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.

Multifit / Polydefix : a framework for the analysis of polycrystal deformation using X-rays

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

Merkel, Sébastien; Hilairet, Nadège

2015-06-27

Multifit/Polydefixis an open source IDL software package for the efficient processing of diffraction data obtained in deformation apparatuses at synchrotron beamlines.Multifitallows users to decompose two-dimensional diffraction images into azimuthal slices, fit peak positions, shapes and intensities, and propagate the results to other azimuths and images.Polydefixis for analysis of deformation experiments. Starting from output files created inMultifitor other packages, it will extract elastic lattice strains, evaluate sample pressure and differential stress, and prepare input files for further texture analysis. TheMultifit/Polydefixpackage is designed to make the tedious data analysis of synchrotron-based plasticity, rheology or other time-dependent experiments very straightforward and accessible tomore » a wider community.« less

Bragg coherent diffraction imaging and metrics for radiation damage in protein micro-crystallography.

PubMed

Coughlan, H D; Darmanin, C; Kirkwood, H J; Phillips, N W; Hoxley, D; Clark, J N; Vine, D J; Hofmann, F; Harder, R J; Maxey, E; Abbey, B

2017-01-01

The proliferation of extremely intense synchrotron sources has enabled ever higher-resolution structures to be obtained using data collected from smaller and often more imperfect biological crystals (Helliwell, 1984). Synchrotron beamlines now exist that are capable of measuring data from single crystals that are just a few micrometres in size. This provides renewed motivation to study and understand the radiation damage behaviour of small protein crystals. Reciprocal-space mapping and Bragg coherent diffractive imaging experiments have been performed on cryo-cooled microcrystals of hen egg-white lysozyme as they undergo radiation damage. Several well established metrics, such as intensity-loss and lattice expansion, are applied to the diffraction data and the results are compared with several new metrics that can be extracted from the coherent imaging experiments. Individually some of these metrics are inconclusive. However, combining metrics, the results suggest that radiation damage behaviour in protein micro-crystals differs from that of larger protein crystals and may allow them to continue to diffract for longer. A possible mechanism to account for these observations is proposed.

Bragg coherent diffraction imaging and metrics for radiation damage in protein micro-crystallography

DOE PAGES

Coughlan, H. D.; Darmanin, C.; Kirkwood, H. J.; ...

2017-01-01

The proliferation of extremely intense synchrotron sources has enabled ever higher-resolution structures to be obtained using data collected from smaller and often more imperfect biological crystals. Synchrotron beamlines now exist that are capable of measuring data from single crystals that are just a few micrometres in size. This provides renewed motivation to study and understand the radiation damage behaviour of small protein crystals. Reciprocal-space mapping and Bragg coherent diffractive imaging experiments have been performed on cryo-cooled microcrystals of hen egg-white lysozyme as they undergo radiation damage. Several well established metrics, such as intensity-loss and lattice expansion, are applied to themore » diffraction data and the results are compared with several new metrics that can be extracted from the coherent imaging experiments. Individually some of these metrics are inconclusive. However, combining metrics, the results suggest that radiation damage behaviour in protein micro-crystals differs from that of larger protein crystals and may allow them to continue to diffract for longer. As a result, a possible mechanism to account for these observations is proposed.« less

Bragg coherent diffraction imaging and metrics for radiation damage in protein micro-crystallography

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

Coughlan, H. D.; Darmanin, C.; Kirkwood, H. J.

The proliferation of extremely intense synchrotron sources has enabled ever higher-resolution structures to be obtained using data collected from smaller and often more imperfect biological crystals. Synchrotron beamlines now exist that are capable of measuring data from single crystals that are just a few micrometres in size. This provides renewed motivation to study and understand the radiation damage behaviour of small protein crystals. Reciprocal-space mapping and Bragg coherent diffractive imaging experiments have been performed on cryo-cooled microcrystals of hen egg-white lysozyme as they undergo radiation damage. Several well established metrics, such as intensity-loss and lattice expansion, are applied to themore » diffraction data and the results are compared with several new metrics that can be extracted from the coherent imaging experiments. Individually some of these metrics are inconclusive. However, combining metrics, the results suggest that radiation damage behaviour in protein micro-crystals differs from that of larger protein crystals and may allow them to continue to diffract for longer. As a result, a possible mechanism to account for these observations is proposed.« less

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

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

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.

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

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

NASA Technical Reports Server (NTRS)

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

2004-01-01

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

Ecological and agricultural applications of synchrotron IR microscopy

NASA Astrophysics Data System (ADS)

Raab, T. K.; Vogel, J. P.

2004-10-01

The diffraction-limited spot size of synchrotron-based IR microscopes provides cell-specific, spectrochemical imaging of cleared leaf, stem and root tissues of the model genetic organism Arabidopsis thaliana, and mutant plants created either by T-DNA insertional inactivation or chemical mutagenesis. Spectra in the wavelength region from 6 to 12 μm provide chemical and physical information on the cell wall polysaccharides of mutants lacking particular biosynthetic enzymes ("Cellulose synthase-like" genes). In parallel experiments, synchrotron IR microscopy delineates the role of Arabidopsis cell wall enzymes as susceptibility factors to the fungus Erysiphe cichoracearum, a causative agent of powdery mildew disease. Three genes, pmr4, pmr5, and pmr6 have been characterized by these methods, and biochemical relations between two of the genes suggested by IR spectroscopy and multivariate statistical techniques could not have been inferred through classical molecular biology. In ecological experiments, live plants can also be imaged in small microcosms with mid-IR transmitting ZnSe windows. Small exudate molecules may be spatially mapped in relation to root architecture at diffraction-limited resolution, and the effect of microbial symbioses on the quantity and quality of exudates inferred. Synchrotron IR microscopy provides a useful adjunct to molecular biological methods and underground observatories in the ongoing assessment of the role of root-soil-microbe communication.

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

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.

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.

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.

Ferroelectrics under the Synchrotron Light: A Review.

PubMed

Fuentes-Cobas, Luis E; Montero-Cabrera, María E; Pardo, Lorena; Fuentes-Montero, Luis

2015-12-30

Currently, an intensive search for high-performance lead-free ferroelectric materials is taking place. ABO₃ perovskites (A = Ba, Bi, Ca, K and Na; B = Fe, Nb, Ti, and Zr) appear as promising candidates. Understanding the structure-function relationship is mandatory, and, in this field, the roles of long- and short-range crystal orders and interactions are decisive. In this review, recent advances in the global and local characterization of ferroelectric materials by synchrotron light diffraction, scattering and absorption are analyzed. Single- and poly-crystal synchrotron diffraction studies allow high-resolution investigations regarding the long-range average position of ions and subtle global symmetry break-downs. Ferroelectric materials, under the action of electric fields, undergo crystal symmetry, crystallite/domain orientation distribution and strain condition transformations. Methodological aspects of monitoring these processes are discussed. Two-dimensional diffraction clarify larger scale ordering: polycrystal texture is measured from the intensities distribution along the Debye rings. Local order is investigated by diffuse scattering (DS) and X-ray absorption fine structure (XAFS) experiments. DS provides information about thermal, chemical and displacive low-dimensional disorders. XAFS investigation of ferroelectrics reveals local B-cation off-centering and oxidation state. This technique has the advantage of being element-selective. Representative reports of the mentioned studies are described.

Interpretation of small-angle diffraction experiments on opal-like photonic crystals

NASA Astrophysics Data System (ADS)

Marlow, F.; Muldarisnur, M.; Sharifi, P.; Zabel, H.

2011-08-01

Comprehensive structural information on artificial opals involving the deviations from the strongly dominating face-centered cubic structure is still missing. Recent structure investigations with neutrons and synchrotron sources have shown a high degree of order but also a number of unexpected scattering features. Here, we point out that the exclusion of the allowed 002-type diffraction peaks by a small atomic form factor is not obvious and that surface scattering has to be included as a possible source for the diffraction peaks. Our neutron diffraction data indicate that surface scattering is the main reason for the smallest-angle peaks in the diffraction patterns.

