial resolution performance and we provide two examples of high spatial and high temporal resolution applications.

Micro and Nano Systems for Space Exploration

NASA Technical Reports Server (NTRS)

Manohara, Harish

2007-01-01

This slide presentation reviews the use of micro and nano systems in Space exploration. Included are: an explanation of the rationales behind nano and micro technologies for space exploration, a review of how the devices are fabricated, including details on lithography with more information on Electron Beam (E-Beam) lithography, and X-ray lithography, a review of micro gyroscopes and inchworm Microactuator as examples of the use of MicroElectoMechanical (MEMS) technology. Also included is information on Carbon Nanotubes, including a review of the CVD growth process. These micro-nano systems have given rise to the next generation of miniature X-ray Diffraction, X-ray Fluorescence instruments, mass spectrometers, and terahertz frequency vacuum tube oscillators and amplifiers, scanning electron microscopes and energy dispersive x-ray spectroscope. The nanotechnology has also given rise to coating technology, such as silicon nanotip anti-reflection coating.

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.

Purification, crystallization and preliminary X-ray diffraction studies of UDP-N-acetylglucosamine pyrophosphorylase from Candida albicans

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

Maruyama, Daisuke; Nishitani, Yuichi; Nonaka, Tsuyoshi

2006-12-01

UDP-N-acetylglucosamine pyrophosphorylase was purified and crystallized and X-ray diffraction data were collected to 2.3 Å resolution. UDP-N-acetylglucosamine pyrophosphorylase (UAP) is an essential enzyme in the synthesis of UDP-N-acetylglucosamine. UAP from Candida albicans was purified and crystallized by the sitting-drop vapour-diffusion method. The crystals of the substrate and product complexes both diffract X-rays to beyond 2.3 Å resolution using synchrotron radiation. The crystals of the substrate complex belong to the triclinic space group P1, with unit-cell parameters a = 47.77, b = 62.89, c = 90.60 Å, α = 90.01, β = 97.72, γ = 92.88°, whereas those of the productmore » complex belong to the orthorhombic space group P2{sub 1}2{sub 1}2{sub 1}, with unit-cell parameters a = 61.95, b = 90.87, c = 94.88 Å.« less

Phase retrieval for crystalline specimens

NASA Astrophysics Data System (ADS)

Arnal, Romain A.; Millane, Rick P.

2017-09-01

The recent availability of ultra-bright and ultra-short X-rays pulses from new sources called x-ray free-electron lasers (XFELs) has introduced a new paradigm in X-ray crystallography. Called "diffraction-before-destruction," this paradigm addresses the main problems that plague crystallography using synchrotron sources. However, the phase problem of coherent diffraction imaging remains: one has to retrieve the phase of the measured diffraction amplitude in order to reconstruct the object. Fibrous and membrane proteins that crystallize in 1D and 2D crystals can now potentially be used for data collection with free-electron lasers. The crystallographic phase problem with such crystalline specimens is eased as the Fourier amplitude can be sampled more finely than at the Bragg sampling along one or two directions. Here we characterise uniqueness of the phase problem for different types of crystalline specimen. Simulated ab initio phase retrieval using iterative projection algorithms for 2D crystals is presented.

Crystallization and preliminary X-ray diffraction study of recombinant ribokinase from Thermus Species 2.9

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

Abramchik, Yu. A.; Timofeev, V. I., E-mail: tostars@mail.ru; Muravieva, T. I.

2016-11-15

Ribokinase from a thermophilic strain of Thermus species 2.9 belonging to the carbohydrate ribokinase family (EC 2.7.1.15) was isolated, purified, and crystallized. The crystallization conditions were found by the vapor-diffusion technique and were then optimized to apply the capillary counter-diffusion technique. The X-ray diffraction data set was collected from the crystals, which were grown by the counter-diffusion technique, at the SPring-8 synchrotron radiation facility to 2.87 Å resolution. The crystals belong to sp. gr. P12{sub 1}1 and have the following unit-cell parameters: a = 81.613 Å, b = 156.132 Å, c = 87.714 Å, α = γ = 90°, βmore » = 103.819°. The X-ray diffraction data set is suitable for determining the three-dimensional structure of the protein by the molecular-replacement method.« less

Mechanisms of Arsenic Sequestration by Prosopis juliflora during the Phytostabilization of Metalliferous Mine Tailings.

PubMed

Hammond, Corin M; Root, Robert A; Maier, Raina M; Chorover, Jon

2018-02-06

Phytostabilization is a cost-effective long-term bioremediation technique for the immobilization of metalliferous mine tailings. However, the biogeochemical processes affecting metal(loid) molecular stabilization and mobility in the root zone remain poorly resolved. The roots of Prosopis juliflora grown for up to 36 months in compost-amended pyritic mine tailings from a federal Superfund site were investigated by microscale and bulk synchrotron X-ray absorption spectroscopy (XAS) and multiple energy micro-X-ray fluorescence imaging to determine iron, arsenic, and sulfur speciation, abundance, and spatial distribution. Whereas ferrihydrite-bound As(V) species predominated in the initial bulk mine tailings, the rhizosphere speciation of arsenic was distinctly different. Root-associated As(V) was immobilized on the root epidermis bound to ferric sulfate precipitates and within root vacuoles as trivalent As(III)-(SR) 3  tris-thiolate complexes. Molar Fe-to-As ratios of root epidermis tissue were two times higher than the 15% compost-amended bulk tailings growth medium. Rhizoplane-associated ferric sulfate phases that showed a high capacity to scavenge As(V) were dissimilar from the bulk-tailings mineralogy as shown by XAS and X-ray diffraction, indicating a root-surface mechanism for their formation or accumulation.

Oxygen storage properties of La 1-xSr xFeO 3-δ for chemical-looping reactions–An in-situ neutron and synchrotron X-ray study

DOE PAGES

Taylor, Daniel D.; Schreiber, Nathaniel J.; Levitas, Benjamin D.; ...

2016-05-16

Oxygen storage materials (OSMs) provide lattice oxygen for a number of chemical-looping reactions including natural gas combustion and methane reforming. La 1–xSr xFeO 3-δ has shown promise for use as an OSM in methane reforming reactions due to its high product selectivity, fast oxide diffusion, and cycle stability. Here, we investigate the structural evolution of the series La 1–xSr xFeO 3-δ for x = 0, 1/3, 1/2, 2/3, and 1, using in situ synchrotron X-ray and neutron diffraction, as it is cycled under the conditions of a chemical-looping reactor (methane and oxygen atmospheres). In the compositions x = 1/3, 1/2,more » 2/3, and 1, we discover an envelope , or temperature range, of oxygen storage capacity (OSC), where oxygen can easily and reversibly be inserted and removed from the OSM. Our in situ X-ray and neutron diffraction results reveal that while samples with higher Sr contents had a higher OSC, those same samples suffered from slower reaction kinetics and some, such as the x = 1/2 and x = 2/3 compositions, had local variations in Sr content, which led to inhomogeneous regions with varying reaction rates. Therefore, we highlight the importance of in situ diffraction studies, and we propose that these measurements are required for the thorough evaluation of future candidate OSMs. Furthermore, we recommend La 2/3Sr 1/3FeO 3-δ as the optimal OSM in the series because its structure remains homogeneous throughout the reaction, and its OSC envelope is similar to that of the higher doped materials.« less

Perfect X-ray focusing via fitting corrective glasses to aberrated optics.

PubMed

Seiboth, Frank; Schropp, Andreas; Scholz, Maria; Wittwer, Felix; Rödel, Christian; Wünsche, Martin; Ullsperger, Tobias; Nolte, Stefan; Rahomäki, Jussi; Parfeniukas, Karolis; Giakoumidis, Stylianos; Vogt, Ulrich; Wagner, Ulrich; Rau, Christoph; Boesenberg, Ulrike; Garrevoet, Jan; Falkenberg, Gerald; Galtier, Eric C; Ja Lee, Hae; Nagler, Bob; Schroer, Christian G

2017-03-01

Due to their short wavelength, X-rays can in principle be focused down to a few nanometres and below. At the same time, it is this short wavelength that puts stringent requirements on X-ray optics and their metrology. Both are limited by today's technology. In this work, we present accurate at wavelength measurements of residual aberrations of a refractive X-ray lens using ptychography to manufacture a corrective phase plate. Together with the fitted phase plate the optics shows diffraction-limited performance, generating a nearly Gaussian beam profile with a Strehl ratio above 0.8. This scheme can be applied to any other focusing optics, thus solving the X-ray optical problem at synchrotron radiation sources and X-ray free-electron lasers.

Synchrotron micro-scale study of trace metal transport and distribution in Spartina alterniflora root system in Yangtze River intertidal zone

DOE PAGES

Feng, Huan; Tappero, Ryan; Zhang, Weiguo; ...

2015-07-26

This study is focused on micro-scale measurement of metal (Ca, Cl, Fe, K, Mn, Cu, Pb, and Zn) distributions in Spartina alterniflora root system. The root samples were collected in the Yangtze River intertidal zone in July 2013. Synchrotron X-ray fluorescence (XRF), computed microtomography (CMT), and X-ray absorption near-edge structure (XANES) techniques, which provide micro-meter scale analytical resolution, were applied to this study. Although it was found that the metals of interest were distributed in both epidermis and vascular tissue with the varying concentrations, the results showed that Fe plaque was mainly distributed in the root epidermis. Other metals (e.g.,more » Cu, Mn, Pb, and Zn) were correlated with Fe in the epidermis possibly due to scavenge by Fe plaque. Relatively high metal concentrations were observed in the root hair tip. As a result, this micro-scale investigation provides insights of understanding the metal uptake and spatial distribution as well as the function of Fe plaque governing metal transport in the root system.« less

[Distribution and speciation of Pb in Arabidopsis thaliana shoot and rhizosphere soil by in situ synchrotron radiation micro X-ray fluorescence and X-ray absorption near edge structure].

PubMed

Shen, Ya-Ting

2014-03-01

In order to investigate plant reacting mechanism with heavy metal stress in organ and tissue level, synchrotron radiation micro X-ray fluorescence (micro-SRXRF) was used to determine element distribution characteristics of K, Ca, Mn, Fe, Cu, Zn, Pb in an Arabidopsis thaliana seedling grown in tailing dam soil taken from a lead-zinc mine exploration area. The results showed a regular distribution characters of K, Ca, Fe, Cu and Zn, while Pb appeared not only in root, but also in a leaf bud which was beyond previously understanding that Pb mainly appeared in plant root. Pb competed with Mn in the distribution of the whole seedling. Pb may cause the increase of oxidative stress in root and leaf bud, and restrict Mn absorption and utilization which explained the phenomenon of seedling death in this tailing damp soil. Speciation of Pb in Arabidopsis thaliana and tailing damp rhizosphere soil were also presented after using PbL3 micro X-ray absorption near edge structure (micro-XANES). By comparison of PbL3 XANES peak shape and peak position between standard samples and rhizosphere soil sample, it was demonstrated that the tailing damp soil was mainly formed by amorphous forms like PbO (64.2%), Pb (OH)2 (28.8%) and Pb3O4 (6.3%) rather than mineral or organic Pb speciations. The low plant bioavailability of Pb demonstrated a further research focusing on Pb absorption and speciation conversion is needed, especially the role of dissolve organic matter in soil which may enhance Pb bioavailability.

Using synchrotron X-ray phase-contrast micro-computed tomography to study tissue damage by laser irradiation.

PubMed

Robinson, Alan M; Stock, Stuart R; Soriano, Carmen; Xiao, Xianghui; Richter, Claus-Peter

2016-11-01

The aim of this study was to determine if X-ray micro-computed tomography could be used to locate and characterize tissue damage caused by laser irradiation and to describe its advantages over classical histology for this application. A surgical CO 2 laser, operated in single pulse mode (100 milliseconds) at different power settings, was used to ablate different types of cadaveric animal tissues. Tissue samples were then harvested and imaged with synchrotron X-ray phase-contrast and micro-computed tomography to generate stacks of virtual sections of the tissues. Subsequently, Fiji (ImageJ) software was used to locate tissue damage, then to quantify volumes of laser ablation cones and thermal coagulation damage from 3D renderings of tissue image stacks. Visual comparisons of tissue structures in X-ray images with those visible by classic light microscopy histology were made. We demonstrated that micro-computed tomography could be used to rapidly identify areas of surgical laser ablation, vacuolization, carbonization, and thermally coagulated tissue. Quantification and comparison of the ablation crater, which represents the volume of ablated tissue, and the thermal coagulation zone volumes were performed faster than we could by classical histology. We demonstrated that these procedures can be performed on fresh hydrated and non-sectioned plastic embedded tissue. We demonstrated that the application of non-destructive micro-computed tomography to the visualization and analysis of laser induced tissue damage without tissue sectioning is possible. This will improve evaluation of new surgical lasers and their corresponding effect on tissues. Lasers Surg. Med. 48:866-877, 2016. © 2016 Wiley Periodicals, Inc. © 2016 Wiley Periodicals, Inc.

Visualisation by high resolution synchrotron X-ray phase contrast micro-tomography of gas films on submerged superhydrophobic leaves.

PubMed

Lauridsen, Torsten; Glavina, Kyriaki; Colmer, Timothy David; Winkel, Anders; Irvine, Sarah; Lefmann, Kim; Feidenhans'l, Robert; Pedersen, Ole

2014-10-01

Floods can completely submerge terrestrial plants but some wetland species can sustain O2 and CO2 exchange with the environment via gas films forming on superhydrophobic leaf surfaces. We used high resolution synchrotron X-ray phase contrast micro-tomography in a novel approach to visualise gas films on submerged leaves of common cordgrass (Spartina anglica). 3D tomograms enabled a hitherto unmatched level of detail regarding the micro-topography of leaf gas films. Gas films formed only on the superhydrophobic adaxial leaf side (water droplet contact angle, Φ=162°) but not on the abaxial side (Φ=135°). The adaxial side of the leaves of common cordgrass is plicate with a longitudinal system of parallel grooves and ridges and the vast majority of the gas film volume was found in large ∼180μm deep elongated triangular volumes in the grooves and these volumes were connected to each neighbouring groove via a fine network of gas tubules (∼1.7μm diameter) across the ridges. In addition to the gas film retained on the leaf exterior, the X-ray phase contrast micro-tomography also successfully distinguished gas spaces internally in the leaf tissues, and the tissue porosity (gas volume per unit tissue volume) ranged from 6.3% to 20.3% in tip and base leaf segments, respectively. We conclude that X-ray phase contrast micro-tomography is a powerful tool to obtain quantitative data of exterior gas features on biological samples because of the significant difference in electron density between air, biological tissues and water. Copyright © 2014 Elsevier Inc. All rights reserved.

Structural-electrochemical relations in the aqueous copper hexacyanoferrate-zinc system examined by synchrotron X-ray diffraction

NASA Astrophysics Data System (ADS)

Renman, Viktor; Ojwang, Dickson O.; Valvo, Mario; Gómez, Cesar Pay; Gustafsson, Torbjörn; Svensson, Gunnar

2017-11-01

The storage process of Zn2+ in the Prussian blue analogue (PBA) copper hexacyanoferrate (Cu[Fe(CN)6]2/3·nH2O - CuHCF) framework structure in a context of rechargeable aqueous batteries is examined by means of in operando synchrotron X-ray diffraction. Via sequential unit-cell parameter refinements of time-resolved diffraction data, it is revealed that the step-profile of the cell output voltage curves during repeated electrochemical insertion and removal of Zn2+ in the CuHCF host structure is associated with a non-linear contraction and expansion of the unit-cell in the range 0.36 < x < 1.32 for Znx/3Cu[Fe(CN)6]2/3·nH2O. For a high insertion cation content there is no apparent change in the unit-cell contraction. Furthermore, a structural analysis with respect to the occupancies of possible Zn2+ sites suggests that the Fe(CN)6 vacancies within the CuHCF framework play an important role in the structural-electrochemical behavior of this particular system. More specifically, it is observed that Zn2+ swaps position during electrochemical cycling, hopping between cavity sites to vacant ferricyanide sites.

Negative thermal expansion and magnetoelastic coupling in the breathing pyrochlore lattice material LiGaCr 4 S 8

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

Pokharel, G.; May, A. F.; Parker, D. S.

In this paper, the physical properties of the spinel LiGaCr 4S 8 have been studied with neutron diffraction, x-ray diffraction, magnetic susceptibility, and heat capacity measurements. The neutron diffraction and synchrotron x-ray diffraction data reveal negative thermal expansion (NTE) below 111(4) K. The magnetic susceptibility deviates from Curie-Weiss behavior with the onset of NTE. At low temperature a broad peak in the magnetic susceptibility at 10.3(3) K is accompanied by the return of normal thermal expansion. First-principles calculations find a strong coupling between the lattice and the simulated magnetic ground state. Finally, these results indicate strong magnetoelastic coupling in LiGaCrmore » 4S 8.« less

Negative thermal expansion and magnetoelastic coupling in the breathing pyrochlore lattice material LiGaCr 4 S 8

DOE PAGES

Pokharel, G.; May, A. F.; Parker, D. S.; ...

2018-04-30

In this paper, the physical properties of the spinel LiGaCr 4S 8 have been studied with neutron diffraction, x-ray diffraction, magnetic susceptibility, and heat capacity measurements. The neutron diffraction and synchrotron x-ray diffraction data reveal negative thermal expansion (NTE) below 111(4) K. The magnetic susceptibility deviates from Curie-Weiss behavior with the onset of NTE. At low temperature a broad peak in the magnetic susceptibility at 10.3(3) K is accompanied by the return of normal thermal expansion. First-principles calculations find a strong coupling between the lattice and the simulated magnetic ground state. Finally, these results indicate strong magnetoelastic coupling in LiGaCrmore » 4S 8.« less

Development of X-ray CCD camera based X-ray micro-CT system

NASA Astrophysics Data System (ADS)

Sarkar, Partha S.; Ray, N. K.; Pal, Manoj K.; Baribaddala, Ravi; Agrawal, Ashish; Kashyap, Y.; Sinha, A.; Gadkari, S. C.

2017-02-01

Availability of microfocus X-ray sources and high resolution X-ray area detectors has made it possible for high resolution microtomography studies to be performed outside the purview of synchrotron. In this paper, we present the work towards the use of an external shutter on a high resolution microtomography system using X-ray CCD camera as a detector. During micro computed tomography experiments, the X-ray source is continuously ON and owing to the readout mechanism of the CCD detector electronics, the detector registers photons reaching it during the read-out period too. This introduces a shadow like pattern in the image known as smear whose direction is defined by the vertical shift register. To resolve this issue, the developed system has been incorporated with a synchronized shutter just in front of the X-ray source. This is positioned in the X-ray beam path during the image readout period and out of the beam path during the image acquisition period. This technique has resulted in improved data quality and hence the same is reflected in the reconstructed images.

Structure of Se-Te glasses studied using neutron, X-ray diffraction and reverse Monte Carlo modelling

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

Itoh, Keiji, E-mail: itoh@okayama-u.ac.jp; Research Reactor Institute, Kyoto University, Kumatori, Osaka 590-0494

Pulsed neutron diffraction and synchrotron X-ray diffraction measurements were performed on Se{sub 100-x}Te{sub x} bulk glasses with x=10, 20, 30 and 40. The coordination numbers obtained from the diffraction results demonstrate that Se and Te atoms are twofold coordinated and the glass structure is formed by the chain network. The three-dimensional structure model for Se{sub 60}Te{sub 40} glass obtained by using reverse Monte Carlo modelling shows that the alternating arrangements of Se and Te atoms compose the major part of the chain clusters but several other fragments such as Se{sub n} chains and Te-Te dimers are also present in largemore » numbers. The chain clusters have geometrically disordered forms and the interchain atomic order is different from those in the crystal structures of trigonal Se and trigonal Te. - Graphical abstract: Coordination environment in Se{sub 60}Te{sub 40} glass.« less

Preliminary studies of enhanced contrast radiography in anatomy and embryology of insects with Elettra synchrotron light

NASA Astrophysics Data System (ADS)

Hönnicke, M. G.; Foerster, L. A.; Navarro-Silva, M. A.; Menk, R.-H.; Rigon, L.; Cusatis, C.

2005-08-01

Enhanced contrast X-ray imaging is achieved by exploiting the real part of the refraction index, which is responsible for the phase shifts, in addition to the imaginary part, which is responsible for the absorption. Such techniques are called X-ray phase contrast imaging. An analyzer-based X-ray phase contrast imaging set-up with Diffraction Enhanced Imaging processing (DEI) were used for preliminary studies in anatomy and embryology of insects. Parasitized stinkbug and moth eggs used as control agents of pests in vegetables and adult stinkbugs and mosquitoes ( Aedes aegypti) were used as samples. The experimental setup was mounted in the SYRMEP beamline at ELETTRA. Images were obtained using a high spatial resolution CCD detector (pixel size 14×14 μm 2) coupled with magnifying optics. Analyzer-based X-ray phase contrast images (PCI) and edge detection images show contrast and details not observed with conventional synchrotron radiography and open the possibility for future study in the embryonic development of insects.

Determination of surface morphology of TiO2 nanostructure using synchrotron radiation

NASA Astrophysics Data System (ADS)

Das, Gangadhar; Kumar, Manoj; Biswas, A. K.; Khooha, Ajay; Mondal, Puspen; Tiwari, M. K.

2017-05-01

Nanostructures of Titanium oxide (TiO2) are being studied for many promising applications, e.g., solar photovoltaics, solar water splitting for H2 fuel generation etc., due to their excellent photo-catalytic properties. We have synthesized low-dimensional TiO2 nanoparticles by gas phase CW CO2 laser pyrolysis. The laser synthesis process has been optimized for the deposition of highly pure, nearly mono-dispersed TiO2 nanoparticles on silicon substrates. Hard x-ray standing wave-field (XSW) measurements in total reflection geometry were carried out on the BL-16 beamline of Indus-2 synchrotron radiation facility in combination with x-ray reflectivity and grazing incidence x-ray fluorescence measurements for the determination of surface morphology of the deposited TiO2 nanostructures. The average particle size of TiO2 nanostructure estimated using transmission electron microscopy (TEM) was found to closely agree with the XSW and grazing incidence x-ray diffraction (GIXRD) results.

X-ray optical simulations supporting advanced commissioning of the coherent hard x-ray beamline at NSLS-II

NASA Astrophysics Data System (ADS)

Wiegart, L.; Rakitin, M.; Fluerasu, A.; Chubar, O.

2017-08-01

We present the application of fully- and partially-coherent synchrotron radiation wavefront propagation simulation functions, implemented in the "Synchrotron Radiation Workshop" computer code, to create a `virtual beamline' mimicking the Coherent Hard X-ray scattering beamline at NSLS-II. The beamline simulation includes all optical beamline components, such as the insertion device, mirror with metrology data, slits, double crystal monochromator and refractive focusing elements (compound refractive lenses and kinoform lenses). A feature of this beamline is the exploitation of X-ray beam coherence, boosted by the low-emittance NSLS-II storage-ring, for techniques such as X-ray Photon Correlation Spectroscopy or Coherent Diffraction Imaging. The key performance parameters are the degree of Xray beam coherence and photon flux, and the trade-off between them needs to guide the beamline settings for specific experimental requirements. Simulations of key performance parameters are compared to measurements obtained during beamline commissioning, and include the spectral flux of the undulator source, the degree of transverse coherence as well as focal spot sizes.

Identification of ancient textile fibres from Khirbet Qumran caves using synchrotron radiation microbeam diffraction

NASA Astrophysics Data System (ADS)

Müller, Martin; Murphy, Bridget; Burghammer, Manfred; Riekel, Christian; Roberts, Mark; Papiz, Miroslav; Clarke, David; Gunneweg, Jan; Pantos, Emmanuel

2004-10-01

Archaeological textiles fragments from the caves of Qumran in the Dead Sea region were investigated by means of X-ray microbeam diffraction on single fibres. This non-destructive technique made the identification of the used plant textile fibres possible. Apart from bast fibres (mainly flax), cotton was identified which was most unexpected in the archaeological context.

Broadband X-ray edge-enhancement imaging of a boron fibre on lithium fluoride thin film detector

NASA Astrophysics Data System (ADS)

Nichelatti, E.; Bonfigli, F.; Vincenti, M. A.; Cecilia, A.; Vagovič, P.; Baumbach, T.; Montereali, R. M.

2016-10-01

The white beam (∼6-80 keV) available at the TopoTomo X-ray beamline of the ANKA synchrotron facility (KIT, Karlsruhe, Germany) was used to perform edge-enhancement imaging tests on lithium fluoride radiation detectors. The diffracted X-ray image of a microscopic boron fibre, consisting of tungsten wire wrapped by boron cladding, was projected onto lithium fluoride thin films placed at several distances, from contact to 1 m . X-ray photons cause the local formation of primary and aggregate colour centres in lithium fluoride; these latter, once illuminated under blue light, luminesce forming visible-light patterns-acquired by a confocal laser scanning microscope-that reproduce the intensity of the X-ray diffracted images. The tests demonstrated the excellent performances of lithium fluoride films as radiation detectors at the investigated photon energies. The experimental results are here discussed and compared with those calculated with a model that takes into account all the processes that concern image formation, storing and readout.

Synchrotron-induced X-ray fluorescence from rat bone and lumber vertebra of different age groups

NASA Astrophysics Data System (ADS)

Rao, Donepudi V.; Swapna, Medasani; Cesareo, Roberto; Brunetti, Antonio; Akatsuka, Tako; Yuasa, Tetsuya; Takeda, Tohoru; Tromba, Giuliana; Gigante, Giovanni E.

2009-02-01

The fluorescence spectra from rat bones of different age groups (8, 56 and 78 weeks) and lumber vertebra were measured with 8, 10 and 12 keV synchrotron X-rays. We have utilized the new hard X-ray micro-spectroscopy beamline facility, X27A, available at NSLS with a primary beam spot size of the order of ˜10 μm. With this spatial resolution and high flux throughput, X-ray fluorescent intensities for Ca and other trace elements were measured using a liquid-nitrogen-cooled 13-element energy-dispersive high-purity germanium detector. Regarding the lumber vertebra, we acquired the fluorescence spectra from the left, right and middle portions and calcium accumulation was evaluated and compared with the other samples. We have identified the major trace elements of Ca, Ni, Fe and Zn and minor trace elements of Ti, Cr and Mn in the sample. The percentage of scattered radiation and trace element contributions from these samples were highlighted at different energies.

Line x-ray source for diffraction enhanced imaging in clinical and industrial applications

NASA Astrophysics Data System (ADS)

Wang, Xiaoqin

Mammography is one type of imaging modalities that uses a low-dose x-ray or other radiation sources for examination of breasts. It plays a central role in early detection of breast cancers. The material similarity of tumor-cell and health cell, breast implants surgery and other factors, make the breast cancers hard to visualize and detect. Diffraction enhanced imaging (DEI), first proposed and investigated by D. Chapman is a new x-ray radiographic imaging modality using monochromatic x-rays from a synchrotron source, which produced images of thick absorbing objects that are almost completely free of scatter. It shows dramatically improved contrast over standard imaging when applied to the same phantom. The contrast is based not only on attenuation but also on the refraction and diffraction properties of the sample. This imaging method may improve image quality of mammography, other medical applications, industrial radiography for non-destructive testing and x-ray computed tomography. However, the size, and cost, of a synchrotron source limits the application of the new modality to be applicable at clinical levels. This research investigates the feasibility of a designed line x-ray source to produce intensity compatible to synchrotron sources. It is composed of a 2-cm in length tungsten filament, installed on a carbon steel filament cup (backing plate), as the cathode and a stationary oxygen-free copper anode with molybdenum coating on the front surface serves as the target. Characteristic properties of the line x-ray source were computationally studied and the prototype was experimentally investigated. SIMIION code was used to computationally study the electron trajectories emanating from the filament towards the molybdenum target. A Faraday cup on the prototype device, proof-of-principle, was used to measure the distribution of electrons on the target, which compares favorably to computational results. The intensities of characteristic x-ray for molybdenum, tungsten and rhodium targets were investigated with different window materials for -30kV to -100kV applied potential. Heat loading and thermal management of the target has been investigated computationally using COMSOL code package, and experimental measurements of target temperature rise was taken via thermocouples attached to the target. Temperature measurements for low voltage, low current regime without active cooling were compared to computational results for code-experiment benchmarking. Two different phantoms were used in the simulation of DEI images, which showed that the designed x-ray source with DEI setup could produce images with significant improved contrast. The computational results, along with experimental measurements on the prototype setup, indicate the possibility of scale up to larger area x-ray source adequate for DEI applications.

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.

Characterization of biogenic ferrihydrite nanoparticles by means of SAXS, SRD and IBA methods

NASA Astrophysics Data System (ADS)

Balasoiu, M.; Kichanov, S.; Pantelica, A.; Pantelica, D.; Stolyar, S.; Iskhakov, R.; Aranghel, D.; Ionescu, P.; Badita, C. R.; Kurkin, S.; Orelovich, O.; Tiutiunikov, S.

2018-03-01

Investigations of biogenic ferrihydrite nanoparticles produced by bacteria Klebsiella oxytoca by applying small angle X-ray scattering, synchrotron radiation diffraction and ion beam analysis methods are reviewed. Different experimental data processing methods are used and analyzed.

Indus-2 X-ray lithography beamline for X-ray optics and material science applications

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

Dhamgaye, V. P., E-mail: vishal@rrcat.gov.in; Lodha, G. S., E-mail: vishal@rrcat.gov.in

2014-04-24

X-ray lithography is an ideal technique by which high aspect ratio and high spatial resolution micro/nano structures are fabricated using X-rays from synchrotron radiation source. The technique has been used for fabricating optics (X-ray, visible and infrared), sensors and actuators, fluidics and photonics. A beamline for X-ray lithography is operational on Indus-2. The beamline offers wide lithographic window from 1-40keV photon energy and wide beam for producing microstructures in polymers upto size ∼100mm × 100mm. X-ray exposures are possible in air, vacuum and He gas environment. The air based exposures enables the X-ray irradiation of resist for lithography and alsomore » irradiation of biological and liquid samples.« less

Structural evolution of Li{sub x}Mn{sub 2}O{sub 4} in lithium-ion battery cells measured in situ using synchrotron X-ray diffraction techniques

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

Mukerjee, S.; Thurston, T.R.; Jisrawi, N.M.

The authors describe synchrotron based X-ray diffraction techniques and issues related to in situ studies of intercalation processes in battery electrodes. They then demonstrate the utility of this technique, through a study of two batches of Li{sub x}Mn{sub 2}O{sub 4} cathode materials. The structural evolution of these spinel materials was monitored in situ during the initial charge of these electrodes in actual battery cells. Significant differences were observed in the two batches, particularly in the intercalation range of x = 0.45 to 0.20. The first-order structural transitions in this region indicated coexistence of two cubic phases in the batch 2more » material, whereas the batch 1 material showed suppressed two-phase coexistence. Batch 2 cells also indicated structural evolution in the low-potential region below 3.0 V in contrast to the batch 1 material. Differences in structural evolution between batches of Li{sub x}Mn{sub 2}O{sub 4} could have important ramifications in their cycle life and stability characteristics.« less

Structure of the Archaeoglobus fulgidus orphan ORF AF1382 determined by sulfur SAD from a moderately diffracting crystal

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

Zhu, Jin-Yi; Fu, Zheng-Qing; Argonne National Laboratory, Argonne, Illinois

2012-09-01

The crystal structure of the 11.14 kDa orphan ORF 1382 from Archaeoglobus fulgidus (AF1382) has been determined by sulfur SAD phasing using data collected from a moderately diffracting crystal and 1.9 Å synchrotron X-rays. The crystal structure of the 11.14 kDa orphan ORF 1382 from Archaeoglobus fulgidus (AF1382) has been determined by sulfur SAD phasing using a moderately diffracting crystal and 1.9 Å wavelength synchrotron X-rays. AF1382 was selected as a structural genomics target by the Southeast Collaboratory for Structural Genomics (SECSG) since sequence analyses showed that it did not belong to the Pfam-A database and thus could represent amore » novel fold. The structure was determined by exploiting longer wavelength X-rays and data redundancy to increase the anomalous signal in the data. AF1382 is a 95-residue protein containing five S atoms associated with four methionine residues and a single cysteine residue that yields a calculated Bijvoet ratio (ΔF{sub anom}/F) of 1.39% for 1.9 Å wavelength X-rays. Coupled with an average Bijvoet redundancy of 25 (two 360° data sets), this produced an excellent electron-density map that allowed 69 of the 95 residues to be automatically fitted. The S-SAD model was then manually completed and refined (R = 23.2%, R{sub free} = 26.8%) to 2.3 Å resolution. High-resolution data were subsequently collected from a better diffracting crystal using 0.97 Å wavelength synchrotron X-rays and the S-SAD model was refined (R = 17.9%, R{sub free} = 21.4%) to 1.85 Å resolution. AF1382 has a winged-helix–turn–helix structure common to many DNA-binding proteins and most closely resembles the N-terminal domain (residues 1–82) of the Rio2 kinase from A. fulgidus, which has been shown to bind DNA, and a number of MarR-family transcriptional regulators, suggesting a similar DNA-binding function for AF1382. The analysis also points out the advantage gained from carrying out data reduction and structure determination on-site while the crystal is still available for further data collection.« less

A furnace and environmental cell for the in situ investigation of molten salt electrolysis using high-energy X-ray diffraction.

PubMed

Styles, Mark J; Rowles, Matthew R; Madsen, Ian C; McGregor, Katherine; Urban, Andrew J; Snook, Graeme A; Scarlett, Nicola V Y; Riley, Daniel P

2012-01-01

This paper describes the design, construction and implementation of a relatively large controlled-atmosphere cell and furnace arrangement. The purpose of this equipment is to facilitate the in situ characterization of materials used in molten salt electrowinning cells, using high-energy X-ray scattering techniques such as synchrotron-based energy-dispersive X-ray diffraction. The applicability of this equipment is demonstrated by quantitative measurements of the phase composition of a model inert anode material, which were taken during an in situ study of an operational Fray-Farthing-Chen Cambridge electrowinning cell, featuring molten CaCl(2) as the electrolyte. The feasibility of adapting the cell design to investigate materials in other high-temperature environments is also discussed.

Diffraction of real and virtual photons in a pyrolytic graphite crystal as source of intensive quasimonochromatic X-ray beam

NASA Astrophysics Data System (ADS)

Bogomazova, E. A.; Kalinin, B. N.; Naumenko, G. A.; Padalko, D. V.; Potylitsyn, A. P.; Sharafutdinov, A. F.; Vnukov, I. E.

2003-01-01

A series of experiments on the parametric X-rays radiation (PXR) generation and radiation soft component diffraction of relativistic electrons in pyrolytic graphite (PG) crystals have been carried out at the Tomsk synchrotron. It is shown that the experimental results with PG crystals are explained by the kinematic PXR theory if we take into account a contribution of the real photons diffraction (transition radiation, bremsstrahlung and PXR photons as well). The measurements of the emission spectrum of channeled electrons in the photon energy range much smaller than the characteristic energy of channeling radiation have been performed with a crystal-diffraction spectrometer. For electrons incident along the <1 1 0> axis of a silicon crystal, the radiation intensity in the energy range 30⩽ ω⩽360 keV exceeds the bremsstrahlung one almost by an order of magnitude. Different possibilities to create an effective source of the monochromatic X-ray beam based on the real and virtual photons diffraction in the PG crystals have been considered.

Inorganic pyrophosphatase crystals from Thermococcus thioreducens for X-ray and neutron diffraction.

PubMed

Hughes, Ronny C; Coates, Leighton; Blakeley, Matthew P; Tomanicek, Steve J; Langan, Paul; Kovalevsky, Andrey Y; García-Ruiz, Juan M; Ng, Joseph D

2012-12-01

Inorganic pyrophosphatase (IPPase) from the archaeon Thermococcus thioreducens was cloned, overexpressed in Escherichia coli, purified and crystallized in restricted geometry, resulting in large crystal volumes exceeding 5 mm3. IPPase is thermally stable and is able to resist denaturation at temperatures above 348 K. Owing to the high temperature tolerance of the enzyme, the protein was amenable to room-temperature manipulation at the level of protein preparation, crystallization and X-ray and neutron diffraction analyses. A complete synchrotron X-ray diffraction data set to 1.85 Å resolution was collected at room temperature from a single crystal of IPPase (monoclinic space group C2, unit-cell parameters a=106.11, b=95.46, c=113.68 Å, α=γ=90.0, β=98.12°). As large-volume crystals of IPPase can be obtained, preliminary neutron diffraction tests were undertaken. Consequently, Laue diffraction images were obtained, with reflections observed to 2.1 Å resolution with I/σ(I) greater than 2.5. The preliminary crystallographic results reported here set in place future structure-function and mechanism studies of IPPase.

2D X-ray and FTIR micro-analysis of the degradation of cadmium yellow pigment in paintings of Henri Matisse

NASA Astrophysics Data System (ADS)

Pouyet, E.; Cotte, M.; Fayard, B.; Salomé, M.; Meirer, F.; Mehta, A.; Uffelman, E. S.; Hull, A.; Vanmeert, F.; Kieffer, J.; Burghammer, M.; Janssens, K.; Sette, F.; Mass, J.

2015-11-01

The chemical and physical alterations of cadmium yellow (CdS) paints in Henri Matisse's The Joy of Life (1905-1906, The Barnes Foundation) have been recognized since 2006, when a survey by portable X-ray fluorescence identified this pigment in all altered regions of the monumental painting. This alteration is visible as fading, discoloration, chalking, flaking, and spalling of several regions of light to medium yellow paint. Since that time, synchrotron radiation-based techniques including elemental and spectroscopic imaging, as well as X-ray scattering have been employed to locate and identify the alteration products observed in this and related works by Henri Matisse. This information is necessary to formulate one or multiple mechanisms for degradation of Matisse's paints from this period, and thus ensure proper environmental conditions for the storage and the display of his works. This paper focuses on 2D full-field X-ray Near Edge Structure imaging, 2D micro-X-ray Diffraction, X-ray Fluorescence, and Fourier Transform Infra-red imaging of the altered paint layers to address one of the long-standing questions about cadmium yellow alteration—the roles of cadmium carbonates and cadmium sulphates found in the altered paint layers. These compounds have often been assumed to be photo-oxidation products, but could also be residual starting reagents from an indirect wet process synthesis of CdS. The data presented here allow identifying and mapping the location of cadmium carbonates, cadmium chlorides, cadmium oxalates, cadmium sulphates, and cadmium sulphides in thin sections of altered cadmium yellow paints from The Joy of Life and Matisse's Flower Piece (1906, The Barnes Foundation). Distribution of various cadmium compounds confirms that cadmium carbonates and sulphates are photo-degradation products in The Joy of Life, whereas in Flower Piece, cadmium carbonates appear to have been a [(partially) unreacted] starting reagent for the yellow paint, a role previously suggested in other altered yellow paints.

Extremely asymmetric diffraction as a method of determining magneto-optical constants for X-rays near absorption edges

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

Andreeva, M. A., E-mail: Mandreeva1@yandex.ru; Repchenko, Yu. L., E-mail: kent160@mail.ru; Smekhova, A. G.

2015-06-15

The spectral dependence of the Bragg peak position under conditions of extremely asymmetric diffraction has been analyzed in the kinematical and dynamical approximations of the diffraction theory. Simulations have been performed for the L{sub 3} absorption edge of yttrium in a single-crystal YFe{sub 2} film; they have shown that the magneto-optical constants (or, equivalently, the dispersion corrections to the atomic scattering factor) for hard X-rays can be determined from this dependence. Comparison with the experimental data obtained for a Nb(4 nm)/YFe{sub 2}(40 nm〈110〉)/Fe(1.5 nm)/Nb(50 nm)/sapphire sample at the European Synchrotron Radiation Facility has been made.

Novel portable press for synchrotron time-resolved 3-D micro-imagining under extreme conditions

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

Philippe, J.; Le Godec, Y., E-mail: yann.legodec@impmc.upmc.fr; Bergame, F.

Here we present the instrumental development to extend the synchrotron X-ray microtomography techniques to in situ studies under static compression (HP) or shear stress or the both conditions at high temperatures (HT). To achieve this, a new rotating tomography Paris-Edinburgh cell (rotoPEc) has been developed. This ultra-compact portable device, easily and successfully adapted to various multi-modal synchrotron experimental set-up at ESRF, SOLEIL and DIAMOND is explained in detail.