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.

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.

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.

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

MxCuBE: a synchrotron beamline control environment customized for macromolecular crystallography experiments

PubMed Central

Gabadinho, José; Beteva, Antonia; Guijarro, Matias; Rey-Bakaikoa, Vicente; Spruce, Darren; Bowler, Matthew W.; Brockhauser, Sandor; Flot, David; Gordon, Elspeth J.; Hall, David R.; Lavault, Bernard; McCarthy, Andrew A.; McCarthy, Joanne; Mitchell, Edward; Monaco, Stéphanie; Mueller-Dieckmann, Christoph; Nurizzo, Didier; Ravelli, Raimond B. G.; Thibault, Xavier; Walsh, Martin A.; Leonard, Gordon A.; McSweeney, Sean M.

2010-01-01

The design and features of a beamline control software system for macromolecular crystallography (MX) experiments developed at the European Synchrotron Radiation Facility (ESRF) are described. This system, MxCuBE, allows users to easily and simply interact with beamline hardware components and provides automated routines for common tasks in the operation of a synchrotron beamline dedicated to experiments in MX. Additional functionality is provided through intuitive interfaces that enable the assessment of the diffraction characteristics of samples, experiment planning, automatic data collection and the on-line collection and analysis of X-ray emission spectra. The software can be run in a tandem client-server mode that allows for remote control and relevant experimental parameters and results are automatically logged in a relational database, ISPyB. MxCuBE is modular, flexible and extensible and is currently deployed on eight macromolecular crystallography beamlines at the ESRF. Additionally, the software is installed at MAX-lab beamline I911-3 and at BESSY beamline BL14.1. PMID:20724792

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.

In-situ Diffraction Study of Magnetite at Simultaneous High Pressure and High Temperature Using Synchrotron Radiation

NASA Astrophysics Data System (ADS)

Wang, L.; Zhang, J.; Wang, S.; Chen, H.; Zhao, Y.

2014-12-01

Magnetite intertwined with the evolution of human civilizations, and remains so today. It is technologically and scientifically important by virtue of its unique magnetic and electrical properties. Magnetite is a common mineral found in a variety of geologic environments, and plays an important role in deciphering the oxygen evolution in the Earth's atmosphere and its deep interiors. The latter application asks for the knowledge of the thermal and elastic properties of magnetite at high pressures and temperatures, which is currently not available in literature. We have carried out a few in-situ diffraction experiments on magnetite using white synchrotron radiation at beamline X17B2 of National Synchrotron Light Source (NSLS). A DIA module in an 1100-ton press and WC anvils were employed for compression, and diffraction spectra were collected at simultaneous high pressures (P) and temperatures (T) (up to 9 GPa and 900 oC). Mixture of amorphous boron and epoxy resin was used as pressure medium, and NaCl as pressure marker. Temperature was recorded by W-Re thermocouples. Commercially purchased magnetite powder and a mixture of the said powder and NaCl (1:1) were used as starting material in separate experiments. Preliminary data analyses have yielded following observations: (1) Charge disordering seen at ambient pressure remains active in current experiments, especially at lower pressures (< 6 GPa); (2) Though at each condition potentially complicated by charge disordering process, isothermal compression curves remains simple and reproducible; (3) During cooling, the reversibility and degree of cation disordering depend on the starting material and/or experimental P-T path; and (4) cation disordering notably reduces the apparent bulk moduli of magnetite.

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.

Experimental measurement of lattice strain pole figures using synchrotron x rays

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

Miller, M.P.; Bernier, J.V.; Park, J.-S.

This article describes a system for mechanically loading test specimens in situ for the determination of lattice strain pole figures and their evolution in multiphase alloys via powder diffraction. The data from these experiments provide insight into the three-dimensional mechanical response of a polycrystalline aggregate and represent an extremely powerful material model validation tool. Relatively thin (0.5 mm) iron/copper specimens were axially strained using a mechanical loading frame beyond the macroscopic yield strength of the material. The loading was halted at multiple points during the deformation to conduct a diffraction experiment using a 0.5x0.5 mm{sup 2} monochromatic (50 keV) xmore » ray beam. Entire Debye rings of data were collected for multiple lattice planes ({l_brace}hkl{r_brace}'s) in both copper and iron using an online image plate detector. Strain pole figures were constructed by rotating the loading frame about the specimen transverse direction. Ideal powder patterns were superimposed on each image for the purpose of geometric correction. The chosen reference material was cerium (IV) oxide powder, which was spread in a thin layer on the downstream face of the specimen using petroleum jelly to prevent any mechanical coupling. Implementation of the system at the A2 experimental station at the Cornell High Energy Synchrotron Source (CHESS) is described. The diffraction moduli measured at CHESS were shown to compare favorably to in situ data from neutron-diffraction experiments conducted on the same alloys.« less

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)

SUNY beamline facilities at the National Synchrotron Light Source (Final Report)

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

Coppens, Philip

2003-06-22

The DOE sponsored SUNY synchrotron project has involved close cooperation among faculty at several SUNY campuses. A large number of students and postdoctoral associates have participated in its operation which was centered at the X3 beamline of the National Synchrotron Light Source at Brookhaven National Laboratory. Four stations with capabilities for Small Angle Scattering, Single Crystal and Powder and Surface diffraction and EXAFS were designed and operated with capability to perform experiments at very low as well as elevated temperatures and under high vacuum. A large amount of cutting-edge science was performed at the facility, which in addition provided excellentmore » training for students and postdoctoral scientists in the field.« less

Ferroelectrics under the Synchrotron Light: A Review

PubMed Central

Fuentes-Cobas, Luis E.; Montero-Cabrera, María E.; Pardo, Lorena; Fuentes-Montero, Luis

2015-01-01

Currently, an intensive search for high-performance lead-free ferroelectric materials is taking place. ABO3 perovskites (A = Ba, Bi, Ca, K and Na; B = Fe, Nb, Ti, and Zr) appear as promising candidates. Understanding the structure–function relationship is mandatory, and, in this field, the roles of long- and short-range crystal orders and interactions are decisive. In this review, recent advances in the global and local characterization of ferroelectric materials by synchrotron light diffraction, scattering and absorption are analyzed. Single- and poly-crystal synchrotron diffraction studies allow high-resolution investigations regarding the long-range average position of ions and subtle global symmetry break-downs. Ferroelectric materials, under the action of electric fields, undergo crystal symmetry, crystallite/domain orientation distribution and strain condition transformations. Methodological aspects of monitoring these processes are discussed. Two-dimensional diffraction clarify larger scale ordering: polycrystal texture is measured from the intensities distribution along the Debye rings. Local order is investigated by diffuse scattering (DS) and X-ray absorption fine structure (XAFS) experiments. DS provides information about thermal, chemical and displacive low-dimensional disorders. XAFS investigation of ferroelectrics reveals local B-cation off-centering and oxidation state. This technique has the advantage of being element-selective. Representative reports of the mentioned studies are described. PMID:28787814

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.

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

Single-crystal diffraction at megabar conditions by synchrotron radiation

NASA Astrophysics Data System (ADS)

Merlini, Marco; Hanfland, Michael

2013-08-01

Crystal structure determination at extreme pressures is currently possible at synchrotron beamlines optimized for such a purpose. We report the description of the experimental setup available at European Synchrotron Radiation Facility ID09 beamline (Grenoble, France) and, with two examples, we illustrate the state-of-the-art experiments currently performed at third-generation synchrotrons. The first example concerns the determination of the equation of state and the structural behavior of low-spin Fe-bearing siderite in the megabar pressure range. Siderite, in fact, undergoes a first-order isosymmetric transition at 45 GPa, and, above this pressure, it features Fe2+ in electronic low-spin configuration. The local configuration of Fe coordination polyhedra, determined by structural refinements, significantly deviates from a regular octahedron. Nevertheless, no further structural transition is detected up to the maximum pressure reached in our experiments, 135 GPa. The analysis of the Fe-O bond length extrapolated to ambient pressure, which indicates that the difference in ionic radii between the high- and the low-spin state of Fe2+ is 0.172 Å, in excellent agreement with the tabulated data by Shannon and Prewitt [Effective ionic radii in oxides and fluorides. Acta Crystallogr. 1969;B25:925-946]. The second example concerns the determination and refinement of the oP8 structure adopted by sodium in the pressure interval 118-125 GPa, using an experimental dataset collected at 118 GPa. The orthorhombic [a=4.7687(15) Å, b=3.0150(6) Å, c=5.2423(7) Å, V=75.4(3) Å3] oP8 structure is topologically related to the MnP structure, with two non-equivalent atoms in the unit cell. Despite the weak scattering factor of Na atoms, the quality of the data also allows meaningful displacement parameters refinements (R1=4.6%, 14 parameters, 190 diffractions, and 105 unique) demonstrating that the current accuracy of diffraction data at extreme pressures can be comparable with ambient condition measurements.

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

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).

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 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.

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.

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

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

Thermal equation of state of Molybdenum determined from in situ synchrotron X-ray diffraction with laser-heated diamond anvil cells

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

Huang, Xiaoli; Li, Fangfei; Zhou, Qiang

Here we report that the equation of state (EOS) of Mo is obtained by an integrated technique of laser-heated DAC and synchrotron X-ray diffraction. The cold compression and thermal expansion of Mo have been measured up to 80 GPa at 300 K, and 92 GPa at 3470 K, respectively. The P-V-T data have been treated with both thermodynamic and Mie–Gruneisen-Debye methods for the thermal EOS inversion. The results are self-consistent and in agreement with the static multi-anvil compression data of Litasov et al. (J. Appl. Phys. 113, 093507 (2013)) and the theoretical data of Zeng et al. (J. Phys. Chem.more » B 114, 298 (2010)). Furthermore, these high pressure and high temperature (HPHT) data with high precision firstly complement and close the gap between the resistive heating and the shock compression experiment.« less

Thermal equation of state of Molybdenum determined from in situ synchrotron X-ray diffraction with laser-heated diamond anvil cells

DOE PAGES

Huang, Xiaoli; Li, Fangfei; Zhou, Qiang; ...

2016-02-17

Here we report that the equation of state (EOS) of Mo is obtained by an integrated technique of laser-heated DAC and synchrotron X-ray diffraction. The cold compression and thermal expansion of Mo have been measured up to 80 GPa at 300 K, and 92 GPa at 3470 K, respectively. The P-V-T data have been treated with both thermodynamic and Mie–Gruneisen-Debye methods for the thermal EOS inversion. The results are self-consistent and in agreement with the static multi-anvil compression data of Litasov et al. (J. Appl. Phys. 113, 093507 (2013)) and the theoretical data of Zeng et al. (J. Phys. Chem.more » B 114, 298 (2010)). Furthermore, these high pressure and high temperature (HPHT) data with high precision firstly complement and close the gap between the resistive heating and the shock compression experiment.« less

Polarized vacuum ultraviolet and X-radiation

NASA Technical Reports Server (NTRS)

Samson, J. A. R.

1978-01-01

The most intense source of polarized vacuum UV and X radiation is synchrotron radiation, which exhibits a degree of partially polarized light between about 80-100%. However, the radiation transmitted by vacuum UV monochromators can also be highly polarized. The Seya-Namioka type of monochromator can produce partially polarized radiation between 50-80%. For certain experiments it is necessary to know the degree of polarization of the radiation being used. Also, when synchrotron radiation and a monochromator are combined the polarization characteristic of both should be known in order to make full use of these polarization properties. The polarizing effect of monochromators (i.e., diffraction gratings) have been measured at the Seya angle and at grazing angles for various spectral orders. Experimental evidence is presented which shows that the reciprocity law holds for polarization by reflection where the angle of incidence and diffraction are unequal. These results are reviewed along with the techniques for measuring the degree of polarization.

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.

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

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

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.

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.

Rapid time-resolved diffraction studies of protein structures using synchrotron radiation

NASA Astrophysics Data System (ADS)

Bartunik, Hans D.; Bartunik, Lesley J.

1992-07-01

The crystal structure of intermediate states in biological reactions of proteins of multi-protein complexes may be studied by time-resolved X-ray diffraction techniques which make use of the high spectral brilliance, continuous wavelength distribution and pulsed time structure of synchrotron radiation. Laue diffraction methods provide a means of investigating intermediate structures with lifetimes in the millisecond time range at presently operational facilities. Third-generation storage rings which are under construction may permit one to reach a time resolution of one microsecond for non-cyclic and one nanosecond for cyclic reactions. The number of individual exposures required for exploring reciprocal space and hence the total time scale strongly depend on the lattice order that may be affected, e.g., by conformational changes. Time-resolved experiments require high population of a specific intermediate which has to be homogeneous over the crystal volume. A number of external excitation techniques have been developed including in situ liberation of active metabolites by laser pulse photolysis of photolabile inactive precursors. First applications to crystal structure analysis of catalytic intermediates of enzymes demonstrate the potential of time-resolved protein crystallography.

Structural and electronic evolution of Cr[subscript 2]O[subscript 3] on compression to 55 GPa

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

Dera, Przemyslaw; Lavina, Barbara; Meng, Yue

2016-08-15

Synchrotron single-crystal x-ray diffraction experiments have been performed on corundum-type Cr{sub 2}O{sub 3} up to a pressure of 55 GPa in Ne and He pressure transmitting media. Diffraction experiments were complemented by measurements of optical absorption spectra with single crystal samples up to 60 GPa. Results of the diffraction data analysis rule out the earlier reported monoclinic distortion at 15-30 GPa, but indicate evidence of two discontinuous transitions of electronic or magnetic nature, most likely associated with a change in magnetic ordering and charge transfer. The compression mechanism established from single crystal refinements indicates much smaller distortion of the Cr{supmore » 3+} coordination environment than was previously assumed.« less

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.

ISPyB: an information management system for synchrotron macromolecular crystallography.

PubMed

Delagenière, Solange; Brenchereau, Patrice; Launer, Ludovic; Ashton, Alun W; Leal, Ricardo; Veyrier, Stéphanie; Gabadinho, José; Gordon, Elspeth J; Jones, Samuel D; Levik, Karl Erik; McSweeney, Seán M; Monaco, Stéphanie; Nanao, Max; Spruce, Darren; Svensson, Olof; Walsh, Martin A; Leonard, Gordon A

2011-11-15

Individual research groups now analyze thousands of samples per year at synchrotron macromolecular crystallography (MX) resources. The efficient management of experimental data is thus essential if the best possible experiments are to be performed and the best possible data used in downstream processes in structure determination pipelines. Information System for Protein crystallography Beamlines (ISPyB), a Laboratory Information Management System (LIMS) with an underlying data model allowing for the integration of analyses down-stream of the data collection experiment was developed to facilitate such data management. ISPyB is now a multisite, generic LIMS for synchrotron-based MX experiments. Its initial functionality has been enhanced to include improved sample tracking and reporting of experimental protocols, the direct ranking of the diffraction characteristics of individual samples and the archiving of raw data and results from ancillary experiments and post-experiment data processing protocols. This latter feature paves the way for ISPyB to play a central role in future macromolecular structure solution pipelines and validates the application of the approach used in ISPyB to other experimental techniques, such as biological solution Small Angle X-ray Scattering and spectroscopy, which have similar sample tracking and data handling requirements.

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

Structural anomalies in undoped Gallium Arsenide observed in high resolution diffraction imaging with monochromatic synchrotron radiation

NASA Technical Reports Server (NTRS)

Steiner, B.; Kuriyama, M.; Dobbyn, R. C.; Laor, U.; Larson, D.; Brown, M.