Carbonate formation in non-aqueous environments by solid-gas carbonation of silicates

NASA Astrophysics Data System (ADS)

Day, S. J.; Thompson, S. P.; Evans, A.; Parker, J. E.

2012-02-01

We have produced synthetic analogues of cosmic silicates using the Sol Gel method, producing amorphous silicates of composition Mg(x)Ca(1-x)SiO3. Using synchrotron X-ray powder diffraction on Beamline I11 at the Diamond Light Source, together with a newly-commissioned gas cell, real-time powder diffraction scans have been taken of a range of silicates exposed to CO2 under non-ambient conditions. The SXPD is complemented by other techniques including Raman and Infrared Spectroscopy and SEM imaging.

Combined Diffraction and Density Functional Theory Calculations of Halogen-Bonded Cocrystal Monolayers

PubMed Central

2013-01-01

This work describes the combined use of synchrotron X-ray diffraction and density functional theory (DFT) calculations to understand the cocrystal formation or phase separation in 2D monolayers capable of halogen bonding. The solid monolayer structure of 1,4-diiodobenzene (DIB) has been determined by X-ray synchrotron diffraction. The mixing behavior of DIB with 4,4′-bipyridyl (BPY) has also been studied and interestingly is found to phase-separate rather than form a cocrystal, as observed in the bulk. DFT calculations are used to establish the underlying origin of this interesting behavior. The DFT calculations are demonstrated to agree well with the recently proposed monolayer structure for the cocrystal of BPY and 1,4-diiodotetrafluorobenzene (DITFB) (the perfluorinated analogue of DIB), where halogen bonding has also been identified by diffraction. Here we have calculated an estimate of the halogen bond strength by DFT calculations for the DITFB/BPY cocrystal monolayer, which is found to be ∼20 kJ/mol. Computationally, we find that the nonfluorinated DIB and BPY are not expected to form a halogen-bonded cocrystal in a 2D layer; for this pair of species, phase separation of the components is calculated to be lower energy, in good agreement with the diffraction results. PMID:24215390

Combined diffraction and density functional theory calculations of halogen-bonded cocrystal monolayers.

PubMed

Sacchi, Marco; Brewer, Adam Y; Jenkins, Stephen J; Parker, Julia E; Friščić, Tomislav; Clarke, Stuart M

2013-12-03

This work describes the combined use of synchrotron X-ray diffraction and density functional theory (DFT) calculations to understand the cocrystal formation or phase separation in 2D monolayers capable of halogen bonding. The solid monolayer structure of 1,4-diiodobenzene (DIB) has been determined by X-ray synchrotron diffraction. The mixing behavior of DIB with 4,4'-bipyridyl (BPY) has also been studied and interestingly is found to phase-separate rather than form a cocrystal, as observed in the bulk. DFT calculations are used to establish the underlying origin of this interesting behavior. The DFT calculations are demonstrated to agree well with the recently proposed monolayer structure for the cocrystal of BPY and 1,4-diiodotetrafluorobenzene (DITFB) (the perfluorinated analogue of DIB), where halogen bonding has also been identified by diffraction. Here we have calculated an estimate of the halogen bond strength by DFT calculations for the DITFB/BPY cocrystal monolayer, which is found to be ∼20 kJ/mol. Computationally, we find that the nonfluorinated DIB and BPY are not expected to form a halogen-bonded cocrystal in a 2D layer; for this pair of species, phase separation of the components is calculated to be lower energy, in good agreement with the diffraction results.

Single-crystal Raman spectroscopy and X-ray crystallography at beamline X26-C of the NSLS

PubMed Central

Stoner-Ma, Deborah; Skinner, John M.; Schneider, Dieter K.; Cowan, Matt; Sweet, Robert M.; Orville, Allen M.

2011-01-01

Three-dimensional structures derived from X-ray diffraction of protein crystals provide a wealth of information. Features and interactions important for the function of macromolecules can be deduced and catalytic mechanisms postulated. Still, many questions can remain, for example regarding metal oxidation states and the interpretation of ‘mystery density’, i.e. ambiguous or unknown features within the electron density maps, especially at ∼2 Å resolutions typical of most macromolecular structures. Beamline X26-C at the National Synchrotron Light Source (NSLS), Brookhaven National Laboratory (BNL), provides researchers with the opportunity to not only determine the atomic structure of their samples but also to explore the electronic and vibrational characteristics of the sample before, during and after X-ray diffraction data collection. When samples are maintained under cryo-conditions, an opportunity to promote and follow photochemical reactions in situ as a function of X-ray exposure is also provided. Plans are in place to further expand the capabilities at beamline X26-C and to develop beamlines at NSLS-II, currently under construction at BNL, which will provide users access to a wide array of complementary spectroscopic methods in addition to high-quality X-ray diffraction data. PMID:21169688

New Findings on the Phase Transitions in Li(sub 1-x)CoO(sub 2) and Li(sub 1-x)NiO(sub 2) Cathode Materials During Cycling: In Situ Synchrotron X-Ray Diffraction Studies

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

Yang, X. Q.; Sun, X.; McBreen, J.

The authors have utilized synchrotron x-ray radiation to perform ''in situ'' x-ray diffraction studies on Li{sub 1-x}CoO{sub 2} and Li{sub 1-x}NiO{sub 2} cathodes. A C/10 charging rate was used for a Li/Li{sub 1-x}CoO{sub 2} cell. For the Li/Li{sub 1-x}NiO{sub 2} cells, C/13 and C/84 rates were applied. The in situ XRD data were collected during the first charge from 3.5 to 5.2 V. For the Li{sub 1-x}CoO{sub 2} cathode, in the composition range of x = 0 to x = 0.5, a new intermediate phase H2a was observed in addition to the two expected hexagonal phases H1 and H2. Inmore » the region very close to x = 0.5, some spectral signatures for the formation of a monoclinic phase M1 were also observed. Further, in the x = 0.8 to x = 1 region, the formation of a CdI{sub 2} type hexagonal phase has been confirmed. However, this new phase is transformed from a CdCl{sub 2} type hexagonal phase, rather than from a monoclinic phase M2 as previously reported in the literature. For the Li{sub 1-x}NiO{sub 2} system, by taking the advantage of the high resolution in 2{theta} angles through the synchrotron based XRD technique, they were able to identify a two-phase coexistence region of hexagonal phase H1 and H2, which has been mistakenly indexed as a single phase region for monoclinic phase M1. Interesting similarities and differences between these two systems are also discussed.« less

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.

Radiation damage in a micron-sized protein crystal studied via reciprocal space mapping and Bragg coherent diffractive imaging.

PubMed

Coughlan, H D; Darmanin, C; Phillips, N W; Hofmann, F; Clark, J N; Harder, R J; Vine, D J; Abbey, B

2015-07-01

For laboratory and synchrotron based X-ray sources, radiation damage has posed a significant barrier to obtaining high-resolution structural data from biological macromolecules. The problem is particularly acute for micron-sized crystals where the weaker signal often necessitates the use of higher intensity beams to obtain the relevant data. Here, we employ a combination of techniques, including Bragg coherent diffractive imaging to characterise the radiation induced damage in a micron-sized protein crystal over time. The approach we adopt here could help screen for potential protein crystal candidates for measurement at X-ray free election laser sources.

Purification, crystallization and preliminary crystallographic analysis of biotin protein ligase from Staphylococcus aureus

PubMed Central

Pendini, Nicole R.; Polyak, Steve W.; Booker, Grant W.; Wallace, John C.; Wilce, Matthew C. J.

2008-01-01

Biotin protein ligase from Staphylococcus aureus catalyses the biotinylation of acetyl-CoA carboxylase and pyruvate carboxylase. Recombinant biotin protein ligase from S. aureus has been cloned, expressed and purified. Crystals were grown using the hanging-drop vapour-diffusion method using PEG 8000 as the precipitant at 295 K. X-ray diffraction data were collected to 2.3 Å resolution from crystals using synchrotron X-ray radiation at 100 K. The diffraction was consistent with the tetragonal space group P42212, with unit-cell parameters a = b = 93.665, c = 131.95. PMID:18540065

Structural alterations of thin actin filaments in muscle contraction by synchrotron X-ray fiber diffraction.

PubMed

Wakabayashi, Katsuzo; Sugimoto, Yasunobu; Takezawa, Yasunori; Ueno, Yutaka; Minakata, Shiho; Oshima, Kanji; Matsuo, Tatsuhito; Kobayashi, Takakazu

2007-01-01

Strong evidence has been accumulated that the conformational changes of the thin actin filaments are occurring and playing an important role in the entire process of muscle contraction. The conformational changes and the mechanical properties of the thin actin filaments we have found by X-ray fiber diffraction on skeletal muscle contraction are explored. Recent studies on the conformational changes of regulatory proteins bound to actin filaments upon activation and in the force generation process are also described. Finally, the roles of structural alterations and dynamics of the actin filaments are discussed in conjunction with the regulation mechanism and the force generation mechanism.

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.

On-the-fly segmentation approaches for x-ray diffraction datasets for metallic glasses

DOE PAGES

Ren, Fang; Williams, Travis; Hattrick-Simpers, Jason; ...

2017-08-30

Investment in brighter sources and larger detectors has resulted in an explosive rise in the data collected at synchrotron facilities. Currently, human experts extract scientific information from these data, but they cannot keep pace with the rate of data collection. Here, we present three on-the-fly approaches—attribute extraction, nearest-neighbor distance, and cluster analysis—to quickly segment x-ray diffraction (XRD) data into groups with similar XRD profiles. An expert can then analyze representative spectra from each group in detail with much reduced time, but without loss of scientific insights. As a result, on-the-fly segmentation would, therefore, result in accelerated scientific productivity.

Radiation damage in a micron-sized protein crystal studied via reciprocal space mapping and Bragg coherent diffractive imaging

PubMed Central

Coughlan, H. D.; Darmanin, C.; Phillips, N. W.; Hofmann, F.; Clark, J. N.; Harder, R. J.; Vine, D. J.; Abbey, B.

2015-01-01

For laboratory and synchrotron based X-ray sources, radiation damage has posed a significant barrier to obtaining high-resolution structural data from biological macromolecules. The problem is particularly acute for micron-sized crystals where the weaker signal often necessitates the use of higher intensity beams to obtain the relevant data. Here, we employ a combination of techniques, including Bragg coherent diffractive imaging to characterise the radiation induced damage in a micron-sized protein crystal over time. The approach we adopt here could help screen for potential protein crystal candidates for measurement at X-ray free election laser sources. PMID:26798804

Radiation damage in a micron-sized protein crystal studied via reciprocal space mapping and Bragg coherent diffractive imaging

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

Coughlan, H. D.; Darmanin, C.; Phillips, N. W.

For laboratory and synchrotron based X-ray sources, radiation damage has posed a significant barrier to obtaining high-resolution structural data from biological macromolecules. The problem is particularly acute for micron-sized crystals where the weaker signal often necessitates the use of higher intensity beams to obtain the relevant data. Here, we employ a combination of techniques, including Bragg coherent diffractive imaging to characterise the radiation induced damage in a micron-sized protein crystal over time. The approach we adopt here could help screen for potential protein crystal candidates for measurement at X-ray free election laser sources.

Radiation damage in a micron-sized protein crystal studied via reciprocal space mapping and Bragg coherent diffractive imaging

DOE PAGES

Coughlan, H. D.; Darmanin, C.; Phillips, N. W.; ...

2015-04-29

For laboratory and synchrotron based X-ray sources, radiation damage has posed a significant barrier to obtaining high-resolution structural data from biological macromolecules. The problem is particularly acute for micron-sized crystals where the weaker signal often necessitates the use of higher intensity beams to obtain the relevant data. Here, we employ a combination of techniques, including Bragg coherent diffractive imaging to characterise the radiation induced damage in a micron-sized protein crystal over time. The approach we adopt here could help screen for potential protein crystal candidates for measurement at X-ray free election laser sources.

Residual strain gradient determination in metal matrix composites by synchrotron X-ray energy dispersive diffraction

NASA Technical Reports Server (NTRS)

Kuntz, Todd A.; Wadley, Haydn N. G.; Black, David R.

1993-01-01

An X-ray technique for the measurement of internal residual strain gradients near the continuous reinforcements of metal matrix composites has been investigated. The technique utilizes high intensity white X-ray radiation from a synchrotron radiation source to obtain energy spectra from small (0.001 cu mm) volumes deep within composite samples. The viability of the technique was tested using a model system with 800 micron Al203 fibers and a commercial purity titanium matrix. Good agreement was observed between the measured residual radial and hoop strain gradients and those estimated from a simple elastic concentric cylinders model. The technique was then used to assess the strains near (SCS-6) silicon carbide fibers in a Ti-14Al-21Nb matrix after consolidation processing. Reasonable agreement between measured and calculated strains was seen provided the probe volume was located 50 microns or more from the fiber/matrix interface.

Applications of synchrotron x-ray diffraction topography to fractography

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

Bilello, J.C.

1983-01-01

Fractographs have been taken using a variety of probes each of which produces different types of information. Methods which have been used to examine fracture surfaces include: (a) optical microscopy, particularly interference contrast methods, (b) scanning electron microscopy (SEM), (c) SEM with electron channelling, (d) SEM with selected-area electron channelling, (e) Berg-Barrett (B-B) topography, and now (f) synchrotron x-radiation fractography (SXRF). This review concentrated on the role that x-ray methods can play in such studies. In particular, the ability to nondestructively assess the subsurface microstructure associated with the fracture to depths of the order of 5 to 10 ..mu..m becomesmore » an important attribute for observations of a large class of semi-brittle metals, semiconductors and ceramics.« less

Determination of the solubility of tin indium oxide using in situ and ex x-ray diffraction

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

Gonzalez, G. B.; Mason, T. O.; Okasinski, J. S.

A novel approach to determine the thermodynamic solubility of tin in indium oxide via the exsolution from tin overdoped nano-ITO powders is presented. High-energy, in situ and ex situ synchrotron X-ray diffraction was utilized to study the solubility limit at temperatures ranging from 900 C to 1375 C. The tin exsolution from overdoped nanopowders and the formation of In{sub 4}Sn{sub 3}O{sub 12} were observed in situ during the first 4-48 h of high-temperature treatment. Samples annealed between 900 C and 1175 C were also studied ex situ with heat treatments for up to 2060 h. Structural results obtained from Rietveldmore » analysis include compositional phase analysis, atomic positions, and lattice parameters. The tin solubility in In{sub 2}O{sub 3} was determined using the phase analysis compositions from X-ray diffraction and the elemental compositions obtained from X-ray fluorescence. Experimental complications that can lead to incorrect tin solubility values in the literature are discussed.« less

Simultaneous multiplexed materials characterization using a high-precision hard X-ray micro-slit array.

PubMed

Zhang, Fan; Allen, Andrew J; Levine, Lyle E; Mancini, Derrick C; Ilavsky, Jan

2015-05-01

The needs both for increased experimental throughput and for in operando characterization of functional materials under increasingly realistic experimental conditions have emerged as major challenges across the whole of crystallography. A novel measurement scheme that allows multiplexed simultaneous measurements from multiple nearby sample volumes is presented. This new approach enables better measurement statistics or direct probing of heterogeneous structure, dynamics or elemental composition. To illustrate, the submicrometer precision that optical lithography provides has been exploited to create a multiplexed form of ultra-small-angle scattering based X-ray photon correlation spectroscopy (USAXS-XPCS) using micro-slit arrays fabricated by photolithography. Multiplexed USAXS-XPCS is applied to follow the equilibrium dynamics of a simple colloidal suspension. While the dependence of the relaxation time on momentum transfer, and its relationship with the diffusion constant and the static structure factor, follow previous findings, this measurements-in-parallel approach reduces the statistical uncertainties of this photon-starved technique to below those associated with the instrument resolution. More importantly, we note the potential of the multiplexed scheme to elucidate the response of different components of a heterogeneous sample under identical experimental conditions in simultaneous measurements. In the context of the X-ray synchrotron community, this scheme is, in principle, applicable to all in-line synchrotron techniques. Indeed, it has the potential to open a new paradigm for in operando characterization of heterogeneous functional materials, a situation that will be even further enhanced by the ongoing development of multi-bend achromat storage ring designs as the next evolution of large-scale X-ray synchrotron facilities around the world.

Simultaneous multiplexed materials characterization using a high-precision hard X-ray micro-slit array

DOE PAGES

Zhang, Fan; Allen, Andrew J.; Levine, Lyle E.; ...

2015-01-01

Here, the needs both for increased experimental throughput and forin operandocharacterization of functional materials under increasingly realistic experimental conditions have emerged as major challenges across the whole of crystallography. A novel measurement scheme that allows multiplexed simultaneous measurements from multiple nearby sample volumes is presented. This new approach enables better measurement statistics or direct probing of heterogeneous structure, dynamics or elemental composition. To illustrate, the submicrometer precision that optical lithography provides has been exploited to create a multiplexed form of ultra-small-angle scattering based X-ray photon correlation spectroscopy (USAXS-XPCS) using micro-slit arrays fabricated by photolithography. Multiplexed USAXS-XPCS is applied to followmore » the equilibrium dynamics of a simple colloidal suspension. While the dependence of the relaxation time on momentum transfer, and its relationship with the diffusion constant and the static structure factor, follow previous findings, this measurements-in-parallel approach reduces the statistical uncertainties of this photon-starved technique to below those associated with the instrument resolution. More importantly, we note the potential of the multiplexed scheme to elucidate the response of different components of a heterogeneous sample underidenticalexperimental conditions in simultaneous measurements. Lastly, in the context of the X-ray synchrotron community, this scheme is, in principle, applicable to all in-line synchrotron techniques. Indeed, it has the potential to open a new paradigm for in operando characterization of heterogeneous functional materials, a situation that will be even further enhanced by the ongoing development of multi-bend achromat storage ring designs as the next evolution of large-scale X-ray synchrotron facilities around the world.« less

Perfect X-ray focusing via fitting corrective glasses to aberrated optics

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

Seiboth, Frank; Schropp, Andreas; Scholz, Maria

2017-03-01

Due to their short wavelength, X-rays can in principle be focused down to a few nanometres and below. At the same time, it is this short wavelength that puts stringent requirements on X-ray optics and their metrology. Both are limited by today’s technology. In this work, we present accurate at wavelength measurements of residual aberrations of a refractive X-ray lens using ptychography to manufacture a corrective phase plate. Together with the fitted phase plate the optics shows diffraction-limited performance, generating a nearly Gaussian beam profile with a Strehl ratio above 0.8. As a result, this scheme can be applied tomore » any other focusing optics, thus solving the X-ray optical problem at synchrotron radiation sources and X-ray free-electron lasers.« less

Perfect X-ray focusing via fitting corrective glasses to aberrated optics

PubMed Central

Seiboth, Frank; Schropp, Andreas; Scholz, Maria; Wittwer, Felix; Rödel, Christian; Wünsche, Martin; Ullsperger, Tobias; Nolte, Stefan; Rahomäki, Jussi; Parfeniukas, Karolis; Giakoumidis, Stylianos; Vogt, Ulrich; Wagner, Ulrich; Rau, Christoph; Boesenberg, Ulrike; Garrevoet, Jan; Falkenberg, Gerald; Galtier, Eric C.; Ja Lee, Hae; Nagler, Bob; Schroer, Christian G.

2017-01-01

Due to their short wavelength, X-rays can in principle be focused down to a few nanometres and below. At the same time, it is this short wavelength that puts stringent requirements on X-ray optics and their metrology. Both are limited by today's technology. In this work, we present accurate at wavelength measurements of residual aberrations of a refractive X-ray lens using ptychography to manufacture a corrective phase plate. Together with the fitted phase plate the optics shows diffraction-limited performance, generating a nearly Gaussian beam profile with a Strehl ratio above 0.8. This scheme can be applied to any other focusing optics, thus solving the X-ray optical problem at synchrotron radiation sources and X-ray free-electron lasers. PMID:28248317

Comment on {open_quote}{open_quote}Comments on the use of asymmetric monochromators for x-ray diffraction on a synchrotron source{close_quote}{close_quote} [Rev. Sci. Instrum. {bold 66}, 2174 (1995)

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

Sanchez del Rio, M.; Cerrina, F.