1988-01-01

Novel, streak-like disruption features restricted to the plane of diffraction have recently been observed in images obtained by synchrotron radiation diffraction from undoped, semi-insulating gallium arsenide crystals. These features were identified as ensembles of very thin platelets or interfaces lying in (110) planes, and a structural model consisting of antiphase domain boundaries was proposed. We report here the other principal features observed in high resolution monochromatic synchrotron radiation diffraction images: (quasi) cellular structure; linear, very low-angle subgrain boundaries in (110) directions, and surface stripes in a (110) direction. In addition, we report systematic differences in the acceptance angle for images involving various diffraction vectors. When these observations are considered together, a unifying picture emerges. The presence of ensembles of thin (110) antiphase platelet regions or boundaries is generally consistent not only with the streak-like diffraction features but with the other features reported here as well. For the formation of such regions we propose two mechanisms, operating in parallel, that appear to be consistent with the various defect features observed by a variety of techniques.

Structural anomalies in undoped gallium arsenide observed in high-resolution diffraction imaging with monochromatic synchrotron radiation

NASA Technical Reports Server (NTRS)

Steiner, B.; Kuriyama, M.; Dobbyn, R. C.; Laor, U.; Larson, D.

1989-01-01

Novel, streak-like disruption features restricted to the plane of diffraction have recently been observed in images obtained by synchrotron radiation diffraction from undoped, semi-insulating gallium arsenide crystals. These features were identified as ensembles of very thin platelets or interfaces lying in (110) planes, and a structural model consisting of antiphase domain boundaries was proposed. We report here the other principal features observed in high resolution monochromatic synchrotron radiation diffraction images: (quasi) cellular structure; linear, very low-angle subgrain boundaries in (110) directions, and surface stripes in a (110) direction. In addition, we report systematic differences in the acceptance angle for images involving various diffraction vectors. When these observations are considered together, a unifying picture emerges. The presence of ensembles of thin (110) antiphase platelet regions or boundaries is generally consistent not only with the streak-like diffraction features but with the other features reported here as well. For the formation of such regions we propose two mechanisms, operating in parallel, that appear to be consistent with the various defect features observed by a variety of techniques.

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.

Elastic plastic self-consistent (EPSC) modeling of plastic deformation in fayalite olivine

DOE PAGES

Burnley, Pamela C

2015-07-01

Elastic plastic self-consistent (EPSC) simulations are used to model synchrotron X-ray diffraction observations from deformation experiments on fayalite olivine using the deformation DIA apparatus. Consistent with results from other in situ diffraction studies of monomineralic polycrystals, the results show substantial variations in stress levels among grain populations. Rather than averaging the lattice reflection stresses or choosing a single reflection to determine the macroscopic stress supported by the specimen, an EPSC simulation is used to forward model diffraction data and determine a macroscopic stress that is consistent with lattice strains of all measured diffraction lines. The EPSC simulation presented here includesmore » kink band formation among the plastic deformation mechanisms in the simulation. The inclusion of kink band formation is critical to the success of the models. This study demonstrates the importance of kink band formation as an accommodation mechanism during plastic deformation of olivine as well as the utility of using EPSC models to interpret diffraction from in situ deformation experiments.« less

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.

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.

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.

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

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).

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.

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.

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

Coherent diffractive imaging using randomly coded masks

DOE PAGES

Seaberg, Matthew H.; d'Aspremont, Alexandre; Turner, Joshua J.

2015-12-07

We experimentally demonstrate an extension to coherent diffractive imaging that encodes additional information through the use of a series of randomly coded masks, removing the need for typical object-domain constraints while guaranteeing a unique solution to the phase retrieval problem. Phase retrieval is performed using a numerical convex relaxation routine known as “PhaseCut,” an iterative algorithm known for its stability and for its ability to find the global solution, which can be found efficiently and which is robust to noise. As a result, the experiment is performed using a laser diode at 532.2 nm, enabling rapid prototyping for future X-raymore » synchrotron and even free electron laser experiments.« less

Coherent diffractive imaging using randomly coded masks

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

Seaberg, Matthew H., E-mail: seaberg@slac.stanford.edu; Linac Coherent Light Source, SLAC National Accelerator Laboratory, 2575 Sand Hill Road, Menlo Park, California 94025; D'Aspremont, Alexandre

2015-12-07

We experimentally demonstrate an extension to coherent diffractive imaging that encodes additional information through the use of a series of randomly coded masks, removing the need for typical object-domain constraints while guaranteeing a unique solution to the phase retrieval problem. Phase retrieval is performed using a numerical convex relaxation routine known as “PhaseCut,” an iterative algorithm known for its stability and for its ability to find the global solution, which can be found efficiently and which is robust to noise. The experiment is performed using a laser diode at 532.2 nm, enabling rapid prototyping for future X-ray synchrotron and even freemore » electron laser experiments.« less

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.

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.

Low-aberration beamline optics for synchrotron infrared nanospectroscopy.

PubMed

Freitas, Raul O; Deneke, Christoph; Maia, Francisco C B; Medeiros, Helton G; Moreno, Thierry; Dumas, Paul; Petroff, Yves; Westfahl, Harry

2018-04-30

Synchrotron infrared nanospectroscopy is a recently developed technique that enables new possibilities in the broadband chemical analysis of materials in the nanoscale, far beyond the diffraction limit in this frequency domain. Synchrotron infrared ports have exploited mainly the high brightness advantage provided by electron storage rings across the whole infrared range. However, optical aberrations in the beam produced by the source depth of bending magnet emission at large angles prevent infrared nanospectroscopy to reach its maximum capability. In this work we present a low-aberration optical layout specially designed and constructed for a dedicated synchrotron infrared nanospectroscopy beamline. We report excellent agreement between simulated beam profiles (from standard wave propagation and raytracing optics simulations) with experimental measurements. We report an important improvement in the infrared nanospectroscopy experiment related to the improved beamline optics. Finally, we demonstrate the performance of the nanospectroscopy endstation by measuring a hyperspectral image of a polar material and we evaluate the setup sensitivity by measuring ultra-thin polymer films down to 6 nm thick.

UV-Visible Absorption Spectroscopy Enhanced X-ray Crystallography at Synchrotron and X-ray Free Electron Laser Sources.

PubMed

Cohen, Aina E; Doukov, Tzanko; Soltis, Michael S

2016-01-01

This review describes the use of single crystal UV-Visible Absorption micro-Spectrophotometry (UV-Vis AS) to enhance the design and execution of X-ray crystallography experiments for structural investigations of reaction intermediates of redox active and photosensitive proteins. Considerations for UV-Vis AS measurements at the synchrotron and associated instrumentation are described. UV-Vis AS is useful to verify the intermediate state of an enzyme and to monitor the progression of reactions within crystals. Radiation induced redox changes within protein crystals may be monitored to devise effective diffraction data collection strategies. An overview of the specific effects of radiation damage on macromolecular crystals is presented along with data collection strategies that minimize these effects by combining data from multiple crystals used at the synchrotron and with the X-ray free electron laser.

Combined synchrotron X-ray tomography and X-ray powder diffraction using a fluorescing metal foil.

PubMed

Kappen, P; Arhatari, B D; Luu, M B; Balaur, E; Caradoc-Davies, T

2013-06-01

This study realizes the concept of simultaneous micro-X-ray computed tomography and X-ray powder diffraction using a synchrotron beamline. A thin zinc metal foil was placed in the primary, monochromatic synchrotron beam to generate a divergent wave to propagate through the samples of interest onto a CCD detector for tomographic imaging, thus removing the need for large beam illumination and high spatial resolution detection. Both low density materials (kapton tubing and a piece of plant) and higher density materials (Egyptian faience) were investigated, and elemental contrast was explored for the example of Cu and Ni meshes. The viability of parallel powder diffraction using the direct beam transmitted through the foil was demonstrated. The outcomes of this study enable further development of the technique towards in situ tomography∕diffraction studies combining micrometer and crystallographic length scales, and towards elemental contrast imaging and reconstruction methods using well defined fluorescence outputs from combinations of known fluorescence targets (elements).