1996-10-01

In the article {open_quote}{open_quote}Comments on the use of asymmetric monochromators for x-ray diffraction on a synchrotron source,{close_quote}{close_quote} by Colin Nave, Ana Gonzalez, Graham Clark, Sean McSweeney, Stewart Cummings, and Michael Hart, Rev. Sci. Instrum. {bold 66}, 2174 (1995), paragraph II, the authors{close_quote} unfamiliarity with our modeling codes leads them to claim that our approach to treat bent-asymmetrically cut crystals in ray tracing calculations is incorrect. Since SHADOW is a widely used code, it is important to correct any misunderstandings, and we give here arguments to demonstrate that our approach is perfectly valid, and the arguments used by the authors tomore » criticize our method are based on an unwarranted conclusion extracted from one of our previous articles. We show that SHADOW, when properly run, treats the cases raised exactly. Indeed, their arguments provide a nice benchmark test for verifying the accuracy of SHADOW {copyright} {ital 1996 American Institute of Physics.}« less

Chemical imaging analysis of the brain with X-ray methods

NASA Astrophysics Data System (ADS)

Collingwood, Joanna F.; Adams, Freddy

2017-04-01

Cells employ various metal and metalloid ions to augment the structure and the function of proteins and to assist with vital biological processes. In the brain they mediate biochemical processes, and disrupted metabolism of metals may be a contributing factor in neurodegenerative disorders. In this tutorial review we will discuss the particular role of X-ray methods for elemental imaging analysis of accumulated metal species and metal-containing compounds in biological materials, in the context of post-mortem brain tissue. X-rays have the advantage that they have a short wavelength and can penetrate through a thick biological sample. Many of the X-ray microscopy techniques that provide the greatest sensitivity and specificity for trace metal concentrations in biological materials are emerging at synchrotron X-ray facilities. Here, the extremely high flux available across a wide range of soft and hard X-rays, combined with state-of-the-art focusing techniques and ultra-sensitive detectors, makes it viable to undertake direct imaging of a number of elements in brain tissue. The different methods for synchrotron imaging of metals in brain tissues at regional, cellular, and sub-cellular spatial resolution are discussed. Methods covered include X-ray fluorescence for elemental imaging, X-ray absorption spectrometry for speciation imaging, X-ray diffraction for structural imaging, phase contrast for enhanced contrast imaging and scanning transmission X-ray microscopy for spectromicroscopy. Two- and three-dimensional (confocal and tomographic) imaging methods are considered as well as the correlation of X-ray microscopy with other imaging tools.

Role of initial heat treatment of the ferrite component on magnetic properties in the composite of ferrimagnetic Co1.75Fe1.25O4 ferrite and non-magnetic BaTiO3 oxide

NASA Astrophysics Data System (ADS)

Bhowmik, R. N.; Kazhugasalamoorthy, S.; Sinha, A. K.

2017-12-01

We have prepared a composite of ferrimagnetic ferrite Co1.75Fe1.25O4 and non-magnetic oxide BaTiO3. The ferrite composition Co1.75Fe1.25O4 has been prepared by chemical co-precipitation and subsequently heated at different temperatures. The heat treated ferrite powder has been mixed with BaTiO3 powder with mass ratio 1:1 and the mixed powder has been finally heated at 1000 °C to form composite material. Structural phase of the composite material has been confirmed by high quality Synchrotron X-ray diffraction pattern and Micro-Raman spectra. The grain surface morphology and elemental composition have been studied by Scanning electron microscope and Energy dispersive X-ray analysis. The distribution of magnetic exchange interactions and blocking behavior of the ferrimagnetic grains in composite samples has been understood by analyzing the temperature and magnetic field dependence of dc magnetization. Finally, information on modified micro-structure and ferrimagnetic parameters in composite samples has been obtained as the variation of annealing temperature of the ferrite component before making composite.

In Situ Assessment of Lattice in an Al-Li Alloy

NASA Technical Reports Server (NTRS)

Beaudoin, A. J.; Obstalecki, M.; Tayon, W.; Hernquist, M.; Mudrock, R.; Kenesei, P.; Lienert, U.

2013-01-01

The lattice strains of individual grains are measured in an Al-Li alloy, AA 2195, using high-energy X-ray diffraction at a synchrotron source. The diffraction of individual grains in this highly textured production alloy was isolated through use of a depth-defining aperture. It is shown that hydrostatic stress, and in turn the stress triaxiality, can vary significantly from grain to grain.

The Status of the Taiwan Photon Source

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

Kuo, C. C.; Wang, J. P.; Chen, J. R.

2010-06-23

NSRRC has been operating a 1.5 GeV synchrotron light source, the Taiwan Light Source (TLS), for over 15 years and has established a large user community. For the future development of synchrotron radiation research in Taiwan, a feasibility study report to construct a 3.0 GeV low-emittance storage ring, the Taiwan Photon Source (TPS), was issued in July 2005. The government approval of the TPS project was obtained in December 2007 and the machine will be built at current site of NSRRC. The project has progressed steadily since and reached several major milestones now: the architect firm has finished the sitemore » plan and civil design, the accelerator design has been fixed, and purchase of long-lead items begins its course. The TPS storage ring has a circumference of 518.4 meters with a concentric booster of 496.8 meters. The storage ring adopted a 24-cell double-bend structure with a 1.6 nm-rad natural emittance. There are six 12-m and eighteen 7-m ID straights. For user research, five new beamlines have been selected for the Phase I operations: the micro protein crystallography, the materials sub-micron diffraction, the inelastic soft x-ray scattering, the coherent x-ray scattering, and the nano probe beamlines. The civil construction is getting ready to start. The commissioning of the TPS storage ring is targeted for 2013.« less

In situ defect annealing of swift heavy ion irradiated CeO 2 and ThO 2 using synchrotron X-ray diffraction and a hydrothermal diamond anvil cell

DOE PAGES

Palomares, Raul I.; Tracy, Cameron L.; Zhang, Fuxiang; ...

2015-04-16

Hydrothermal diamond anvil cells (HDACs) provide facile means for coupling synchrotron Xray techniques with pressure up to 10 GPa and temperature up to 1300 K. This manuscript reports on an application of the HDAC as an ambient-pressure sample environment for performing in situ defect annealing and thermal expansion studies of swift heavy ion irradiated CeO 2 and ThO 2 using synchrotron X-ray diffraction. The advantages of the in situ HDAC technique over conventional annealing methods include: rapid temperature ramping and quench times, high-resolution measurement capability, simultaneous annealing of multiple samples, and prolonged temperature- and apparatus stability at high temperatures. Isochronalmore » annealing between 300 K and 1100 K revealed 2-stage and 1-stage defect recovery processes for irradiated CeO 2 and ThO 2, respectively; indicating that the morphology of the defects produced by swift heavy ion irradiation of these two materials differs significantly. These results suggest that electronic configuration plays a major role in both the radiation-induced defect production and high temperature defect recovery mechanisms of CeO 2 and ThO 2.« less

Application of x-ray absorption fine structure (XAFS) to local-order analysis in Fe-Cr maghemite-like materials

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

Montero-Cabrera, M. E., E-mail: elena.montero@cimav.edu.mx; Fuentes-Cobas, L. E.; Macías-Ríos, E.

2015-07-23

The maghemite-like oxide system γ-Fe{sub 2-x}Cr{sub x}O{sub 3} (x=0.75, 1 and 1.25) was studied by X-ray absorption fine structure (XAFS) and by synchrotron radiation X-ray diffraction (XRD). Measurements were performed at the Stanford Synchrotron Radiation Lightsource at room temperature, at beamlines 2-1, 2-3 and 4-3. High-resolution XRD patterns were processed by means of the Rietveld method. In cases of atoms being neighbors in the Periodic Table, the order/disorder degree of the considered solutions is indiscernible by “normal” (absence of “anomalous scattering”) diffraction experiments. Thus, maghemite-like materials were investigated by XAFS in both Fe and Cr K-edges to clarify, via short-rangemore » structure characterization, the local ordering of the investigated system. Athena and Artemis graphic user interfaces for IFEFFIT and FEFF8.4 codes were employed for XAFS spectra interpretation. Pre-edge decomposition and theoretical modeling of X-ray absorption near edge structure (XANES) transitions were performed. By analysis of the Cr K-edge XANES, it has been confirmed that Cr is located in an octahedral environment. Fitting of the extended X-ray absorption fine structure (EXAFS) spectra was performed under the consideration that the central atom of Fe is allowed to occupy octa- and tetrahedral positions, while Cr occupies only octahedral ones. Coordination number of neighboring atoms, interatomic distances and their quadratic deviation average were determined for x=1, by fitting simultaneously the EXAFS spectra of both Fe and Cr K-edges. The results of fitting the experimental spectra with theoretical standards showed that the cation vacancies tend to follow a regular pattern within the structure of the iron-chromium maghemite (FeCrO{sub 3})« less

Determining Individual Phase Flow Properties in a Quench and Partitioning Steel with In Situ High-Energy X-Ray Diffraction and Multiphase Elasto-Plastic Self-Consistent Method

NASA Astrophysics Data System (ADS)

Hu, Xiaohua; Choi, Kyoo Sil; Sun, Xin; Ren, Yang; Wang, Yangdong

2016-12-01

The micromechanical properties of the constituent phases were characterized for advanced high-strength steels (AHSS) produced by a quenching and partitioning (Q&P) process with in situ tensile loading under synchrotron-based, high-energy X-ray diffraction. The constituent phases present are retained austenite and three martensites (tempered, untampered, and freshly formed martensites). For the material investigated, the 200 and 220 lattice strains of the retained austenite phase were calculated by examining the changes of the X-ray diffraction peak positions during deformation. The 200 and 211 lattice strains of the various martensitic phases with similar crystal structures were determined by separating their overlapped diffraction peaks. Apart from tempered and untempered martensite, the diffraction peaks of freshly formed martensite as a result of austenite-to-martensite transformation can also be separated due to a high initial austenite volume fraction. The phase stresses are first estimated with an empirical relationship through the X-ray diffraction elastic constants. A multiphase elasto-plastic self-consistent model is next used for more accurate determination of the constitutive behaviors of the various phases by comparing the predicted lattice strain distributions and global stress-strain curves with the measured ones. The determined constitutive laws will be used for microstructure-based modeling for sheet formability of the Q&P AHSS steel.

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

Deformation in metallic glasses studied by synchrotron x-ray diffraction

DOE PAGES

Dmowski, Wojciech; Egami, Takeshi; Tong, Yang

2016-01-11

In this study, high mechanical strength is one of the superior properties of metallic glasses which render them promising as a structural material. However, understanding the process of mechanical deformation in strongly disordered matter, such as metallic glass, is exceedingly difficult because even an effort to describe the structure qualitatively is hampered by the absence of crystalline periodicity. In spite of such challenges, we demonstrate that high-energy synchrotron X-ray diffraction measurement under stress, using a two-dimensional detector coupled with the anisotropic pair-density function (PDF) analysis, has greatly facilitated the effort of unraveling complex atomic rearrangements involved in the elastic, anelastic,more » and plastic deformation of metallic glasses. Even though PDF only provides information on the correlation between two atoms and not on many-body correlations, which are often necessary in elucidating various properties, by using stress as means of exciting the system we can garner rich information on the nature of the atomic structure and local atomic rearrangements during deformation in glasses.« less

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.

Assessment of Barium Sulphate Formation and Inhibition at Surfaces with Synchrotron X-ray Diffraction (SXRD)

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

E Mavredaki; A Neville; K Sorbie

2011-12-31

The precipitation of barium sulphate from aqueous supersaturated solutions is a well-known problem in the oil industry often referred to as 'scaling'. The formation and growth of barite on surfaces during the oil extraction process can result in malfunctions within the oil facilities and serious damage to the equipment. The formation of barium sulphate at surfaces remains an important topic of research with the focus being on understanding the mechanisms of formation and means of control. In situ synchrotron X-ray diffraction (SXRD) was used to investigate the formation of barium sulphate on a stainless steel surface. The effect of Poly-phosphinocarboxylicmore » acid (PPCA) and Diethylenetriamine-penta-methylenephosphonic acid (DETPMP) which are two commercial inhibitors for barium sulphate was examined. The in situ SXRD measurements allowed the identification of the crystal faces of the deposited barite in the absence and presence of the two inhibitors. The preferential effect of the inhibitors on some crystal planes is reported and the practical significance discussed.« less

Validating a Model for Welding Induced Residual Stress Using High-Energy X-ray Diffraction

DOE PAGES

Mach, J. C.; Budrow, C. J.; Pagan, D. C.; ...

2017-03-15

Integrated computational materials engineering (ICME) provides a pathway to advance performance in structures through the use of physically-based models to better understand how manufacturing processes influence product performance. As one particular challenge, consider that residual stresses induced in fabrication are pervasive and directly impact the life of structures. For ICME to be an effective strategy, it is essential that predictive capability be developed in conjunction with critical experiments. In the present paper, simulation results from a multi-physics model for gas metal arc welding are evaluated through x-ray diffraction using synchrotron radiation. A test component was designed with intent to developmore » significant gradients in residual stress, be representative of real-world engineering application, yet remain tractable for finely spaced strain measurements with positioning equipment available at synchrotron facilities. Finally, the experimental validation lends confidence to model predictions, facilitating the explicit consideration of residual stress distribution in prediction of fatigue life.« less

Validating a Model for Welding Induced Residual Stress Using High-Energy X-ray Diffraction

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

Mach, J. C.; Budrow, C. J.; Pagan, D. C.

Integrated computational materials engineering (ICME) provides a pathway to advance performance in structures through the use of physically-based models to better understand how manufacturing processes influence product performance. As one particular challenge, consider that residual stresses induced in fabrication are pervasive and directly impact the life of structures. For ICME to be an effective strategy, it is essential that predictive capability be developed in conjunction with critical experiments. In the present paper, simulation results from a multi-physics model for gas metal arc welding are evaluated through x-ray diffraction using synchrotron radiation. A test component was designed with intent to developmore » significant gradients in residual stress, be representative of real-world engineering application, yet remain tractable for finely spaced strain measurements with positioning equipment available at synchrotron facilities. Finally, the experimental validation lends confidence to model predictions, facilitating the explicit consideration of residual stress distribution in prediction of fatigue life.« less

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

Beam-smiling in bent-Laue monochromators

NASA Astrophysics Data System (ADS)

Ren, B.; Dilmanian, F. A.; Chapman, L. D.; Wu, X. Y.; Zhong, Z.; Ivanov, I.; Thomlinson, W. C.; Huang, X.

1997-07-01

When a wide fan-shaped x-ray beam is diffracted by a bent crystal in the Laue geometry, the profile of the diffracted beam generally does not appear as a straight line, but as a line with its ends curved up or curved down. This effect, referred to as "beam-smiling", has been a major obstacle in developing bent-Laue crystal monochromators for medical applications of synchrotron x-ray. We modeled a cylindrically bent crystal using the Finite Element Analysis (FEA) method, and we carried out experiments at the National Synchrotron Light Source and Cornell High Energy Synchrotron Source. Our studies show that, while beam-smiling exists in most of the crystal's area because of anticlastic bending effects, there is a region parallel to the bending axis of the crystal where the diffracted beam is "smile-free". By applying asymmetrical bending, this smile-free region can be shifted vertically away from the geometric center of the crystal, as desired. This leads to a novel method of compensating for beam-smiling. We will discuss the method of "differential bending" for smile removal, beam-smiling in the Cauchios and the polychromatic geometry, and the implications of the method on developing single- and double-bent Laue monochromators. The experimental results will be discussed, concentrating on specific beam-smiling observation and removal as applied to the new monochromator of the Multiple Energy Computed Tomography [MECT] project of the Medical Department, Brookhaven National Laboratory.

Crystallization and preliminary X-ray analysis of a low density lipoprotein from human plasma.

PubMed

Prassl, R; Chapman, J M; Nigon, F; Sara, M; Eschenburg, S; Betzel, C; Saxena, A; Laggner, P

1996-11-15

Single crystals of human plasma low density lipoprotein (LDL), the major transport vehicle for cholesterol in blood, have been produced with a view to analysis of the three-dimensional structure by x-ray crystallography. Crystals with dimensions of approximately 200 x 100 x 50 microm have been reproducibly obtained from highly homogeneous LDL particle subspecies, isolated in the density ranges d = 1.0271-1. 0297 g/ml and d = 1.0297-1.0327 g/ml. Electron microscopic imaging of ultrathin-sectioned preparations of the crystals confirmed the existence of a regular, quasihexagonal arrangement of spherical particles of approximately 18 nm in diameter, thereby resembling the dimensions characteristic of LDL after dehydration and fixation. X-ray diffraction with synchrotron radiation under cryogenic conditions revealed the presence of well resolved diffraction spots, to a resolution of about 29 A. The diffraction patterns are indexed in terms of a triclinic lattice with unit cell dimensions of a = 16. 1 nm, b = 39.0 nm, c = 43.9 nm; alpha = 96.2 degrees, beta = 92.1 degrees, gamma = 102 degrees, and with space group P1.

Low-dose, high-resolution and high-efficiency ptychography at STXM beamline of SSRF

NASA Astrophysics Data System (ADS)

Xu, Zijian; Wang, Chunpeng; Liu, Haigang; Tao, Xulei; Tai, Renzhong

2017-06-01

Ptychography is a diffraction-based X-ray microscopy method that can image extended samples quantitatively while remove the resolution limit imposed by image-forming optical elements. As a natural extension of scanning transmission X-ray microscopy (STXM) imaging method, we developed soft X-ray ptychographic coherent diffraction imaging (PCDI) method at the STXM endstation of BL08U beamline of Shanghai Synchrotron Radiation Facility. Compared to the traditional STXM imaging, the new PCDI method has resulted in significantly lower dose, higher resolution and higher efficiency imaging in our platform. In the demonstration experiments shown here, a spatial resolution of sub-10 nm was obtained for a gold nanowires sample, which is much better than the limit resolution 30 nm of the STXM method, while the radiation dose is only 1/12 of STXM.

Exploring actinide materials through synchrotron radiation techniques.

PubMed

Shi, Wei-Qun; Yuan, Li-Yong; Wang, Cong-Zhi; Wang, Lin; Mei, Lei; Xiao, Cheng-Liang; Zhang, Li; Li, Zi-Jie; Zhao, Yu-Liang; Chai, Zhi-Fang

2014-12-10

Synchrotron radiation (SR) based techniques have been utilized with increasing frequency in the past decade to explore the brilliant and challenging sciences of actinide-based materials. This trend is partially driven by the basic needs for multi-scale actinide speciation and bonding information and also the realistic needs for nuclear energy research. In this review, recent research progresses on actinide related materials by means of various SR techniques were selectively highlighted and summarized, with the emphasis on X-ray absorption spectroscopy, X-ray diffraction and scattering spectroscopy, which are powerful tools to characterize actinide materials. In addition, advanced SR techniques for exploring future advanced nuclear fuel cycles dealing with actinides are illustrated as well. © 2014 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Low thermal conductivity and improved thermoelectric performance of nanocrystalline silicon germanium films by sputtering

NASA Astrophysics Data System (ADS)

Perez Taborda, J. A.; Romero, J. J.; Abad, B.; Muñoz-Rojo, M.; Mello, A.; Briones, F.; Gonzalez, M. S. Martin

2016-04-01

Si x Ge1-x alloys are well-known thermoelectric materials with a high figure of merit at high temperatures. In this work, metal-induced crystallization (MIC) has been used to grow Si0.8Ge0.2 films that present improved thermoelectric performance (zT = 5.6 × 10-4 at room temperature)—according to previously reported values on films—with a relatively large power factor (σ · S 2 = 16 μW · m-1 · K-2). More importantly, a reduction in the thermal conductivity at room temperature (κ = 1.13 ± 0.12 W · m-1 · K-1) compared to other Si-Ge films (˜3 W · m-1 · K-1) has been found. Whereas the usual crystallization of amorphous SiGe (a-SiGe) is achieved at high temperatures and for long times, which triggers dopant loss, MIC reduces the crystallization temperature and the heating time. The associated dopant loss is thus avoided, resulting in a nanostructuration of the film. Using this method, we obtained Si0.8Ge0.2 films (grown by DC plasma sputtering) with appropriate compositional and structural properties. Different thermal treatments were tested in situ (by heating the sample inside the deposition chamber) and ex situ (annealed in an external furnace with controlled conditions). From the studies of the films by: x-ray diffraction (XRD), synchrotron radiation grazing incidence x-ray diffraction (SR-GIXRD), micro Raman, scanning electron microscopy (SEM), x-ray photoemission spectroscopy (XPS), Hall effect, Seebeck coefficient, electrical and thermal conductivity measurements, we observed that the in situ films at 500 °C presented the best zT values with no gold contamination.