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

Characterization of high energy Xe ion irradiation effects in single crystal molybdenum with depth-resolved synchrotron microbeam diffraction

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

Yun, Di; Miao, Yinbin; Xu, Ruqing

2016-04-01

Microbeam X-ray diffraction experiments were conducted at beam line 34-ID of the Advanced Photon Source (APS) on fission fragment energy Xe heavy ion irradiated single crystal Molybdenum (Mo). Lattice strain measurements were obtained with a depth resolution of 0.7 mu m, which is critical in resolving the peculiar heterogeneity of irradiation damage associated with heavy ion irradiation. Q-space diffraction peak shift measurements were correlated with lattice strain induced by the ion irradiations. Transmission electron microscopy (TEM) characterizations were performed on the as-irradiated materials as well. Nanometer sized Xe bubble microstructures were observed via TEM. Molecular Dynamics (MD) simulations were performedmore » to help interpret the lattice strain measurement results from the experiment. This study showed that the irradiation effects by fission fragment energy Xe ion irradiations can be collaboratively understood with the depth resolved X-ray diffraction and TEM measurements under the assistance of MD simulations. (c) 2015 Elsevier B.V. All rights reserved.« less

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

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.

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

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

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.

Synchrotron FTIR Imaging For The Identification Of Cell Types Within Human Tissues

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

Walsh, Michael J.; Pounder, F. Nell; Nasse, Michael J.

2010-02-03

The use of synchrotron Fourier Transform Infrared spectroscopy (S-FTIR) has been shown to be a very promising tool for biomedical research. S-FTIR spectroscopy allows for the fast acquisition of infrared (IR) spectra at a spatial resolution approaching the IR diffraction limit. The development of the Infrared Environmental Imaging (IRENI) beamline at the Synchrotron Radiation Center (SRC) at the University of Wisconsin-Madison has allowed for diffraction limited imaging measurements of cells in human prostate and breast tissues. This has allowed for the identification of cell types within tissues that would otherwise not have been resolvable using conventional FTIR sources.

The new HMI beamline MAGS: an instrument for hard X-ray diffraction at BESSY.

PubMed

Dudzik, Esther; Feyerherm, Ralf; Diete, Wolfgang; Signorato, Riccardo; Zilkens, Christopher

2006-11-01

The Hahn-Meitner-Institute Berlin is operating the new hard X-ray diffraction beamline MAGS at the Berlin synchrotron radiation source BESSY. The beamline is intended to complement the existing neutron instrumentation at the Berlin Neutron Scattering Centre. The new beamline uses a 7 T multipole wiggler to produce photon fluxes in the 10(11)-10(12) photons s(-1) (100 mA)(-1) (0.1% bandwidth)(-1) range at energies from 4 to 30 keV at the experiment. It has active bendable optics to provide flexible horizontal and vertical focusing and to compensate the large heat load from the wiggler source. The experimental end-station consists of a six-circle Huber diffractometer which can be used with an additional (polarization) analyser and different sample environments. The beamline is intended for single-crystal diffraction and resonant magnetic scattering experiments for the study of ordering phenomena, phase transitions and materials science.

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 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.

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.

Thermal expansion of monogermanides of 3d-metals

NASA Astrophysics Data System (ADS)

Valkovskiy, G. A.; Altynbaev, E. V.; Kuchugura, M. D.; Yashina, E. G.; Sukhanov, A. S.; Dyadkin, V. A.; Tsvyashchenko, A. V.; Sidorov, V. A.; Fomicheva, L. N.; Bykova, E.; Ovsyannikov, S. V.; Chernyshov, D. Yu; Grigoriev, S. V.

2016-09-01

Temperature dependent powder and single-crystal synchrotron diffraction, specific heat, magnetic susceptibility and small-angle neutron scattering experiments have revealed an anomalous response of MnGe. The anomaly becomes smeared out with decreasing Mn content in Mn1-x Co x Ge and Mn1-x Fe x Ge solid solutions. Mn spin state instability is discussed as a possible candidate for the observed effects.

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

Coppens, Philip; Makal, Anna; Fournier, Bertrand

In picosecond and slower pump–probe diffraction experiments, collection of response–ratio correlation sets prior to full data collection provides an invaluable confirmation of the existence of a light-induced signal prior to full data collection. If a response to light exposure is observed, the quality of the data being collected can be assessed. We present a number of such correlation plots both for synchrotron and in-house pump–probe data collection.

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

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

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.

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 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

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

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

Diffraction imaging (topography) with monochromatic synchrotron radiation

NASA Technical Reports Server (NTRS)

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

1988-01-01

Structural information of special interest to crystal growers and device physicists is now available from high resolution monochromatic synchrotron diffraction imaging (topography). In the review, the importance of superior resolution in momentum transfer and in space is described, and illustrations are taken from a variety of crystals: gallium arsenide, cadmium telluride, mercuric iodide, bismuth silicon oxide, and lithium niobate. The identification and understanding of local variations in crystal growth processes are shown. Finally, new experimental opportunities now available for exploitation are indicated.

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.

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

Sauter, Nicholas K., E-mail: nksauter@lbl.gov; Hattne, Johan; Grosse-Kunstleve, Ralf W.

The Computational Crystallography Toolbox (cctbx) is a flexible software platform that has been used to develop high-throughput crystal-screening tools for both synchrotron sources and X-ray free-electron lasers. Plans for data-processing and visualization applications are discussed, and the benefits and limitations of using graphics-processing units are evaluated. Current pixel-array detectors produce diffraction images at extreme data rates (of up to 2 TB h{sup −1}) that make severe demands on computational resources. New multiprocessing frameworks are required to achieve rapid data analysis, as it is important to be able to inspect the data quickly in order to guide the experiment in realmore » time. By utilizing readily available web-serving tools that interact with the Python scripting language, it was possible to implement a high-throughput Bragg-spot analyzer (cctbx.spotfinder) that is presently in use at numerous synchrotron-radiation beamlines. Similarly, Python interoperability enabled the production of a new data-reduction package (cctbx.xfel) for serial femtosecond crystallography experiments at the Linac Coherent Light Source (LCLS). Future data-reduction efforts will need to focus on specialized problems such as the treatment of diffraction spots on interleaved lattices arising from multi-crystal specimens. In these challenging cases, accurate modeling of close-lying Bragg spots could benefit from the high-performance computing capabilities of graphics-processing units.« less

The use of a mini-κ goniometer head in macromolecular crystallography diffraction experiments

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

Brockhauser, Sandor; UJF–EMBL–CNRS UMI 3265, 6 Rue Jules Horowitz, 38043 Grenoble; Ravelli, Raimond B. G.

2013-07-01

Hardware and software solutions for MX data-collection strategies using the EMBL/ESRF miniaturized multi-axis goniometer head are presented. Most macromolecular crystallography (MX) diffraction experiments at synchrotrons use a single-axis goniometer. This markedly contrasts with small-molecule crystallography, in which the majority of the diffraction data are collected using multi-axis goniometers. A novel miniaturized κ-goniometer head, the MK3, has been developed to allow macromolecular crystals to be aligned. It is available on the majority of the structural biology beamlines at the ESRF, as well as elsewhere. In addition, the Strategy for the Alignment of Crystals (STAC) software package has been developed to facilitatemore » the use of the MK3 and other similar devices. Use of the MK3 and STAC is streamlined by their incorporation into online analysis tools such as EDNA. The current use of STAC and MK3 on the MX beamlines at the ESRF is discussed. It is shown that the alignment of macromolecular crystals can result in improved diffraction data quality compared with data obtained from randomly aligned crystals.« less

Synchrotron X-ray diffraction investigations on strains in the oxide layer of an irradiated Zircaloy fuel cladding

NASA Astrophysics Data System (ADS)

Chollet, Mélanie; Valance, Stéphane; Abolhassani, Sousan; Stein, Gene; Grolimund, Daniel; Martin, Matthias; Bertsch, Johannes

2017-05-01

For the first time the microstructure of the oxide layer of a Zircaloy-2 cladding after 9 cycles of irradiation in a boiling water reactor has been analyzed with synchrotron micro-X-ray diffraction. Crystallographic strains of the monoclinic and to some extent of the tetragonal ZrO2 are depicted through the thick oxide layer. Thin layers of sub-oxide at the oxide-metal interface as found for autoclave-tested samples and described in the literature, have not been observed in this material maybe resulting from irradiation damage. Shifts of selected diffraction peaks of the monoclinic oxide show that the uniform strain produced during oxidation is orientated in the lattice and displays variations along the oxide layer. Diffraction peaks and their shifts from families of diffracting planes could be translated into a virtual tensor. This virtual tensor exhibits changes through the oxide layer passing by tensile or compressive components.