Source identification of PM10, collected at a heavy-traffic roadside, by analyzing individual particles using synchrotron radiation.

PubMed

Yue, Weisheng; Li, Yan; Li, Xiaolin; Yu, Xiaohan; Deng, Biao; Liu, Jiangfeng; Wan, Tianmin; Zhang, Guilin; Huang, Yuying; He, Wei; Hua, Wei

2004-09-01

Synchrotron radiation microbeam X-ray fluorescence (micro-SXRF) was used to analyze individual aerosol particles collected at a height of 2 m above a heavy-traffic roadside in a heavy-industrial area of Shanghai. A pattern recognition technique, which took micro-SXRF spectra of single aerosol particles as its fingerprint, was used to identify the origins of the particles. The particles collected from the environmental monitoring site are mainly from metallurgic industry (26%), unleaded gasoline automobile exhaust (15%), coal combustion (10%), cement dust (10%) and motorcycle exhaust (8%).

Investigation of the structure of human dental tissue at multiple length scales using high energy synchrotron X-ray SAXS/WAXS

NASA Astrophysics Data System (ADS)

Sui, Tan; Landini, Gabriel; Korsunsky, Alexander M.

2011-10-01

High energy (>50keV) synchrotron X-ray scattering experiments were carried out on beamline I12 JEEP at the Diamond Light Source (DLS, Oxford, UK). Although a complete human tooth could be studied, in the present study attention was focused on coupons from the region of the Dentin-Enamel Junction (DEJ). Simultaneous high energy SAXS/WAXS measurements were carried out. Quantitative analysis of the results allows multiple length scale characterization of the nano-crystalline structure of dental tissues. SAXS patterns analysis provide insight into the mean thickness and orientation of hydroxyapatite particles, while WAXS (XRD) patterns allow the determination of the crystallographic unit cell parameters of the hydroxyapatite phase. It was found that the average particle thickness determined from SAXS interpretation varies as a function of position in the vicinity of the DEJ. Most mineral particles are randomly orientated within dentin, although preferred orientation emerges and becomes stronger on approach to the enamel. Within the enamel, texture is stronger than anywhere in the dentin, and the determination of lattice parameters can be accomplished by Pawley refinement of the multiple peak diffraction pattern. The results demonstrate the feasibility of using high energy synchrotron X-ray beams for the characterization of human dental tissues. This opens up the opportunity of studying thick samples (e.g., complete teeth) in complex sample environments (e.g., under saline solution). This opens new avenues for the application of high energy synchrotron X-ray scattering to dental research.

Comparative analysis of ex-situ and operando X-ray diffraction experiments for lithium insertion materials

NASA Astrophysics Data System (ADS)

Brant, William R.; Li, Dan; Gu, Qinfen; Schmid, Siegbert

2016-01-01

A comparative study of ex-situ and operando X-ray diffraction techniques using the fast lithium ion conductor Li0.18Sr0.66Ti0.5Nb0.5O3 is presented. Ex-situ analysis of synchrotron X-ray diffraction data suggests that a single phase material exists for all discharges to as low as 0.422 V. For samples discharged to 1 V or lower, i.e. with higher lithium content, it is possible to determine the lithium position from the X-ray data. However, operando X-ray diffraction from a coin cell reveals that a kinetically driven two phase region occurs during battery cycling below 1 V. Through monitoring the change in unit cell dimension during electrochemical cycling the dynamics of lithium insertion are explored. A reduction in the rate of unit cell expansion of 22(2)% part way through the first discharge and 13(1)% during the second discharge is observed. This reduction may be caused by a drop in lithium diffusion into the bulk material for higher lithium contents. A more significant change is a jump in the unit cell expansion by 60(2)% once the lithium content exceeds one lithium ion per vacant site. It is suggested that this jump is caused by damping of octahedral rotations, thus establishing a link between lithium content and octahedral rotations.

High Pressure X-Ray Diffraction Studies of Nanocrystalline Materials

NASA Technical Reports Server (NTRS)

Palosz, B.; Stel'makh, S.; Grzanka, E.; Gierlotka, S.; Palosz, W.

2004-01-01

Experimental evidence obtained for a variety of nanocrystalline materials suggest that the crystallographic structure of a very small size particle deviates from that in the bulk crystals. In this paper we show the effect of the surface of nanocrystals on their structure by the analysis of generation and distribution of macro- and micro-strains at high pressures and their dependence on the grain size in nanocrystalline powders of Sic. We studied the structure of Sic nanocrystals by in-situ high-pressure powder diffraction technique using synchrotron and neutron sources and hydrostatic or isostatic pressure conditions. The diffraction measurements were done in HASYLAB at DESY using a Diamond Anvil Cell (DAC) in the energy dispersive geometry in the diffraction vector range up to 3.5 - 4/A and under pressures up to 50 GPa at room temperature. In-situ high pressure neutron diffraction measurements were done at LANSCE in Los Alamos National Laboratory using the HIPD and HIPPO diffractometers with the Paris-Edinburgh and TAP-98 cells, respectively, in the diffraction vector range up to 26 Examination of the response of the material to external stresses requires nonstandard methodology of the materials characterization and description. Although every diffraction pattern contains a complete information on macro- and micro-strains, a high pressure experiment can reveal only those factors which contribute to the characteristic diffraction patterns of the crystalline phases present in the sample. The elastic properties of powders with the grain size from several nm to micrometers were examined using three methodologies: (l), the analysis of positions and widths of individual Bragg reflections (used for calculating macro- and micro-strains generated during densification) [I], (2). the analysis of the dependence of the experimental apparent lattice parameter, alp, on the diffraction vector Q [2], and (3), the atomic Pair Distribution Function (PDF) technique [3]. The results of our studies show, that Sic nanocrystals have the features of two phases, each with its distinct elastic properties. and under pressures up to 8 GPa.

In situ study of maize starch gelatinization under ultra-high hydrostatic pressure using X-ray diffraction.

PubMed

Yang, Zhi; Gu, Qinfen; Hemar, Yacine

2013-08-14

The gelatinization of waxy (very low amylose) and high-amylose maize starches by ultra-high hydrostatic pressure (up to 6 GPa) was investigated in situ using synchrotron X-ray powder diffraction on samples held in a diamond anvil cell (DAC). The starch pastes, made by mixing starch and water in a 1:1 ratio, were pressurized and measured at room temperature. X-ray diffraction pattern showed that at 2.7 GPa waxy starch, which displayed A-type XRD pattern at atmospheric pressure, exhibited a faint B-type-like pattern. The B-type crystalline structures of high-amylose starch were not affected even when 1.5 GPa pressure was applied. However, both waxy and high-amylose maize starches can be fully gelatinized at 5.9 GPa and 5.1 GPa, respectively. In the case of waxy maize starch, upon release of pressure (to atmospheric pressure) crystalline structure appeared as a result of amylopectin aggregation. Copyright © 2013 Elsevier Ltd. All rights reserved.

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.

The role of iron in neurodegenerative disorders: insights and opportunities with synchrotron light

PubMed Central

Collingwood, Joanna F.; Davidson, Mark R.

2014-01-01

There is evidence for iron dysregulation in many forms of disease, including a broad spectrum of neurodegenerative disorders. In order to advance our understanding of the pathophysiological role of iron, it is helpful to be able to determine in detail the distribution of iron as it relates to metabolites, proteins, cells, and tissues, the chemical state and local environment of iron, and its relationship with other metal elements. Synchrotron light sources, providing primarily X-ray beams accompanied by access to longer wavelengths such as infra-red, are an outstanding tool for multi-modal non-destructive analysis of iron in these systems. The micro- and nano-focused X-ray beams that are generated at synchrotron facilities enable measurement of iron and other transition metal elements to be performed with outstanding analytic sensitivity and specificity. Recent developments have increased the scope for methods such as X-ray fluorescence mapping to be used quantitatively rather than semi-quantitatively. Burgeoning interest, coupled with technical advances and beamline development at synchrotron facilities, has led to substantial improvements in resources and methodologies in the field over the past decade. In this paper we will consider how the field has evolved with regard to the study of iron in proteins, cells, and brain tissue, and identify challenges in sample preparation and analysis. Selected examples will be used to illustrate the contribution, and future potential, of synchrotron X-ray analysis for the characterization of iron in model systems exhibiting iron dysregulation, and for human cases of neurodegenerative disorders including Alzheimer’s disease, Parkinson’s disease, Friedreich’s ataxia, and amyotrophic lateral sclerosis. PMID:25191270

Microscopy of biological sample through advanced diffractive optics from visible to X-ray wavelength regime.

PubMed

Di Fabrizio, Enzo; Cojoc, Dan; Emiliani, Valentina; Cabrini, Stefano; Coppey-Moisan, Maite; Ferrari, Enrico; Garbin, Valeria; Altissimo, Matteo

2004-11-01

The aim of this report is to demonstrate a unified version of microscopy through the use of advanced diffractive optics. The unified scheme derives from the technical possibility of realizing front wave engineering in a wide range of electromagnetic spectrum. The unified treatment is realized through the design and nanofabrication of phase diffractive elements (PDE) through which wave front beam shaping is obtained. In particular, we will show applications, by using biological samples, ranging from micromanipulation using optical tweezers to X-ray differential interference contrast (DIC) microscopy combined with X-ray fluorescence. We report some details on the design and physical implementation of diffractive elements that besides focusing also perform other optical functions: beam splitting, beam intensity, and phase redistribution or mode conversion. Laser beam splitting is used for multiple trapping and independent manipulation of micro-beads surrounding a cell as an array of tweezers and for arraying and sorting microscopic size biological samples. Another application is the Gauss to Laguerre-Gauss mode conversion, which allows for trapping and transfering orbital angular momentum of light to micro-particles immersed in a fluid. These experiments are performed in an inverted optical microscope coupled with an infrared laser beam and a spatial light modulator for diffractive optics implementation. High-resolution optics, fabricated by means of e-beam lithography, are demonstrated to control the intensity and the phase of the sheared beams in x-ray DIC microscopy. DIC experiments with phase objects reveal a dramatic increase in image contrast compared to bright-field x-ray microscopy. Besides the topographic information, fluorescence allows detection of certain chemical elements (Cl, P, Sc, K) in the same setup, by changing the photon energy of the x-ray beam. (c) 2005 Wiley-Liss, Inc.

Grid-enhanced X-ray coded aperture microscopy with polycapillary optics

PubMed Central

Sowa, Katarzyna M.; Last, Arndt; Korecki, Paweł

2017-01-01

Polycapillary devices focus X-rays by means of multiple reflections of X-rays in arrays of bent glass capillaries. The size of the focal spot (typically 10–100 μm) limits the resolution of scanning, absorption and phase-contrast X-ray imaging using these devices. At the expense of a moderate resolution, polycapillary elements provide high intensity and are frequently used for X-ray micro-imaging with both synchrotrons and X-ray tubes. Recent studies have shown that the internal microstructure of such an optics can be used as a coded aperture that encodes high-resolution information about objects located inside the focal spot. However, further improvements to this variant of X-ray microscopy will require the challenging fabrication of tailored devices with a well-defined capillary microstructure. Here, we show that submicron coded aperture microscopy can be realized using a periodic grid that is placed at the output surface of a polycapillary optics. Grid-enhanced X-ray coded aperture microscopy with polycapillary optics does not rely on the specific microstructure of the optics but rather takes advantage only of its focusing properties. Hence, submicron X-ray imaging can be realized with standard polycapillary devices and existing set-ups for micro X-ray fluorescence spectroscopy. PMID:28322316

Grid-enhanced X-ray coded aperture microscopy with polycapillary optics.

PubMed

Sowa, Katarzyna M; Last, Arndt; Korecki, Paweł

2017-03-21

Polycapillary devices focus X-rays by means of multiple reflections of X-rays in arrays of bent glass capillaries. The size of the focal spot (typically 10-100 μm) limits the resolution of scanning, absorption and phase-contrast X-ray imaging using these devices. At the expense of a moderate resolution, polycapillary elements provide high intensity and are frequently used for X-ray micro-imaging with both synchrotrons and X-ray tubes. Recent studies have shown that the internal microstructure of such an optics can be used as a coded aperture that encodes high-resolution information about objects located inside the focal spot. However, further improvements to this variant of X-ray microscopy will require the challenging fabrication of tailored devices with a well-defined capillary microstructure. Here, we show that submicron coded aperture microscopy can be realized using a periodic grid that is placed at the output surface of a polycapillary optics. Grid-enhanced X-ray coded aperture microscopy with polycapillary optics does not rely on the specific microstructure of the optics but rather takes advantage only of its focusing properties. Hence, submicron X-ray imaging can be realized with standard polycapillary devices and existing set-ups for micro X-ray fluorescence spectroscopy.

Real time observation of mouse fetal skeleton using a high resolution X-ray synchrotron

PubMed Central

Chang, Dong Woo; Kim, Bora; Shin, Jae Hoon; Yun, Young Min; Je, Jung Ho; Hwu, Yeu kuang; Yoon, Jung Hee

2011-01-01

The X-ray synchrotron is quite different from conventional radiation sources. This technique may expand the capabilities of conventional radiology and be applied in novel manners for special cases. To evaluate the usefulness of X-ray synchrotron radiation systems for real time observations, mouse fetal skeleton development was monitored with a high resolution X-ray synchrotron. A non-monochromatized X-ray synchrotron (white beam, 5C1 beamline) was employed to observe the skeleton of mice under anesthesia at embryonic day (E)12, E14, E15, and E18. At the same time, conventional radiography and mammography were used to compare with X-ray synchrotron. After synchrotron radiation, each mouse was sacrificed and stained with Alizarin red S and Alcian blue to observe bony structures. Synchrotron radiation enabled us to view the mouse fetal skeleton beginning at gestation. Synchrotron radiation systems facilitate real time observations of the fetal skeleton with greater accuracy and magnification compared to mammography and conventional radiography. Our results show that X-ray synchrotron systems can be used to observe the fine structures of internal organs at high magnification. PMID:21586868

Polyglycolic Acid–Polylactic Acid Scaffold Response to Different Progenitor Cell In Vitro Cultures: A Demonstrative and Comparative X-Ray Synchrotron Radiation Phase-Contrast Microtomography Study

PubMed Central

Moroncini, Francesca; Mazzoni, Serena; Belicchi, Marzia Laura Chiara; Villa, Chiara; Erratico, Silvia; Colombo, Elena; Calcaterra, Francesca; Brambilla, Lucia; Torrente, Yvan; Albertini, Gianni; Della Bella, Silvia

2014-01-01

Spatiotemporal interactions play important roles in tissue development and function, especially in stem cell-seeded bioscaffolds. Cells interact with the surface of bioscaffold polymers and influence material-driven control of cell differentiation. In vitro cultures of different human progenitor cells, that is, endothelial colony-forming cells (ECFCs) from a healthy control and a patient with Kaposi sarcoma (an angioproliferative disease) and human CD133+ muscle-derived stem cells (MSH 133+ cells), were seeded onto polyglycolic acid–polylactic acid scaffolds. Three-dimensional (3D) images were obtained by X-ray phase-contrast microtomography (micro-CT) and processed with the Modified Bronnikov Algorithm. The method enabled high spatial resolution detection of the 3D structural organization of cells on the bioscaffold and evaluation of the way and rate at which cells modified the construct at different time points from seeding. The different cell types displayed significant differences in the proliferation rate. In conclusion, X-ray synchrotron radiation phase-contrast micro-CT analysis proved to be a useful and sensitive tool to investigate the spatiotemporal pattern of progenitor cell organization on a bioscaffold. PMID:23879738

Characterization of a human tooth with carious lesions using conventional and synchrotron radiation-based micro computed tomography

NASA Astrophysics Data System (ADS)

Dziadowiec, Iwona; Beckmann, Felix; Schulz, Georg; Deyhle, Hans; Müller, Bert

2014-09-01

In a dental office, every day X rays of teeth within the oral cavity are obtained. Caries induces a mineral loss and, therefore, becomes visible by reduced X-ray absorption. The detailed spatial distribution of the mineral loss, however, is inaccessible in conventional dental radiology, since the dose for such studies is intolerable. As a consequence, such measurements can only be performed after tooth extraction. We have taken advantage of synchrotron radiation-based micro computed tomography to characterize a human tooth with a rather small, natural caries lesion and an artificially induced lesion provoked by acidic etching. Both halves of the tooth were separately visualized from 2400 radiographs recorded at the beam line P07 / PETRA III (HASYLAB at DESY, Hamburg, Germany) with an asymmetric rotation axis at photon energy of 45 keV. Because of the setup, one finds an energy shift in the horizontal plane, to be corrected. After the appropriate three-dimensional registration of the data with the ones of the same crown using the better accessible phoenix nanotom® m of General Electric, Wunstorf, Germany, one can determine the joint histogram, which enable to calibrate the system with the conventional X-ray source.

Lattice-Preferred Orientation in Deformed Novaculite - Comparison of in-situ Results Using BEARTEX and Post-Mortem EBSD Analyses

NASA Astrophysics Data System (ADS)

Willenweber, A.; Thomas, S.; Burnley, P. C.

2012-12-01

The Berkeley Texture Package BEARTEX is a Windows-based computer software that combines various algorithms to analyze lattice-preferred orientation in polycrystalline materials. BEARTEX was initially designed to interpret diffraction intensity data from pole figure goniometers. Recently it has been successfully used to process synthetic forsterite powder diffraction data from in-situ synchrotron X-ray diffraction taken during deformation (Bollinger et al. 2012). Our study aims to test the practicability of using BEARTEX to analyze the evolution of lattice-preferred orientation in natural polycrystalline quartz (novaculite) during deformation. In-situ X-ray diffraction data was collected during the deformation of novaculite at 2.5 GPa and up to 1000 °C in a D-DIA apparatus using the ten-element energy-dispersive detector at the NSLS beamline X17B2. Diffraction intensities are a function of crystal orientation, expressed in azimuth angle η and pole distance ψ. The latter is the angle between the normal of a given diffraction plane and the vertical direction of the D-DIA apparatus - our principal stress direction during compression. Orientation-dependent diffraction intensities were corrected for different responses of the single detectors and x-ray absorption effects of the anvils. Orientation distributions (ODs) and inverse pole figures were calculated using BEARTEX. In addition, electron backscatter diffraction (EBSD) analyses were carried out on the deformed novaculite samples. Generated pole figures were compared with those derived from BEARTEX. Textural properties of our novaculite starting material complicated the BEARTEX analyses. The relatively strong variation of grain sizes in our natural specimens caused non-random diffraction intensity distributions. Those lead to non-random distributions of crystal orientations when analyzed with BEARTEX, although pole figures from EBSD data clearly show random crystal orientations. In an attempt to solve this problem, we employed a scanning routine when recording in-situ synchrotron X-ray diffraction and so collected diffraction from multiple sample volumes rather than from one single spot. Here, we will present a comparison of pole figures derived from independent BEARTEX and EBSD analyses for a series of novaculite experiments and discuss the practicability of BEARTEX to analyze the evolution of lattice-preferred orientation in natural polycrystalline quartz. REFERENCES C. BOLLINGER, S. MERKEL AND P. RATERRON (2012): In situ quantitative analysis of stress and texture development in forsterite aggregates deformed at 6 GPa and 1373 K. J. Appl. Cryst., 45, 263-271.

3D/4D analyses of damage and fracture behaviours in structural materials via synchrotron X-ray tomography.