Operation of the Australian Store.Synchrotron for macromolecular crystallography

PubMed Central

Meyer, Grischa R.; Aragão, David; Mudie, Nathan J.; Caradoc-Davies, Tom T.; McGowan, Sheena; Bertling, Philip J.; Groenewegen, David; Quenette, Stevan M.; Bond, Charles S.; Buckle, Ashley M.; Androulakis, Steve

2014-01-01

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 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). Several 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. PMID:25286837

Operation of the Australian Store.Synchrotron for macromolecular crystallography.

PubMed

Meyer, Grischa R; Aragão, David; Mudie, Nathan J; Caradoc-Davies, Tom T; McGowan, Sheena; Bertling, Philip J; Groenewegen, David; Quenette, Stevan M; Bond, Charles S; Buckle, Ashley M; Androulakis, Steve

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 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). Several 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.

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.

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.

Backbone N xH compounds at high pressures

DOE PAGES

Goncharov, Alexander F.; Holtgrewe, Nicholas; Qian, Guangrui; ...

2015-06-05

Optical and synchrotron x-ray diffraction diamond anvil cell experiments have been combined with first principles theoretical structure predictions to investigate mixtures of N 2 and H 2 up to 55 GPa. Our experiments show the formation of structurally complex van der Waals compounds above 10 GPa. However, we found that these N xH (0.52, H 2, and NH 3 above approximately 40 GPa. Lastly, our results suggest new pathways for synthesis of environmentally benign high energy-density materials. These materials could also exist as alternative planetary ices.

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

Dynamic full-field infrared imaging with multiple synchrotron beams

PubMed Central

Stavitski, Eli; Smith, Randy J.; Bourassa, Megan W.; Acerbo, Alvin S.; Carr, G. L.; Miller, Lisa M.

2013-01-01

Microspectroscopic imaging in the infrared (IR) spectral region allows for the examination of spatially resolved chemical composition on the microscale. More than a decade ago, it was demonstrated that diffraction limited spatial resolution can be achieved when an apertured, single pixel IR microscope is coupled to the high brightness of a synchrotron light source. Nowadays, many IR microscopes are equipped with multi-pixel Focal Plane Array (FPA) detectors, which dramatically improve data acquisition times for imaging large areas. Recently, progress been made toward efficiently coupling synchrotron IR beamlines to multi-pixel detectors, but they utilize expensive and highly customized optical schemes. Here we demonstrate the development and application of a simple optical configuration that can be implemented on most existing synchrotron IR beamlines in order to achieve full-field IR imaging with diffraction-limited spatial resolution. Specifically, the synchrotron radiation fan is extracted from the bending magnet and split into four beams that are combined on the sample, allowing it to fill a large section of the FPA. With this optical configuration, we are able to oversample an image by more than a factor of two, even at the shortest wavelengths, making image restoration through deconvolution algorithms possible. High chemical sensitivity, rapid acquisition times, and superior signal-to-noise characteristics of the instrument are demonstrated. The unique characteristics of this setup enabled the real time study of heterogeneous chemical dynamics with diffraction-limited spatial resolution for the first time. PMID:23458231

Secure web book to store structural genomics research data.

PubMed

Manjasetty, Babu A; Höppner, Klaus; Mueller, Uwe; Heinemann, Udo

2003-01-01

Recently established collaborative structural genomics programs aim at significantly accelerating the crystal structure analysis of proteins. These large-scale projects require efficient data management systems to ensure seamless collaboration between different groups of scientists working towards the same goal. Within the Berlin-based Protein Structure Factory, the synchrotron X-ray data collection and the subsequent crystal structure analysis tasks are located at BESSY, a third-generation synchrotron source. To organize file-based communication and data transfer at the BESSY site of the Protein Structure Factory, we have developed the web-based BCLIMS, the BESSY Crystallography Laboratory Information Management System. BCLIMS is a relational data management system which is powered by MySQL as the database engine and Apache HTTP as the web server. The database interface routines are written in Python programing language. The software is freely available to academic users. Here we describe the storage, retrieval and manipulation of laboratory information, mainly pertaining to the synchrotron X-ray diffraction experiments and the subsequent protein structure analysis, using BCLIMS.

Structure determination of Ba5AlF13 by coupling electron, synchrotron and neutron powder diffraction, solid-state NMR and ab initio calculations.

PubMed

Martineau, Charlotte; Allix, Mathieu; Suchomel, Matthew R; Porcher, Florence; Vivet, François; Legein, Christophe; Body, Monique; Massiot, Dominique; Taulelle, Francis; Fayon, Franck

2016-10-04

The room temperature structure of Ba 5 AlF 13 has been investigated by coupling electron, synchrotron and neutron powder diffraction, solid-state high-resolution NMR ( 19 F and 27 Al) and first principles calculations. An initial structural model has been obtained from electron and synchrotron powder diffraction data, and its main features have been confirmed by one- and two-dimensional NMR measurements. However, DFT GIPAW calculations of the 19 F isotropic shieldings revealed an inaccurate location of one fluorine site (F3, site 8a), which exhibited unusual long F-Ba distances. The atomic arrangement was reinvestigated using neutron powder diffraction data. Subsequent Fourier maps showed that this fluorine atom occupies a crystallographic site of lower symmetry (32e) with partial occupancy (25%). GIPAW computations of the NMR parameters validate the refined structural model, ruling out the presence of local static disorder and indicating that the partial occupancy of this F site reflects a local motional process. Visualisation of the dynamic process was then obtained from the Rietveld refinement of neutron diffraction data using an anharmonic description of the displacement parameters to account for the thermal motion of the mobile fluorine. The whole ensemble of powder diffraction and NMR data, coupled with first principles calculations, allowed drawing an accurate structural model of Ba 5 AlF 13 , including site-specific dynamical disorder in the fluorine sub-network.

The RATIO method for time-resolved Laue crystallography

PubMed Central

Coppens, Philip; Pitak, Mateusz; Gembicky, Milan; Messerschmidt, Marc; Scheins, Stephan; Benedict, Jason; Adachi, Shin-ichi; Sato, Tokushi; Nozawa, Shunsuke; Ichiyanagi, Kohei; Chollet, Matthieu; Koshihara, Shin-ya

2009-01-01

A RATIO method for analysis of intensity changes in time-resolved pump–probe Laue diffraction experiments is described. The method eliminates the need for scaling the data with a wavelength curve representing the spectral distribution of the source and removes the effect of possible anisotropic absorption. It does not require relative scaling of series of frames and removes errors due to all but very short term fluctuations in the synchrotron beam. PMID:19240334

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

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.

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.

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.

Demonstration of a chamber for strain mapping of steel specimens under mechanical load in a hydrogen environment by synchrotron radiation

NASA Astrophysics Data System (ADS)

Connolly, Matthew; Park, Jun-Sang; Bradley, Peter; Lauria, Damian; Slifka, Andrew; Drexler, Elizabeth

2018-06-01

We demonstrate a hydrogen gas chamber suitable for lattice strain measurements and capturing radiographs of a steel specimen under a mechanical load using high energy synchrotron x-rays. The chamber is suitable for static and cyclic mechanical loading. Experiments were conducted at the 1-ID-E end station of the Advanced Photon Source, Argonne National Laboratory. Diffraction patterns show a high signal-to-noise ratio suitable for lattice strain measurements for the specimen and with minimal scattering and overlap from the gas chamber manufactured from aluminum. In situ radiographs of a specimen in the hydrogen chamber show the ability to track a growing crack and to map the lattice strain around the crack with high spatial and strain resolution.

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

DOE PAGES

Lyubimov, Artem Y.; Murray, Thomas D.; Koehl, Antoine; ...

2015-03-27

X-ray free-electron lasers (XFELs) promise to enable the collection of interpretable diffraction data from samples that are refractory to data collection at synchrotron sources. At present, however, more efficient sample-delivery methods that minimize the consumption of microcrystalline material are needed to allow the application of XFEL sources to a wide range of challenging structural targets of biological importance. Here, a microfluidic chip is presented in which microcrystals can be captured at fixed, addressable points in a trap array from a small volume (<10 µl) of a pre-existing slurry grown off-chip. The device can be mounted on a standard goniostat formore » 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

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.; Murray, Thomas D.; Koehl, Antoine

X-ray free-electron lasers (XFELs) promise to enable the collection of interpretable diffraction data from samples that are refractory to data collection at synchrotron sources. At present, however, more efficient sample-delivery methods that minimize the consumption of microcrystalline material are needed to allow the application of XFEL sources to a wide range of challenging structural targets of biological importance. Here, a microfluidic chip is presented in which microcrystals can be captured at fixed, addressable points in a trap array from a small volume (<10 µl) of a pre-existing slurry grown off-chip. The device can be mounted on a standard goniostat formore » 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

Expression, purification, crystallization and preliminary X-ray diffraction analysis of the DDX3 RNA helicase domain

PubMed Central

Rodamilans, Bernardo; Montoya, Guillermo

2007-01-01

DDX3 is a human RNA helicase that is involved in RNA processing and important human diseases. This enzyme belongs to the DEAD-box protein family, the members of which are characterized by the presence of nine conserved motifs including the Asp-Glu-Ala-Asp motif that defines the family. DDX3 has two distinct domains: an ATP-binding domain in the central region of the protein and a helicase domain in the carboxy-terminal region. The helicase domain of DDX3 was cloned and overexpressed in Escherichia coli. Crystallization experiments yielded crystals that were suitable for X-ray diffraction analysis. The final crystallization conditions were a reservoir solution consisting of 2 M ammonium sulfate, 0.1 M imidazole pH 6.4 plus 5 mM spermine tetrahydrochloride and a protein solution containing 10 mM HEPES, 500 mM ammonium sulfate pH 8.0. The crystals of the helicase domain belong to the monoclinic space group P21, with unit-cell parameters a = 43.85, b = 60.72, c = 88.39 Å, α = γ = 90, β = 101.02°, and contained three molecules per asymmetric unit. These crystals diffracted to a resolution limit of 2.2 Å using synchrotron radiation at the European Synchrotron Radiation Facility (ESRF) and the Swiss Light Source (SLS). PMID:17401195

Expression, purification, crystallization and preliminary X-ray diffraction analysis of the DDX3 RNA helicase domain.

PubMed

Rodamilans, Bernardo; Montoya, Guillermo

2007-04-01

DDX3 is a human RNA helicase that is involved in RNA processing and important human diseases. This enzyme belongs to the DEAD-box protein family, the members of which are characterized by the presence of nine conserved motifs including the Asp-Glu-Ala-Asp motif that defines the family. DDX3 has two distinct domains: an ATP-binding domain in the central region of the protein and a helicase domain in the carboxy-terminal region. The helicase domain of DDX3 was cloned and overexpressed in Escherichia coli. Crystallization experiments yielded crystals that were suitable for X-ray diffraction analysis. The final crystallization conditions were a reservoir solution consisting of 2 M ammonium sulfate, 0.1 M imidazole pH 6.4 plus 5 mM spermine tetrahydrochloride and a protein solution containing 10 mM HEPES, 500 mM ammonium sulfate pH 8.0. The crystals of the helicase domain belong to the monoclinic space group P2(1), with unit-cell parameters a = 43.85, b = 60.72, c = 88.39 A, alpha = gamma = 90, beta = 101.02 degrees , and contained three molecules per asymmetric unit. These crystals diffracted to a resolution limit of 2.2 A using synchrotron radiation at the European Synchrotron Radiation Facility (ESRF) and the Swiss Light Source (SLS).

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.

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.

The use of workflows in the design and implementation of complex experiments in macromolecular crystallography.

PubMed

Brockhauser, Sandor; Svensson, Olof; Bowler, Matthew W; Nanao, Max; Gordon, Elspeth; Leal, Ricardo M F; Popov, Alexander; Gerring, Matthew; McCarthy, Andrew A; Gotz, Andy

2012-08-01

The automation of beam delivery, sample handling and data analysis, together with increasing photon flux, diminishing focal spot size and the appearance of fast-readout detectors on synchrotron beamlines, have changed the way that many macromolecular crystallography experiments are planned and executed. Screening for the best diffracting crystal, or even the best diffracting part of a selected crystal, has been enabled by the development of microfocus beams, precise goniometers and fast-readout detectors that all require rapid feedback from the initial processing of images in order to be effective. All of these advances require the coupling of data feedback to the experimental control system and depend on immediate online data-analysis results during the experiment. To facilitate this, a Data Analysis WorkBench (DAWB) for the flexible creation of complex automated protocols has been developed. Here, example workflows designed and implemented using DAWB are presented for enhanced multi-step crystal characterizations, experiments involving crystal reorientation with kappa goniometers, crystal-burning experiments for empirically determining the radiation sensitivity of a crystal system and the application of mesh scans to find the best location of a crystal to obtain the highest diffraction quality. Beamline users interact with the prepared workflows through a specific brick within the beamline-control GUI MXCuBE.

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.

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.

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

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

NASA Astrophysics Data System (ADS)

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

2013-12-01

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

TakeTwo: an indexing algorithm suited to still images with known crystal parameters

PubMed Central

Ginn, Helen Mary; Roedig, Philip; Kuo, Anling; Evans, Gwyndaf; Sauter, Nicholas K.; Ernst, Oliver; Meents, Alke; Mueller-Werkmeister, Henrike; Miller, R. J. Dwayne; Stuart, David Ian

2016-01-01

The indexing methods currently used for serial femtosecond crystallography were originally developed for experiments in which crystals are rotated in the X-ray beam, providing significant three-dimensional information. On the other hand, shots from both X-ray free-electron lasers and serial synchrotron crystallo­graphy experiments are still images, in which the few three-dimensional data available arise only from the curvature of the Ewald sphere. Traditional synchrotron crystallography methods are thus less well suited to still image data processing. Here, a new indexing method is presented with the aim of maximizing information use from a still image given the known unit-cell dimensions and space group. Efficacy for cubic, hexagonal and orthorhombic space groups is shown, and for those showing some evidence of diffraction the indexing rate ranged from 90% (hexagonal space group) to 151% (cubic space group). Here, the indexing rate refers to the number of lattices indexed per image. PMID:27487826

TakeTwo: an indexing algorithm suited to still images with known crystal parameters

DOE PAGES

Ginn, Helen Mary; Roedig, Philip; Kuo, Anling; ...

2016-08-01

The indexing methods currently used for serial femtosecond crystallography were originally developed for experiments in which crystals are rotated in the X-ray beam, providing significant three-dimensional information. On the other hand, shots from both X-ray free-electron lasers and serial synchrotron crystallography experiments are still images, in which the few three-dimensional data available arise only from the curvature of the Ewald sphere. Traditional synchrotron crystallography methods are thus less well suited to still image data processing. Here, a new indexing method is presented with the aim of maximizing information use from a still image given the known unit-cell dimensions and spacemore » group. Efficacy for cubic, hexagonal and orthorhombic space groups is shown, and for those showing some evidence of diffraction the indexing rate ranged from 90% (hexagonal space group) to 151% (cubic space group). Here, the indexing rate refers to the number of lattices indexed per image.« 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.