PubMed

Toda, Hiroyuki

2014-11-01

X-ray microtomography has been utilized for the in-situ observation of various structural metals under external loading. Recent advances in X-ray microtomography provide remarkable tools to image the interior of materials. In-situ X-ray microtomography provides a unique possibility to access the 3D character of internal microstructure and its time evolution behaviours non-destructively, thereby enabling advanced techniques for measuring local strain distribution. Local strain mapping is readily enabled by processing such high-resolution tomographic images either by the particle tracking technique or the digital image correlation technique [1]. Procedures for tracking microstructural features which have been developed by the authors [2], have been applied to analyse localised deformation and damage evolution in a material [3]. Typically several tens of thousands of microstructural features, such as particles and pores, are tracked in a tomographic specimen (0.2 - 0.3 mm(3) in volume). When a sufficient number of microstructural features is dispersed in 3D space, the Delaunay tessellation algorithm is used to obtain local strain distribution. With these techniques, 3D strain fields can be measured with reasonable accuracy. Even local crack driving forces, such as local variations in the stress intensity factor, crack tip opening displacement and J integral along a crack front line, can be measured from discrete crack tip displacement fields [4]. In the present presentation, complicated crack initiation and growth behaviour and the extensive formation of micro cracks ahead of a crack tip are introduced as examples.A novel experimental method has recently been developed by amalgamating a pencil beam X-Ray diffraction (XRD) technique with the microstructural tracking technique [5]. The technique provides information about individual grain orientations and 1-micron-level grain morphologies in 3D together with high-density local strain mapping. The application of this technique to the deformation behavior of a polycrystalline aluminium alloy will be demonstrated in the presentation [6].The synchrotron-based microtomography has been mainly utilized to light materials due to their good X-ray transmission. In the present talk, the application of the synchrotron-based microtomography to steels will be also introduced. Degradation of contrast and spatial resolution due to forward scattering could be avoided by selecting appropriate experimental conditions in order to obtain superior spatial resolution close to the physical limit even in ferrous materials [7]. © The Author 2014. Published by Oxford University Press on behalf of The Japanese Society of Microscopy. All rights reserved. For permissions, please e-mail: journals.permissions@oup.com.

Confinement-induced liquid ordering investigated by x-ray phase retrieval

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

Bunk, Oliver; Diaz, Ana; Pfeiffer, Franz

2007-02-15

Using synchrotron x-ray diffraction, we have determined the ensemble-averaged density profile of colloidal fluids within confining channels of different widths. We observe an oscillatory ordering-disordering behavior of the colloidal particles as a function of the channel width, while the colloidal solution remains in the liquid state. This phenomenon has been suggested by surface force studies of hard-sphere fluids and also theoretically predicted, but here we see it by direct measurements of the structure for comparable systems.

One body, many heads; the Cerberus of catalysis. A new multipurpose in-situ cell for XAS at ALBA

NASA Astrophysics Data System (ADS)

Guilera, G.; Rey, F.; Hernández-Fenollosa, J.; Cortés-Vergaz, J. J.

2013-04-01

A new multi-purpose in-situ cell and its control system have been developed for synchrotron-based techniques as are X-Ray Absorption spectroscopy (XAS) and X-Ray Diffraction (XRD). The cell is made of a stainless steel 'body' and three different exchangeable 'heads' to tackle different scientific areas that include solid-gas catalysis, solid-liquid catalysis and electrocatalysis. The different versions of the cell are herein described and their functionality is exemplified by some case studies.

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.

Structures of Astromaterials Revealed by EBSD

NASA Technical Reports Server (NTRS)

Zolensky, M.

2018-01-01

Groups at the Johnson Space Center and the University of Tokyo have been using electron back-scattered diffraction (EBSD) to reveal the crystal structures of extraterrestrial minerals for many years. Even though we also routinely use transmission electron microscopy, synchrotron X-ray diffraction (SXRD), and conventional electron diffraction, we find that EBSD is the most powerful technique for crystal structure elucidation in many instances. In this talk I describe a few of the cases where we have found EBSD to provide crucial, unique information. See attachment.

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.

Synchrotron X-ray microscopy and spectroscopy analysis of iron in hemochromatosis liver and intestines

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

Ko, J .Y. Peter; Sham, Tsun-Kong; Chakrabarti, Subrata

2009-12-01

Hemochromatosis is a genetic disorder that causes body to store excess iron in organs such as heart or liver. Distribution of iron, as well as copper, zinc and calcium, and chemical identity of iron in hemochromatosis liver and intestine were investigated by X-ray microprobe experiments, which consist of X-ray microscopy and micro-X-ray absorption fine structure. Our results show that iron concentration in hemochromatosis liver tissue is high, while much less Fe is found in intestinal tissue. Moreover, chemical identity of Fe in hemochromatosis liver can be identified. X-ray microprobe experiments allows for examining elemental distribution at an excellent spatial resolution.more » Moreover, chemical identity of element of interest can be obtained.« less

Imaging local electric fields produced upon synchrotron X-ray exposure

DOE PAGES

Dettmar, Christopher M.; Newman, Justin A.; Toth, Scott J.; ...

2014-12-31

Electron–hole separation following hard X-ray absorption during diffraction analysis of soft materials under cryogenic conditions produces substantial local electric fields visualizable by second harmonic generation (SHG) microscopy. Monte Carlo simulations of X-ray photoelectron trajectories suggest the formation of substantial local electric fields in the regions adjacent to those exposed to X-rays, indicating a possible electric-field–induced SHG (EFISH) mechanism for generating the observed signal. In studies of amorphous vitreous solvents, analysis of the SHG spatial profiles following X-ray microbeam exposure was consistent with an EFISH mechanism. Within protein crystals, exposure to 12-keV (1.033-Å) X-rays resulted in increased SHG in the regionmore » extending ~3 μm beyond the borders of the X-ray beam. Moderate X-ray exposures typical of those used for crystal centering by raster scanning through an X-ray beam were sufficient to produce static electric fields easily detectable by SHG. The X-ray–induced SHG activity was observed with no measurable loss for longer than 2 wk while maintained under cryogenic conditions, but disappeared if annealed to room temperature for a few seconds. In conclusion, these results provide direct experimental observables capable of validating simulations of X-ray–induced damage within soft materials. Additionally, X-ray–induced local fields may potentially impact diffraction resolution through localized piezoelectric distortions of the lattice.« less

Energy resolution of the CdTe-XPAD detector: calibration and potential for Laue diffraction measurements on protein crystals.

PubMed

Medjoubi, Kadda; Thompson, Andrew; Bérar, Jean-François; Clemens, Jean-Claude; Delpierre, Pierre; Da Silva, Paulo; Dinkespiler, Bernard; Fourme, Roger; Gourhant, Patrick; Guimaraes, Beatriz; Hustache, Stéphanie; Idir, Mourad; Itié, Jean-Paul; Legrand, Pierre; Menneglier, Claude; Mercere, Pascal; Picca, Frederic; Samama, Jean-Pierre

2012-05-01

The XPAD3S-CdTe, a CdTe photon-counting pixel array detector, has been used to measure the energy and the intensity of the white-beam diffraction from a lysozyme crystal. A method was developed to calibrate the detector in terms of energy, allowing incident photon energy measurement to high resolution (approximately 140 eV), opening up new possibilities in energy-resolved X-ray diffraction. In order to demonstrate this, Laue diffraction experiments were performed on the bending-magnet beamline METROLOGIE at Synchrotron SOLEIL. The X-ray energy spectra of diffracted spots were deduced from the indexed Laue patterns collected with an imaging-plate detector and then measured with both the XPAD3S-CdTe and the XPAD3S-Si, a silicon photon-counting pixel array detector. The predicted and measured energy of selected diffraction spots are in good agreement, demonstrating the reliability of the calibration method. These results open up the way to direct unit-cell parameter determination and the measurement of high-quality Laue data even at low resolution. Based on the success of these measurements, potential applications in X-ray diffraction opened up by this type of technology are discussed.

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.

Noise properties and task-based evaluation of diffraction-enhanced imaging

PubMed Central

Brankov, Jovan G.; Saiz-Herranz, Alejandro; Wernick, Miles N.

2014-01-01

Abstract. Diffraction-enhanced imaging (DEI) is an emerging x-ray imaging method that simultaneously yields x-ray attenuation and refraction images and holds great promise for soft-tissue imaging. The DEI has been mainly studied using synchrotron sources, but efforts have been made to transition the technology to more practical implementations using conventional x-ray sources. The main technical challenge of this transition lies in the relatively lower x-ray flux obtained from conventional sources, leading to photon-limited data contaminated by Poisson noise. Several issues that must be understood in order to design and optimize DEI imaging systems with respect to noise performance are addressed. Specifically, we: (a) develop equations describing the noise properties of DEI images, (b) derive the conditions under which the DEI algorithm is statistically optimal, (c) characterize the imaging performance that can be obtained as measured by task-based metrics, and (d) consider image-processing steps that may be employed to mitigate noise effects. PMID:26158056

Compensation of X-ray mirror shape-errors using refractive optics

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

Sawhney, Kawal, E-mail: Kawal.sawhney@diamond.ac.uk; Laundy, David; Pape, Ian

2016-08-01

Focusing of X-rays to nanometre scale focal spots requires high precision X-ray optics. For nano-focusing mirrors, height errors in the mirror surface retard or advance the X-ray wavefront and after propagation to the focal plane, this distortion of the wavefront causes blurring of the focus resulting in a limit on the spatial resolution. We describe here the implementation of a method for correcting the wavefront that is applied before a focusing mirror using custom-designed refracting structures which locally cancel out the wavefront distortion from the mirror. We demonstrate in measurements on a synchrotron radiation beamline a reduction in the sizemore » of the focal spot of a characterized test mirror by a factor of greater than 10 times. This technique could be used to correct existing synchrotron beamline focusing and nanofocusing optics providing a highly stable wavefront with low distortion for obtaining smaller focus sizes. This method could also correct multilayer or focusing crystal optics allowing larger numerical apertures to be used in order to reduce the diffraction limited focal spot size.« less

In situ surface/interface x-ray diffractometer for oxide molecular beam epitaxy

NASA Astrophysics Data System (ADS)

Lee, J. H.; Tung, I. C.; Chang, S.-H.; Bhattacharya, A.; Fong, D. D.; Freeland, J. W.; Hong, Hawoong

2016-01-01

In situ studies of oxide molecular beam epitaxy by synchrotron x-ray scattering has been made possible by upgrading an existing UHV/molecular beam epitaxy (MBE) six-circle diffractometer system. For oxide MBE growth, pure ozone delivery to the chamber has been made available, and several new deposition sources have been made available on a new 12 in. CF (ConFlat, a registered trademark of Varian, Inc.) flange. X-ray diffraction has been used as a major probe for film growth and structures for the system. In the original design, electron diffraction was intended for the secondary diagnostics available without the necessity of the x-ray and located at separate positions. Deposition of films was made possible at the two diagnostic positions. And, the aiming of the evaporation sources is fixed to the point between two locations. Ozone can be supplied through two separate nozzles for each location. Also two separate thickness monitors are installed. Additional features of the equipment are also presented together with the data taken during typical oxide film growth to illustrate the depth of information available via in situ x-ray techniques.

In situ surface/interface x-ray diffractometer for oxide molecular beam epitaxy.

PubMed

Lee, J H; Tung, I C; Chang, S-H; Bhattacharya, A; Fong, D D; Freeland, J W; Hong, Hawoong

2016-01-01

In situ studies of oxide molecular beam epitaxy by synchrotron x-ray scattering has been made possible by upgrading an existing UHV/molecular beam epitaxy (MBE) six-circle diffractometer system. For oxide MBE growth, pure ozone delivery to the chamber has been made available, and several new deposition sources have been made available on a new 12 in. CF (ConFlat, a registered trademark of Varian, Inc.) flange. X-ray diffraction has been used as a major probe for film growth and structures for the system. In the original design, electron diffraction was intended for the secondary diagnostics available without the necessity of the x-ray and located at separate positions. Deposition of films was made possible at the two diagnostic positions. And, the aiming of the evaporation sources is fixed to the point between two locations. Ozone can be supplied through two separate nozzles for each location. Also two separate thickness monitors are installed. Additional features of the equipment are also presented together with the data taken during typical oxide film growth to illustrate the depth of information available via in situ x-ray techniques.

Coherent Synchrotron-Based Micro-Imaging Employed for Studies of Micro-Gap Formation in Dental Implants

NASA Astrophysics Data System (ADS)

Rack, T.; Zabler, S.; Rack, A.; Stiller, M.; Riesemeier, H.; Cecilia, A.; Nelson, K.

2011-09-01

Biocompatible materials such as titanium are regularly applied in oral surgery. Titanium-based implants for the replacement of missing teeth demand a high mechanical precision in order to minimize micro-bacterial leakage, especially when two-piece concepts are used. Synchrotron-based hard x-ray radiography, unlike conventional laboratory radiography, allows high spatial resolution in combination with high contrast even when micro-sized features in such highly attenuating objects are visualized. Therefore, micro-gap formation at interfaces in two-piece dental implants with the sample under different mechanical loads can be studied. We show the existence of micro-gaps in implants with conical connections and study the mechanical behavior of the mating zone of conical implants during loading. The micro-gap is a potential source of implant failure, i.e., bacterial leakage, which can be a stimulus for an inflammatory process.

Coherent Synchrotron-Based Micro-Imaging Employed for Studies of Micro-Gap Formation in Dental Implants

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

Rack, T.; Stiller, M.; Nelson, K.

Biocompatible materials such as titanium are regularly applied in oral surgery. Titanium-based implants for the replacement of missing teeth demand a high mechanical precision in order to minimize micro-bacterial leakage, especially when two-piece concepts are used. Synchrotron-based hard x-ray radiography, unlike conventional laboratory radiography, allows high spatial resolution in combination with high contrast even when micro-sized features in such highly attenuating objects are visualized. Therefore, micro-gap formation at interfaces in two-piece dental implants with the sample under different mechanical loads can be studied. We show the existence of micro-gaps in implants with conical connections and study the mechanical behavior ofmore » the mating zone of conical implants during loading. The micro-gap is a potential source of implant failure, i.e., bacterial leakage, which can be a stimulus for an inflammatory process.« less

Isolation, purification, crystallization, and preliminary X-ray diffraction study of the crystals of HU protein from M. gallisepticum

NASA Astrophysics Data System (ADS)

Nikolaeva, A. Yu.; Timofeev, V. I.; Boiko, K. M.; Korzhenevskii, D. A.; Rakitina, T. V.; Dorovatovskii, P. V.; Lipkin, A. V.

2015-11-01

HU proteins are involved in bacterial DNA and RNA repair. Since these proteins are absent in cells of higher organisms, inhibitors of HU proteins can be used as effective and safe antibiotics. The crystallization conditions for the M. gallisepticum HU protein were found and optimized by the vapor-diffusion method. The X-ray diffraction data set was collected to 2.91 Å resolution from the crystals grown by the vapor-diffusion method on a synchrotron source. The crystals of the HU protein belong to sp. gr. P41212 and have the following unit-cell parameters: a = b = 97.94 Å, c = 77.92 Å, α = β = γ = 90°.

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.

Transmission in situ and operando high temperature X-ray powder diffraction in variable gaseous environments

NASA Astrophysics Data System (ADS)

Schlicker, Lukas; Doran, Andrew; Schneppmüller, Peter; Gili, Albert; Czasny, Mathias; Penner, Simon; Gurlo, Aleksander

2018-03-01

This work describes a device for time-resolved synchrotron-based in situ and operando X-ray powder diffraction measurements at elevated temperatures under controllable gaseous environments. The respective gaseous sample environment is realized via a gas-tight capillary-in-capillary design, where the gas flow is achieved through an open-end 0.5 mm capillary located inside a 0.7 mm capillary filled with a sample powder. Thermal mass flow controllers provide appropriate gas flows and computer-controlled on-the-fly gas mixing capabilities. The capillary system is centered inside an infrared heated, proportional integral differential-controlled capillary furnace allowing access to temperatures up to 1000 °C.

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.

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.

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

Mazuritskiy, M. I., E-mail: mazurmik@gmail.com; Lerer, A. M.; Makhno, P. V.

The angular distribution of the X-ray intensity at the exit of microchannel plates at grazing incidence of monochromatic radiation on the walls of microcapillaries has been investigated. The angles and energies of the primary radiation quanta at which the synchrotron beam excites X-ray fluorescence propagating inside polycapillary structures have been determined. The angular dependences of the intensity distribution of X-rays transmitted through the microcapillaries have been studied theoretically and experimentally for energies corresponding to the region of anomalous dispersion near the L{sub 2,3} absorption edges of silicon. The propagation of waves in hollow polycapillary waveguides, the excitation of X-ray fluorescence,more » and the X-ray diffraction at the exit of microchannel plates have been modeled mathematically. The mathematical model takes into account the presence of a transition layer on the microchannel surface.« less

3D Imaging of Microbial Biofilms: Integration of Synchrotron Imaging and an Interactive Visualization Interface

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

Thomas, Mathew; Marshall, Matthew J.; Miller, Erin A.

2014-08-26

Understanding the interactions of structured communities known as “biofilms” and other complex matrixes is possible through the X-ray micro tomography imaging of the biofilms. Feature detection and image processing for this type of data focuses on efficiently identifying and segmenting biofilms and bacteria in the datasets. The datasets are very large and often require manual interventions due to low contrast between objects and high noise levels. Thus new software is required for the effectual interpretation and analysis of the data. This work specifies the evolution and application of the ability to analyze and visualize high resolution X-ray micro tomography datasets.

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

Aldridge, James D.; Womick, Jordan M.; Rosmus, Kimberly A.

Novel quaternary lanthanide-substituted oxides of stoichiometry LnxY2-xTi2O7 (where Ln is lanthanum, neodymium, samarium, gadolinium, or ytterbium) were prepared by traditional high-temperature, solid-state techniques and characterized by X-ray powder diffraction. Samples with nominal values of x up to 1.0 were attempted. The well-studied ternary cubic pyrochlore compound yttrium titanium oxide (Y2Ti2O7, space group Fd-3m, Z = 8), served as a parent structural framework in which Ln3+ cations were substituted on the Y3+ site. Laboratory-grade X-ray powder diffraction data revealed pure quaternary pyrochlore phases for LnxY2-xTi2O7 with x ≤ 0.2. Pyrochlore phase purity was verified by Rietveld analysis using high-resolution synchrotron X-raymore » powder diffraction data when x ≤ 0.2, however, for La3+ substitution specifically, pure quaternary pyrochlore formed at x<0.1. Band gap energies on selected samples were determined using optical diffuse reflectance spectroscopy and showed that these materials can be classified as electrical insulators with indirect band gap energies around 3.7 eV.« less

Characterization of fossil remains using XRF, XPS and XAFS spectroscopies

NASA Astrophysics Data System (ADS)

Zougrou, I. M.; Katsikini, M.; Pinakidou, F.; Brzhezinskaya, M.; Papadopoulou, L.; Vlachos, E.; Tsoukala, E.; Paloura, E. C.

2016-05-01

Synchrotron radiation micro-X-Ray Fluorescence (μ-XRF), X-ray photoelectron (XPS) and X-ray Absorption Fine Structure (XAFS) spectroscopies are applied for the study of paleontological findings. More specifically the costal plate of a gigantic terrestrial turtle Titanochelon bacharidisi and a fossilized coprolite of the cave spotted hyena Crocuta crocuta spelaea are studied. Ca L 2,3-edge NEXAFS and Ca 2p XPS are applied for the identification and quantification of apatite and Ca containing minerals. XRF mapping and XAFS are employed for the study of the spatial distribution and speciation of the minerals related to the deposition environment.

X-ray pushing of a mechanical microswing.

PubMed

Siria, A; Rodrigues, M S; Dhez, O; Schwartz, W; Torricelli, G; Ledenmat, S; Rochat, N; Auvert, G; Bikondoa, O; Metzger, T H; Wermeille, D; Felici, R; Comin, F; Chevrier, J

2008-11-05

We report here for the first time the combination of x-ray synchrotron light and a micro-electro-mechanical system (MEMS). We show how it is possible to modulate in real time a MEMS mass distribution to induce a nanometric and tunable mechanical oscillation. The quantitative experimental demonstration we present here uses periodic thermal dilatation of a Ge microcrystal attached to a Si microlever, induced by controlled absorption of an intensity modulated x-ray microbeam. The mechanism proposed can be envisaged either for the detection of small heat flux or for the actuation of a mechanical system.

Deformation Behavior of Cementite in Deformed High Carbon Steel Observed by X-ray Diffraction with Synchrotron Radiation

NASA Astrophysics Data System (ADS)

Taniyama, Akira; Takayama, Toru; Arai, Masahiro; Hamada, Takanari

2017-10-01

The deformation behavior of cementite in drawn pearlitic steel and spheroidal cementite steel, which have hypereutectoid composition, was investigated by X-ray diffraction using synchrotron radiation. A detailed analysis of diffraction peak profiles reveals that the deformation behavior strongly depends on the shape of cementite in steel. The unit cell volume of the cementite in the drawn pearlitic steel compressively and elastically deforms by 1.5 to 2 pct of the initial volume at the early stage of drawing, whereas that in the drawn spheroidal cementite steel is compressed by 1 pct of the initial volume even at a large true strain. The cementite in the drawn pearlitic steel fragments into small pieces with increasing the true strain, and these pieces change to amorphous cementite. The dislocation densities of the cementite in the drawn pearlitic steel and in the drawn spheroidal cementite steel are estimated to be 1013/m2 before drawing and 1014/m2 after drawing. Although the large strain is induced in the cementite by drawing, the maximum strain energy in the cementite is too small to contribute to the dissolution of the cementite.

A synchrotron X-ray diffraction deconvolution method for the measurement of residual stress in thermal barrier coatings as a function of depth.

PubMed

Li, C; Jacques, S D M; Chen, Y; Daisenberger, D; Xiao, P; Markocsan, N; Nylen, P; Cernik, R J

2016-12-01

The average residual stress distribution as a function of depth in an air plasma-sprayed yttria stabilized zirconia top coat used in thermal barrier coating (TBC) systems was measured using synchrotron radiation X-ray diffraction in reflection geometry on station I15 at Diamond Light Source, UK, employing a series of incidence angles. The stress values were calculated from data deconvoluted from diffraction patterns collected at increasing depths. The stress was found to be compressive through the thickness of the TBC and a fluctuation in the trend of the stress profile was indicated in some samples. Typically this fluctuation was observed to increase from the surface to the middle of the coating, decrease a little and then increase again towards the interface. The stress at the interface region was observed to be around 300 MPa, which agrees well with the reported values. The trend of the observed residual stress was found to be related to the crack distribution in the samples, in particular a large crack propagating from the middle of the coating. The method shows promise for the development of a nondestructive test for as-manufactured samples.

Controlled nucleation and growth of CdS nanoparticles in a polymer matrix.

PubMed

Di Luccio, Tiziana; Laera, Anna Maria; Tapfer, Leander; Kempter, Susanne; Kraus, Robert; Nickel, Bert

2006-06-29

In-situ synchrotron X-ray diffraction (XRD) was used to monitor the thermal decomposition (thermolysis) of Cd thiolates precursors embedded in a polymer matrix and the nucleation of CdS nanoparticles. A thiolate precursor/polymer solid foil was heated to 300 degrees C in the X-ray diffraction setup of beamline W1.1 at Hasylab, and the diffraction curves were each recorded at 10 degrees C. At temperatures above 240 degrees C, the precursor decomposition is complete and CdS nanoparticles grow within the polymer matrix forming a nanocomposite with interesting optical properties. The nanoparticle structural properties (size and crystal structure) depend on the annealing temperature. Transmission electron microscopy (TEM) and photoluminescence (PL) analyses were used to characterize the nanoparticles. A possible mechanism driving the structural transformation of the precursor is inferred from the diffraction features arising at the different temperatures.

Use of synchrotron radiation to characterize metals in plants: the case of Cd in the hyperacumulator Arabidopsis halleri

NASA Astrophysics Data System (ADS)

Isaure, M.; Sarret, G.; Verbruggen, N.

2010-12-01

Phytoremediation uses plants to extract (phytoextraction) or stabilize (phytostabilization) metals accumulated in soils, and can be an alternative to invasive physico-chemical remediation techniques. Its development requires the knowledge of the mechanisms involved in metal tolerance and accumulation in plants, and particularly the way that plants transfer and store metals. In that context, synchrotron radiation based techniques such as micro-focused X-Ray Fluorescence (µXRF), and micro-focused X-ray Absorption Spectroscopy, including Extended X-ray Absorption Fine Structure and X-ray Absorption Near Edge Structure, are particularly suited to determine the localization and the chemical forms of metals in the different tissues, cells and sub-cellular compartments. Arabidopsis halleri is a Zn, Cd hyperaccumulating plant, naturally growing on contaminated sites, and is a model plant to investigate metal hyperaccumulation. This work presents the application of µXRF and Cd µXANES to determine the distribution and speciation of Cd in this species. Results showed that Cd was mainly located in the mesophyll and veins of leaves. It is bound to S ligands in some leaves and to O/N ligands in other ones, and the observed variations may be related to the age of the leaves. Cd speciation seems to differ from other metals, and particularly Zn, generally encountered in hyperaccumulators. High local Cd concentrations were also detected at the base of trichomes, epidermal hairs of leaves, associated to O/N ligands, probably to the cell wall. This phenomenon was also observed on non-hyperaccumulators and is clearly not the major sink for Cd, but trichomes might play a role in the detoxification process. This study illustrates the suitability of synchrotron radiation based techniques to investigate metal distribution and speciation in plants.

Crystallographic Characterization of Extraterrestrial Materials by Energy-Scanning X-ray Diffraction

NASA Technical Reports Server (NTRS)

Hagiya, Kenji; Mikouchi, Takashi; Ohsumi, Kazumasa; Terada, Yasuko; Yagi, Naoto; Komatsu, Mutsumi; Yamaguchi, Shoki; Hirata, Arashi; Kurokawa, Ayaka; Zolensky, Michael E. (Principal Investigator)

2016-01-01

We have continued our long-term project using X-ray diffraction to characterize a wide range of extraterrestrial samples. The stationary sample method with polychromatic X-rays is advantageous because the irradiated area of the sample is always same and fixed, meaning that all diffraction spots occur from the same area of the sample, however, unit cell parameters cannot be directly obtained by this method though they are very important for identification of mineral and for determination of crystal structures. In order to obtain the cell parameters even in the case of the sample stationary method, we apply energy scanning of a micro-beam of monochromatic SR at SPring-8.

Atomic pair distribution function at the Brazilian Synchrotron Light Laboratory: application to the Pb 1–x La xZr 0.40Ti 0.60O 3 ferroelectric system

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

Saleta, M. E.; Eleotério, M.; Mesquita, A.

2017-07-29

This work reports the setting up of the X-ray diffraction and spectroscopy beamline at the Brazilian Synchrotron Light Laboratory for performing total scattering experiments to be analyzed by atomic pair distribution function (PDF) studies. The results of a PDF refinement for Al 2O 3 standard are presented and compared with data acquired at a beamline of the Advanced Photon Source, where it is common to perform this type of experiment. A preliminary characterization of the Pb 1–xLa xZr 0.40Ti 0.60O 3 ferroelectric system, withx= 0.11, 0.12 and 0.15, is also shown.

Plutonium-uranium mixed oxide characterization by coupling micro-X-ray diffraction and absorption investigations

NASA Astrophysics Data System (ADS)

Degueldre, C.; Martin, M.; Kuri, G.; Grolimund, D.; Borca, C.

2011-09-01

Plutonium-uranium mixed oxide (MOX) fuels are currently used in nuclear reactors. The potential differences of metal redox state and microstructural developments of the matrix before and after irradiation are commonly analysed by electron probe microanalysis. In this work the structure and next-neighbor atomic environments of Pu and U oxide features within unirradiated homogeneous MOX and irradiated (60 MW d kg -1) MOX samples was analysed by micro-X-ray fluorescence (μ-XRF), micro-X-ray diffraction (μ-XRD) and micro-X-ray absorption fine structure (μ-XAFS) spectroscopy. The grain properties, chemical bonding, valences and stoichiometry of Pu and U are determined from the experimental data gained for the unirradiated as well as for irradiated fuel material examined in the center of the fuel as well as in its peripheral zone (rim). The formation of sub-grains is observed as well as their development from the center to the rim (polygonization). In the irradiated sample Pu remains tetravalent (>95%) and no (<5%) Pu(V) or Pu(VI) can be detected while the fuel could undergo slight oxidation in the rim zone. Any slight potential plutonium oxidation is buffered by the uranium dioxide matrix while locally fuel cladding interaction could also affect the redox of the fuel.

Evaluation of laboratory powder X-ray micro-diffraction for applications in the fields of cultural heritage and forensic science.

PubMed

Svarcová, Silvie; Kocí, Eva; Bezdicka, Petr; Hradil, David; Hradilová, Janka

2010-09-01

The uniqueness and limited amounts of forensic samples and samples from objects of cultural heritage together with the complexity of their composition requires the application of a wide range of micro-analytical methods, which are non-destructive to the samples, because these must be preserved for potential late revision. Laboratory powder X-ray micro-diffraction (micro-XRD) is a very effective non-destructive technique for direct phase analysis of samples smaller than 1 mm containing crystal constituents. It compliments optical and electron microscopy with elemental micro-analysis, especially in cases of complicated mixtures containing phases with similar chemical composition. However, modification of X-ray diffraction to the micro-scale together with its application for very heterogeneous real samples leads to deviations from the standard procedure. Knowledge of both the limits and the phenomena which can arise during the analysis is crucial for the meaningful and proper application of the method. We evaluated basic limits of micro-XRD equipped with a mono-capillary with an exit diameter of 0.1 mm, for example the size of irradiated area, appropriate grain size, and detection limits allowing identification of given phases. We tested the reliability and accuracy of quantitative phase analysis based on micro-XRD data in comparison with conventional XRD (reflection and transmission), carrying out experiments with two-phase model mixtures simulating historic colour layers. Furthermore, we demonstrate the wide use of micro-XRD for investigation of various types of micro-samples (contact traces, powder traps, colour layers) and we show how to enhance data quality by proper choice of experiment geometry and conditions.

Investigation of high-energy ion-irradiated MA957 using synchrotron radiation under in-situ tension

DOE PAGES

Mo, Kun; Yun, Di; Miao, Yinbin; ...

2016-01-02

In this paper, an MA957 oxide dispersion-strengthened (ODS) alloy was irradiated with high-energy ions in the Argonne Tandem Linac Accelerator System. Fe ions at an energy of 84 MeV bombarded MA957 tensile specimens, creating a damage region similar to 7.5 μm in depth; the peak damage (similar to 40 dpa) was estimated to be at similar to 7 μm from the surface. Following the irradiation, in-situ high-energy X-ray diffraction measurements were performed at the Advanced Photon Source in order to study the dynamic deformation behavior of the specimens after ion irradiation damage. In-situ X-ray measurements taken during tensile testing ofmore » the ion-irradiated MA957 revealed a difference in loading behavior between the irradiated and un-irradiated regions of the specimen. At equivalent applied stresses, lower lattice strains were found in the radiation-damaged region than those in the un-irradiated region. This might be associated with a higher level of Type II stresses as a result of radiation hardening. The study has demonstrated the feasibility of combining high-energy ion radiation and high-energy synchrotron X-ray diffraction to study materials' radiation damage in a dynamic manner.« less

Sub-atomic resolution X-ray crystallography and neutron crystallography: promise, challenges and potential.

PubMed

Blakeley, Matthew P; Hasnain, Samar S; Antonyuk, Svetlana V

2015-07-01

The International Year of Crystallography saw the number of macromolecular structures deposited in the Protein Data Bank cross the 100000 mark, with more than 90000 of these provided by X-ray crystallography. The number of X-ray structures determined to sub-atomic resolution (i.e. ≤1 Å) has passed 600 and this is likely to continue to grow rapidly with diffraction-limited synchrotron radiation sources such as MAX-IV (Sweden) and Sirius (Brazil) under construction. A dozen X-ray structures have been deposited to ultra-high resolution (i.e. ≤0.7 Å), for which precise electron density can be exploited to obtain charge density and provide information on the bonding character of catalytic or electron transfer sites. Although the development of neutron macromolecular crystallography over the years has been far less pronounced, and its application much less widespread, the availability of new and improved instrumentation, combined with dedicated deuteration facilities, are beginning to transform the field. Of the 83 macromolecular structures deposited with neutron diffraction data, more than half (49/83, 59%) were released since 2010. Sub-mm(3) crystals are now regularly being used for data collection, structures have been determined to atomic resolution for a few small proteins, and much larger unit-cell systems (cell edges >100 Å) are being successfully studied. While some details relating to H-atom positions are tractable with X-ray crystallography at sub-atomic resolution, the mobility of certain H atoms precludes them from being located. In addition, highly polarized H atoms and protons (H(+)) remain invisible with X-rays. Moreover, the majority of X-ray structures are determined from cryo-cooled crystals at 100 K, and, although radiation damage can be strongly controlled, especially since the advent of shutterless fast detectors, and by using limited doses and crystal translation at micro-focus beams, radiation damage can still take place. Neutron crystallography therefore remains the only approach where diffraction data can be collected at room temperature without radiation damage issues and the only approach to locate mobile or highly polarized H atoms and protons. Here a review of the current status of sub-atomic X-ray and neutron macromolecular crystallography is given and future prospects for combined approaches are outlined. New results from two metalloproteins, copper nitrite reductase and cytochrome c', are also included, which illustrate the type of information that can be obtained from sub-atomic-resolution (∼0.8 Å) X-ray structures, while also highlighting the need for complementary neutron studies that can provide details of H atoms not provided by X-ray crystallography.

Projection x-ray topography system at 1-BM x-ray optics test beamline at the advanced photon source

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

Stoupin, Stanislav, E-mail: sstoupin@aps.anl.gov; Liu, Zunping; Trakhtenberg, Emil

2016-07-27

Projection X-ray topography of single crystals is a classic technique for the evaluation of intrinsic crystal quality of large crystals. In this technique a crystal sample and an area detector (e.g., X-ray film) collecting intensity of a chosen crystallographic reflection are translated simultaneously across an X-ray beam collimated in the diffraction scattering plane (e.g., [1, 2]). A bending magnet beamline of a third-generation synchrotron source delivering x-ray beam with a large horizontal divergence, and therefore, a large horizontal beam size at a crystal sample position offers an opportunity to obtain X-ray topographs of large crystalline samples (e.g., 6-inch wafers) inmore » just a few exposures. Here we report projection X-ray topography system implemented recently at 1-BM beamline of the Advanced Photon Source. A selected X-ray topograph of a 6-inch wafer of 4H-SiC illustrates capabilities and limitations of the technique.« less

[Application research of DEI technique based on synchrotron X-ray source in imaging rabbit eyeball in vitro].

PubMed

Yin, Hong-xia; Huang, Zhi-feng; Wang, Zhen-chang; Liu, Zhao-hui; Li, Yong; Zhu, Pei-ping

2010-03-23

To study the application of DEI technique in imaging the small structures of rabbit eyeball. DEI technique was used to image the eyeball of New Zealand white rabbit in vitro. The experiments were performed using beamline 4W1A at the topography station of Beijing Synchrotron Radiation Facility (BSRF). DEI image showed clearly the fine structures of the rabbit eyeball, such as the transparent cornea, the sclera, the ciliaris, and the ciliary body. DEI is a new X-ray imaging modality which achieves high contrast and spatial resolution. It also showed obvious effect of edge enhancement. DEI has good potential in observing the micro-structures of eyeballs and other small organs.

The photodegradation of cadmium yellow paints in Henri Matisse's Le Bonheur de vivre (1905-1906)

NASA Astrophysics Data System (ADS)

Mass, Jennifer L.; Opila, Robert; Buckley, Barbara; Cotte, Marine; Church, Jonathan; Mehta, Apurva

2013-04-01

Evidence for the alteration of the yellow paints in Henri Matisse's Le Bonheur de vivre (1905-1906, The Barnes Foundation) has been observed since the 1990s. The changes in this iconic work of Matisse's Fauvist period include lightening, darkening, and flaking of the yellow paints. Handheld X-ray fluorescence (XRF) and multispectral imaging surveys reveal that the degradation is confined to cadmium yellow (CdS) paints. The discoloration of cadmium yellow paints in Impressionist, Post-Impressionist and early modernist work from the 1880s through the 1920s has been ascribed to the photo-oxidative degradation of CdS. Preliminary investigations of the degraded yellow paints in this work involved Cd LIII-edge X-ray Absorption Near Edge Spectroscopy (XANES) at the Stanford Synchrotron Radiation Light Source (SSRL Menlo Park, California) and Scanning Electron Microscopy-energy dispersive X-ray analysis (SEM-EDS) at the Winterthur Museum Scientific Research and Analysis Laboratory. To determine if the visual changes in the paints did in fact indicate photo-oxidative degradation and if different chemistries could be observed for the lightened versus darkened regions, synchrotron radiation-micro Fourier Transform InfraRed (SR-μFTIR) spectroscopy, X-ray Fluorescence (SR-μXRF) mapping and micro X-ray Absorption Near Edge Spectroscopy (μXANES) mapping at the Cd LIII-edge of the altered paint cross-sections were carried out at the European synchrotron radiation facility (ESRF, Grenoble, France) beamline ID-21. The goal is to elucidate the discoloration mechanisms observed in the paint using elemental and speciation mapping. The μXANES mapping and SR-FTIR imaging showed a substantial enrichment of CdCO3 in the off-white surface crust of the faded/discolored CdS paint. This suggests that the CdCO3 is present as an insoluble photodegradation product rather than solely a paint filler or starting reagent. Additionally, oxalates and sulfates were found to be concentrated at the alteration surface.

Combined operando X-ray diffraction-electrochemical impedance spectroscopy detecting solid solution reactions of LiFePO4 in batteries.

PubMed

Hess, Michael; Sasaki, Tsuyoshi; Villevieille, Claire; Novák, Petr

2015-09-08

Lithium-ion batteries are widely used for portable applications today; however, often suffer from limited recharge rates. One reason for such limitation can be a reduced active surface area during phase separation. Here we report a technique combining high-resolution operando synchrotron X-ray diffraction coupled with electrochemical impedance spectroscopy to directly track non-equilibrium intermediate phases in lithium-ion battery materials. LiFePO4, for example, is known to undergo phase separation when cycled under low-current-density conditions. However, operando X-ray diffraction under ultra-high-rate alternating current and direct current excitation reveal a continuous but current-dependent, solid solution reaction between LiFePO4 and FePO4 which is consistent with previous experiments and calculations. In addition, the formation of a preferred phase with a composition similar to the eutectoid composition, Li0.625FePO4, is evident. Even at a low rate of 0.1C, ∼20% of the X-ray diffractogram can be attributed to non-equilibrium phases, which changes our understanding of the intercalation dynamics in LiFePO4.

Beamline P02.1 at PETRA III for high-resolution and high-energy powder diffraction

PubMed Central

Dippel, Ann-Christin; Liermann, Hanns-Peter; Delitz, Jan Torben; Walter, Peter; Schulte-Schrepping, Horst; Seeck, Oliver H.; Franz, Hermann

2015-01-01

Powder X-ray diffraction techniques largely benefit from the superior beam quality provided by high-brilliance synchrotron light sources in terms of photon flux and angular resolution. The High Resolution Powder Diffraction Beamline P02.1 at the storage ring PETRA III (DESY, Hamburg, Germany) combines these strengths with the power of high-energy X-rays for materials research. The beamline is operated at a fixed photon energy of 60 keV (0.207 Å wavelength). A high-resolution monochromator generates the highly collimated X-ray beam of narrow energy bandwidth. Classic crystal structure determination in reciprocal space at standard and non-ambient conditions are an essential part of the scientific scope as well as total scattering analysis using the real space information of the pair distribution function. Both methods are complemented by in situ capabilities with time-resolution in the sub-second regime owing to the high beam intensity and the advanced detector technology for high-energy X-rays. P02.1’s efficiency in solving chemical and crystallographic problems is illustrated by presenting key experiments that were carried out within these fields during the early stage of beamline operation. PMID:25931084

Mapping the metal uptake in plants from Jasper Ridge Biological Preserve using synchrotron micro-focused X-ray fluorescence spectroscopy

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

Lo, Allison

2015-08-20

Serpentine soil originates in the Earth’s mantle and contains high concentrations of potentially toxic transition metals. Although serpentine soil limits plant growth, endemic and adapted plants at Jasper Ridge Biological Preserve, located behind SLAC National Accelerator Laboratory, can tolerate these conditions. Serpentine soil and seeds belonging to native California and invasive plants were collected at Jasper Ridge. The seeds were grown hydroponically and on serpentine and potting soil to examine the uptake and distribution of ions in the roots and shoots using synchrotron micro-focused X-ray fluorescence spectroscopy. The results were used to determine differences between serpentine-tolerant plants. Rye grown onmore » potting soil was enriched in Ni, Fe, Mn, and Cr compared to purple needlegrass grown on serpentine soil. Serpentine vegetation equally suppressed the uptake of Mn, Ni, and Fe in the roots and shoots. The uptake of Ca and Mg affected the uptake of other elements such as K, S, and P.« less

Aging effect on Zn retention on a calcareous soil: column experiments and synchrotron X-ray micro-spectroscopic investigation.

PubMed

Sayen, Stéphanie; Guillon, Emmanuel

2014-07-15

In this study, a combination of column experiments and micro-analytical techniques exploiting synchrotron generated X-rays was used to assess the effect of aging time on Zn retention and mobility in the specific case of calcareous soils (high pH value, ≈ 8). The samples were subjected to aging for 2, 6, 17, and 63 days. Freshly added Zn mainly existed as an exchangeable form, and this metal fraction decreased over time due to Zn redistribution to stronger binding sites. Thus, after aging for 63 days, 45% of Zn is remobilized from exchangeable sites to stronger binding sites. μ-XRF maps were used to find correlations among elements in the sample, and μ-XANES spectra were recorded to precise Zn speciation. These analyses evidenced an increasing partitioning of Zn from organic matter to iron oxy(hydr)oxides over time. The occurrence of hydrozincite is evidenced in all samples. Copyright © 2014 Elsevier B.V. All rights reserved.

Surface-treated self-standing curved crystals as high-efficiency elements for X- and γ-ray optics: theory and experiment.

PubMed

Bonnini, Elisa; Buffagni, Elisa; Zappettini, Andrea; Doyle, Stephen; Ferrari, Claudio

2015-06-01

The efficiency of a Laue lens for X- and γ-ray focusing in the energy range 60-600 keV is closely linked to the diffraction efficiency of the single crystals composing the lens. A powerful focusing system is crucial for applications like medical imaging and X-ray astronomy where wide beams must be focused. Mosaic crystals with a high density, such as Cu or Au, and bent crystals with curved diffracting planes (CDPs) are considered for the realization of a focusing system for γ-rays, owing to their high diffraction efficiency in a predetermined angular range. In this work, a comparison of the efficiency of CDP crystals and Cu and Au mosaic crystals was performed on the basis of the theory of X-ray diffraction. Si, GaAs and Ge CDP crystals with optimized thicknesses and moderate radii of curvature of several tens of metres demonstrate comparable or superior performance with respect to the higher atomic number mosaic crystals generally used. In order to increase the efficiency of the lens further, a stack of several CDP crystals is proposed as an optical element. CDP crystals were obtained by a surface-damage method, and a stack of two surface-damaged bent Si crystals was prepared and tested. Rocking curves of the stack were performed with synchrotron radiation at 19 keV to check the lattice alignment: they exhibited only one diffraction peak.

Recent advances in continuum plasticity: phenomenological modeling and experimentation using X-ray diffraction

NASA Astrophysics Data System (ADS)

Edmiston, John Kearney

This work explores the field of continuum plasticity from two fronts. On the theory side, we establish a complete specification of a phenomenological theory of plasticity for single crystals. The model serves as an alternative to the popular crystal plasticity formulation. Such a model has been previously proposed in the literature; the new contribution made here is the constitutive framework and resulting simulations. We calibrate the model to available data and use a simple numerical method to explore resulting predictions in plane strain boundary value problems. Results show promise for further investigation of the plasticity model. Conveniently, this theory comes with a corresponding experimental tool in X-ray diffraction. Recent advances in hardware technology at synchrotron sources have led to an increased use of the technique for studies of plasticity in the bulk of materials. The method has been successful in qualitative observations of material behavior, but its use in quantitative studies seeking to extract material properties is open for investigation. Therefore in the second component of the thesis several contributions are made to synchrotron X-ray diffraction experiments, in terms of method development as well as the quantitative reporting of constitutive parameters. In the area of method development, analytical tools are developed to determine the available precision of this type of experiment—a crucial aspect to determine if the method is to be used for quantitative studies. We also extract kinematic information relating to intragranular inhomogeneity which is not accessible with traditional methods of data analysis. In the area of constitutive parameter identification, we use the method to extract parameters corresponding to the proposed formulation of plasticity for a titanium alloy (HCP) which is continuously sampled by X-ray diffraction during uniaxial extension. These results and the lessons learned from the efforts constitute early reporting of the quantitative profitability of undertaking such a line of experimentation for the study of plastic deformation processes.

Direct synchrotron x-ray measurements of local strain fields in elastically and plastically bent metallic glasses

DOE PAGES

Wu, Yuan; Stoica, Alexandru Dan; Ren, Yang; ...

2015-09-03

In situ high-energy synchrotron X-ray diffraction was conducted on elastically and plastically bent bulk metallic glass (BMG) thin plates, from which distinct local elastic strain fields were mapped spatially. These directly measured residual strain fields can be nicely interpreted by our stress analysis, and also validate a previously proposed indirect residual-stress-measurement method by relating nanoindentation hardness to residual stresses. Local shear strain variations on the cross sections of these thin plates were found in the plastically bent BMG, which however cannot be determined from the indirect indentation method. As a result, this study has important implications in designing and manipulatingmore » internal strain fields in BMGs for the purpose of ductility enhancement.« less

X-ray analysis of residual stress gradients in TiN coatings by a Laplace space approach and cross-sectional nanodiffraction: a critical comparison.

PubMed

Stefenelli, Mario; Todt, Juraj; Riedl, Angelika; Ecker, Werner; Müller, Thomas; Daniel, Rostislav; Burghammer, Manfred; Keckes, Jozef

2013-10-01

Novel scanning synchrotron cross-sectional nanobeam and conventional laboratory as well as synchrotron Laplace X-ray diffraction methods are used to characterize residual stresses in exemplary 11.5 µm-thick TiN coatings. Both real and Laplace space approaches reveal a homogeneous tensile stress state and a very pronounced compressive stress gradient in as-deposited and blasted coatings, respectively. The unique capabilities of the cross-sectional approach operating with a beam size of 100 nm in diameter allow the analysis of stress variation with sub-micrometre resolution at arbitrary depths and the correlation of the stress evolution with the local coating microstructure. Finally, advantages and disadvantages of both approaches are extensively discussed.

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).

The structural and magnetic phase transitions in a ``parent'' Fe pnictide compound

NASA Astrophysics Data System (ADS)

Ni, Ni; Allred, Jared; Cao, Huibo; Tian, Wei; Liu, Lian; Cho, Kyuil; Krogstad, Matthew; Ma, Jie; Taddei, Keith; Tanatar, Makariy; Prozorov, Ruslan; Matsuda, Masaaki; Rosenkranz, Stephan; Uemura, Yasutomo; Jiang, Shan

2015-03-01

We will present transport, thermodynamic, synchrotron X-ray, neutron diffraction, μSR, ARPES and polarized optical image measurements on the ``parent'' compound of the 112 high Tc superconducting Fe pnictide family. Structural and magnetic phase transitions are revealed. Detailed magnetic structure was solved by single crystal neutron diffraction. We will discuss the similarity and difference of these transitions comparing to the parent compounds of other Fe pnictide superconductors.

Comparison of a CCD and an APS for soft X-ray diffraction

NASA Astrophysics Data System (ADS)

Stewart, Graeme; Bates, R.; Blue, A.; Clark, A.; Dhesi, S. S.; Maneuski, D.; Marchal, J.; Steadman, P.; Tartoni, N.; Turchetta, R.

2011-12-01

We compare a new CMOS Active Pixel Sensor (APS) to a Princeton Instruments PIXIS-XO: 2048B Charge Coupled Device (CCD) with soft X-rays tested in a synchrotron beam line at the Diamond Light Source (DLS). Despite CCDs being established in the field of scientific imaging, APS are an innovative technology that offers advantages over CCDs. These include faster readout, higher operational temperature, in-pixel electronics for advanced image processing and reduced manufacturing cost. The APS employed was the Vanilla sensor designed by the MI3 collaboration and funded by an RCUK Basic technology grant. This sensor has 520 x 520 square pixels, of size 25 μm on each side. The sensor can operate at a full frame readout of up to 20 Hz. The sensor had been back-thinned, to the epitaxial layer. This was the first time that a back-thinned APS had been demonstrated at a beam line at DLS. In the synchrotron experiment soft X-rays with an energy of approximately 708 eV were used to produce a diffraction pattern from a permalloy sample. The pattern was imaged at a range of integration times with both sensors. The CCD had to be operated at a temperature of -55°C whereas the Vanilla was operated over a temperature range from 20°C to -10°C. We show that the APS detector can operate with frame rates up to two hundred times faster than the CCD, without excessive degradation of image quality. The signal to noise of the APS is shown to be the same as that of the CCD at identical integration times and the response is shown to be linear, with no charge blooming effects. The experiment has allowed a direct comparison of back thinned APS and CCDs in a real soft x-ray synchrotron experiment.

Industry-relevant magnetron sputtering and cathodic arc ultra-high vacuum deposition system for in situ x-ray diffraction studies of thin film growth using high energy synchrotron radiation.

PubMed

Schroeder, J L; Thomson, W; Howard, B; Schell, N; Näslund, L-Å; Rogström, L; Johansson-Jõesaar, M P; Ghafoor, N; Odén, M; Nothnagel, E; Shepard, A; Greer, J; Birch, J

2015-09-01

We present an industry-relevant, large-scale, ultra-high vacuum (UHV) magnetron sputtering and cathodic arc deposition system purposefully designed for time-resolved in situ thin film deposition/annealing studies using high-energy (>50 keV), high photon flux (>10(12) ph/s) synchrotron radiation. The high photon flux, combined with a fast-acquisition-time (<1 s) two-dimensional (2D) detector, permits time-resolved in situ structural analysis of thin film formation processes. The high-energy synchrotron-radiation based x-rays result in small scattering angles (<11°), allowing large areas of reciprocal space to be imaged with a 2D detector. The system has been designed for use on the 1-tonne, ultra-high load, high-resolution hexapod at the P07 High Energy Materials Science beamline at PETRA III at the Deutsches Elektronen-Synchrotron in Hamburg, Germany. The deposition system includes standard features of a typical UHV deposition system plus a range of special features suited for synchrotron radiation studies and industry-relevant processes. We openly encourage the materials research community to contact us for collaborative opportunities using this unique and versatile scientific instrument.

Synchrotron X-Ray Diffraction Study of Structure and Growth of Adsorbed Layers

NASA Astrophysics Data System (ADS)

Dai, Pengcheng

Synchrotron x-ray diffraction and scanning-tunneling -microscopy (STM) experiments reveal a new commensurate monolayer structure of 10CB (decylcyanobiphenyl) molecules adsorbed on the (0001) graphite surface. Our results are consistent with two generic structures for nCB monolayers on surfaces of hexagonal symmetry. The monolayer d spacing of the new phase inferred by STM is 10% layer than that obtained by x-ray diffraction on the same sample. We suggest that part of this discrepancy results from a systematic error introduced in calibration of the STM length scale against the graphite substrate. For multilayer nCB films, we find that a polycrystalline structure is formed and most of the adsorbed molecules are aligned with their long axis perpendicular to the graphite surface. Synchrotron x-ray scattering has been used to investigate the structure and growth of xenon physisorbed on the Ag(111) surface using a specially designed ultra -high vacuum (UHV) chamber. For growth under quasi-equilibrium conditions, the bulk Xe-Xe spacing is reached at monolayer completion and solid films of thickness >= 220 A are observed in which an 'ABC' stacking sequence predominates. Under kinetic growth conditions, intensity oscillations at the Xe anti-Bragg position of the specular rod are observed as a function of time, indicating layer -by-layer growth. Analysis of the specular reflectivity at different coverages yields the fractional layer occupancies and the spacing between the Ag(111) surface and first Xe layer. We have conducted a series of low-energy electron diffraction (LEED) 'kinetic isotherm' experiments on both xenon and hexane rm(C_6H_{14 }) films adsorbed on the Ag(111) surface. Our preliminary results show that under the pressure and temperature range accessible to the experiments, all of the Xe kinetic isotherms fall on a universal curve which is concave upward. However, the hexane kinetic isotherms have a qualitatively different shape (S-like) at the higher temperatures while being similar to Xe at low temperatures. From these experiments, we determine that the growth of xenon from submonolayer to 0.9 monolayer is 'zero-order'. However, the growth of hexane is more complicated. It follows the 'first-order' at low temperatures, and changes to S-like shape at high temperatures which we do not yet understand.

Unusual thermal expansion of Sr{sub 2}IrO{sub 4}: A variable temperature synchrotron X-ray diffraction study

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

Ranjbar, Ben; Kennedy, Brendan J.

The structure of Sr{sub 2}IrO{sub 4} has been studied between 20 and 1273 K using synchrotron X-ray diffraction. Sr{sub 2}IrO{sub 4} undergoes an apparently continuous transition from I4{sub 1}/acd to I4/mmm near 1123 K. The cooperative tilting of the corner sharing IrO{sub 6} octahedra in I4{sub 1}/acd results in highly anisotropic and unusual thermal expansion behavior with negative thermal expansion along the c-axis. - Graphical abstract: The progressive reduction in the magnitude of the tilting of the corner sharing IrO{sub 6} octahedra in Sr{sub 2}IrO{sub 4} results in negative thermal expansion along the c-axis before undergoing an apparently continuous transitionmore » from I4{sub 1}/acd to I4/mmm near 1123 K. - Highlights: • Thermal expansion of Sr{sub 2}IrO{sub 4} was studied using Synchrotron-XRD. • Unusual negative thermal expansion along c-axis observed. • I4{sub 1}/acd→I4/mmm phase transition detected near 1120 K. • Tilting of the corner sharing IrO{sub 6} octahedra related to the observed NTE.« less

In search of the elusive IrB{sub 2}: Can mechanochemistry help?

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

Xie, Zhilin; Blair, Richard G.; Department of Physics, University of Central Florida, Orlando, FL 32816

The previously unknown hexagonal ReB{sub 2}-type IrB{sub 2} diboride and orthorhombic IrB monoboride phases were produced by mechanochemical syntheses. High energy ball milling of elemental Ir and B powder for 30 h, followed by annealing of the powder at 1050 °C for 48 h, resulted in the formation of the desired phases. Both traditional laboratory and high resolution synchrotron X-ray diffraction (XRD) analyses were used for phase identification of the synthesized powder. In addition to XRD, scanning electron microscopy and transmission electron microscopy were employed to further characterize the microstructure of the phases produced. - Graphical abstract: ReB{sub 2}-type IrB{submore » 2} and a new IrB have been successfully synthesized for the first time using mechanochemical method. Crystal structures of IrB{sub 2} and IrB were studied by synchrotron X-ray diffraction. Microstructures of the new phases were characterized by SEM and TEM. - Highlights: • ReB{sub 2}-type IrB{sub 2} and a new IrB have been synthesized by mechanochemical method. • Crystal structures of IrB{sub 2} and IrB were studied by synchrotron XRD. • Microstructures of the new phases were characterized by SEM and TEM.« less

Shining a light on Jarosite: formation, alteration and stability studies using in situ experimental synchrotron and neutron techniques.

NASA Astrophysics Data System (ADS)

Brand, H. E. A.; Scarlett, N. V. Y.; Wilson, S. A.; Frierdich, A. J.; Grey, I. E.

2016-12-01

Jarosites and related minerals are critical to a range of mineral processing and research applications. They are used in the removal of iron species from smelting processes; they occur in metal bioleaching systems, and they are present in acid mine drainage environments. There has been a recent resurgence in interest in jarosites since their detection on Mars. In this context, the presence of jarosite has been recognised as a likely indicator of liquid water at the surface of Mars in the past & it is thought that their study will provide insight into the environmental history of Mars. Acid sulfate soils cover large areas of the Australian coastline and are likely to be a major constituent of the Martian environment. The oxidation of acid sulfate soils, coupled with potential release of heavy metals and acidic groundwaters, can have serious consequences for fragile ecosystems. Understanding these sediments will provide insight into the biogeochemical processes that affect the lifetimes of transient mineral species on Earth, and may be used to better understand soil acidification, contaminant mobility at sites affected by acid and metalliferous drainage, and even constrain past weathering and putative biosignatures on Mars. Knowledge of the behaviour of jarosite minerals under the actual conditions that they are found in is crucial to understanding their potential environmental impacts on both Earth and Mars. To this end, we are engaged in a program to study the formation, stability and alteration of natural and synthetic jarosite minerals using a complementary suite of in situ synchrotron and neutron techniques. There are 3 sections to this work that will introduce the experimental techniques and sample environments that make these measurements possible: Studying the nucleation and growth of jarosites under laboratory conditions. The experimentation consisted of time-resolved synchrotron small angle X-ray scattering and X-ray diffraction. Studying the stability of natural & synthetic jarosites with temperature and pressure using synchrotron and neutron diffraction. Parallel neutron and X-ray imaging at OPAL and the Australian Synchrotron, combined with synchrotron pseudo-microdiffraction to map the mineralogy and structural relationships within naturally occurring jarosite nodules.

Development of the GEM-TPC X-ray Polarimeter with the Scalable Readout System

NASA Astrophysics Data System (ADS)

Kitaguchi, Takao; Hayato, Asami; Iwakiri, Wataru; Takeuchi, Yoko; Kubota, Megu; Nishida, Kazuki; Enoto, Teruaki; Tamagawa, Toru

2018-02-01

We have developed a gaseous Time Projection Chamber (TPC) containing a single-layered foil of a gas electron multiplier (GEM) to open up a new window on cosmic X-ray polarimetry in the 2-10 keV band. The micro-pattern TPC polarimeter in combination with the Scalable Readout System produced by the RD51 collaboration has been built as an engineering model to optimize detector parameters and improve polarimeter sensitivity. The polarimeter was characterized with unpolarized X-rays from an X-ray generator in a laboratory and polarized X-rays on the BL32B2 beamline at the SPring-8 synchrotron radiation facility. Preliminary results show that the polarimeter has a comparable modulation factor to a prototype of the flight one.

Cesium Speciation in Dust from Municipal Solid Waste and Sewage Sludge Incineration by Synchrotron Radiation Micro-X-ray Analysis.

PubMed

Shiota, Kenji; Takaoka, Masaki; Fujimori, Takashi; Oshita, Kazuyuki; Terada, Yasuko

2015-11-17

The chemical behavior of Cs in waste incineration processes is important to consider when disposing of radionuclide-contaminated waste from the Fukushima Daiichi nuclear power plant accident in Japan. To determine the speciation of Cs, we attempted the direct speciation of trace amounts of stable Cs in the dust from municipal solid waste incineration (MSWI) and sewage sludge incineration (SSI) by micro-X-ray fluorescence (μ-XRF) and micro-X-ray absorption fine structure (μ-XAFS) at the SPring-8 facility. The μ-XRF results revealed that locally produced Cs was present in MSWI and SSI dust within the cluster size range of 2-10 μm. The μ-XAFS analysis confirmed that the speciation of Cs in MSWI dust was similar to that of CsCl, while in SSI dusts it was similar to pollucite. The solubility of Cs was considered to be influenced by the exact Cs species present in incineration residue.

Crystallization and preliminary X-ray diffraction analysis of recombinant phosphoribosylpyrophosphate synthetase from the Thermophilic thermus thermophilus strain HB27

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

Abramchik, Yu. A.; Timofeev, V. I., E-mail: tostars@mail.ru; Muravieva, T. I.

2017-01-15

Phosphoribosylpyrophosphate synthetases (PRPP synthetases) are among the key enzymes essential for vital functions of organisms and are involved in the biosynthesis of purine and pyrimidine nucleotides, coenzymes, and the amino acids histidine and tryptophan. These enzymes are used in biotechnology for the combined chemoenzymatic synthesis of natural nucleotide analogs. Recombinant phosphoribosylpyrophosphate synthetase I from the thermophilic strain HB27 of the bacterium Thermus thermophilus (T. th HB27) has high thermal stability and shows maximum activity at 75°Ð¡, due to which this enzyme holds promise for biotechnological applications. In order to grow crystals and study them by X-ray crystallography, an enzyme sample,more » which was produced using a highly efficient producer strain, was purified by affinity and gel-filtration chromatography. The screening of crystallization conditions was performed by the vapor-diffusion technique. The crystals of the enzyme suitable for X-ray diffraction were grown by the counter-diffusion method through a gel layer. These crystals were used to collect the X-ray diffraction data set at the SPring-8 synchrotron radiation facility (Japan) to 3-Å resolution. The crystals belong to sp. gr. P2{sub 1} and have the following unitcell parameters: a = 107.7 Å, b = 112.6 Å, c = 110.2 Å, α = γ = 90°, β = 116.6°. The X-ray diffraction data set is suitable for determining the three-dimensional structure of the enzyme at 3.0-Å resolution.« less