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.

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

DOE PAGES

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

2016-07-06

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

X-ray diffraction 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

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.

Photoelectron diffraction and holography: Some new directions

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

Fadley, C.S.

1993-08-01

Photoelectron diffraction has by now become a versatile and powerful technique for studying surface structures, with special capabilities for resolving chemical and magnetic states of atoms and deriving direct structural information from both forward scattering along bond directions and back-scattering path length differences. Further fitting experiment to theory can lead to structural accuracies in the {plus_minus}0.03 ){Angstrom} range. Holographic inversions of such diffraction data also show considerable promise for deriving local three-dimensional structures around a given emitter with accuracies of {plus_minus}0.2--0.3 {Angstrom}. Resolving the photoelectron spin in some way and using circularly polarized radiation for excitation provide added dimensions formore » the study of magnetic systems and chiral experimental geometries. Synchrotron radiation with the highest brightness and energy resolution, as well as variable polarization, is crucial to the full exploitation of these techniques.« less

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

Development of a silicon microstrip detector with single photon sensitivity for fast dynamic diffraction experiments at a synchrotron radiation beam

NASA Astrophysics Data System (ADS)

Arakcheev, A.; Aulchenko, V.; Kudashkin, D.; Shekhtman, L.; Tolochko, B.; Zhulanov, V.

2017-06-01

Time-resolved experiments on the diffraction of synchrotron radiation (SR) from crystalline materials provide information on the evolution of a material structure after a heat, electron beam or plasma interaction with a sample under study. Changes in the material structure happen within a microsecond scale and a detector with corresponding parameters is needed. The SR channel 8 of the VEPP-4M storage ring provides radiation from the 7-pole wiggler that allows to reach several tens photons within one μs from a tungsten crystal for the most intensive diffraction peak. In order to perform experiments that allow to measure the evolution of tungsten crystalline structure under the impact of powerful laser beam, a new detector is developed, that can provide information about the distribution of a scattered SR flux in space and its evolution in time at a microsecond scale. The detector is based on the silicon p-in-n microstrip sensor with DC-coupled metal strips. The sensor contains 1024 30 mm long strips with a 50 μm pitch. 64 strips are bonded to the front-end electronics based on APC128 ASICs. The APC128 ASIC contains 128 channels that consist of a low noise integrator with 32 analogue memory cells each. The integrator equivalent noise charge is about 2000 electrons and thus the signal from individual photons with energy above 40 keV can be observed. The signal can be stored at the analogue memory with 10 MHz rate. The first measurements with the beam scattered from a tungsten crystal with energy near 60 keV demonstrated the capability of this prototype to observe the spatial distribution of the photon flux with the intensity from below one photon per channel up to 0~10 photons per channel with a frame rate from 10 kHz up to 1 MHz.

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.

Diffraction-Enhanced Computed Tomographic Imaging of Growing Piglet Joints by Using a Synchrotron Light Source

PubMed Central

Rhoades, Glendon W; Belev, George S; Chapman, L Dean; Wiebe, Sheldon P; Cooper, David M; Wong, Adelaine TF; Rosenberg, Alan M

2015-01-01

The objective of this project was to develop and test a new technology for imaging growing joints by means of diffraction-enhanced imaging (DEI) combined with CT and using a synchrotron radiation source. DEI–CT images of an explanted 4-wk-old piglet stifle joint were acquired by using a 40-keV beam. The series of scanned slices was later ‘stitched’ together, forming a 3D dataset. High-resolution DEI-CT images demonstrated fine detail within all joint structures and tissues. Striking detail of vasculature traversing between bone and cartilage, a characteristic of growing but not mature joints, was demonstrated. This report documents for the first time that DEI combined with CT and a synchrotron radiation source can generate more detailed images of intact, growing joints than can currently available conventional imaging modalities. PMID:26310464

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.

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...

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.

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.

Diffraction-limited storage-ring vacuum technology

PubMed Central

Al-Dmour, Eshraq; Ahlback, Jonny; Einfeld, Dieter; Tavares, Pedro Fernandes; Grabski, Marek

2014-01-01

Some of the characteristics of recent ultralow-emittance storage-ring designs and possibly future diffraction-limited storage rings are a compact lattice combined with small magnet apertures. Such requirements present a challenge for the design and performance of the vacuum system. The vacuum system should provide the required vacuum pressure for machine operation and be able to handle the heat load from synchrotron radiation. Small magnet apertures result in the conductance of the chamber being low, and lumped pumps are ineffective. One way to provide the required vacuum level is by distributed pumping, which can be realised by the use of a non-evaporable getter (NEG) coating of the chamber walls. It may not be possible to use crotch absorbers to absorb the heat from the synchrotron radiation because an antechamber is difficult to realise with such a compact lattice. To solve this, the chamber walls can work as distributed absorbers if they are made of a material with good thermal conductivity, and distributed cooling is used at the location where the synchrotron radiation hits the wall. The vacuum system of the 3 GeV storage ring of MAX IV is used as an example of possible solutions for vacuum technologies for diffraction-limited storage rings. PMID:25177979

Crystal-Site-Selective Spectrum of Fe3BO6 by Synchrotron Mössbauer Diffraction with Pure Nuclear Bragg Scattering

NASA Astrophysics Data System (ADS)

Nakamura, Shin; Mitsui, Takaya; Fujiwara, Kosuke; Ikeda, Naoshi; Kurokuzu, Masayuki; Shimomura, Susumu

2017-08-01

We have succeeded in obtaining the crystal-site-selective spectra of the collinear antiferromagnet Fe3BO6 using a synchrotron Mössbauer diffractometer with pure nuclear Bragg scattering at SPring-8 BL11XU. Well-resolved 300, 500, and 700 reflection spectra, having asymmetric line shapes owing to the higher-order interference effect between the nuclear energy levels, were quantitatively analyzed using a formula based on the dynamical theory of diffraction. Reasonable hyperfine parameters were obtained. The intensity ratio of Fe1 to Fe2 subspectra is in accordance with the nuclear structure factor. However, when the spectrum is measured at the peak position of the rocking curve (very near the Bragg position), the value of the center shift deviates from its intrinsic value. This is also due to the dynamical effect of γ-ray diffraction. To avoid this problem, it is necessary to use diffraction angles near the foot of the rocking curve, approximately 0.02° apart from the peak position.

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.

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.

Synchrotron-based XRD from rat bone of different age groups.

PubMed

Rao, D V; Gigante, G E; Cesareo, R; Brunetti, A; Schiavon, N; Akatsuka, T; Yuasa, T; Takeda, T

2017-05-01

Synchrotron-based XRD spectra from rat bone of different age groups (w, 56 w and 78w), lumber vertebra at early stages of bone formation, Calcium hydroxyapatite (HAp) [Ca 10 (PO 4 ) 6 (OH) 2 ] bone fill with varying composition (60% and 70%) and bone cream (35-48%), has been acquired with 15keV synchrotron X-rays. Experiments were performed at Desy, Hamburg, Germany, utilizing the Resonant and Diffraction beamline (P9), with 15keV X-rays (λ=0.82666 A 0 ). Diffraction data were quantitatively analyzed using the Rietveld refinement approach, which allowed us to characterize the structure of these samples in their early stages. Hydroxyapatite, received considerable attention in medical and materials sciences, since these materials are the hard tissues, such as bone and teeth. Higher bioactivity of these samples gained reasonable interest for biological application and for bone tissue repair in oral surgery and orthopedics. The results obtained from these samples, such as phase data, crystalline size of the phases, as well as the degree of crystallinity, confirm the apatite family crystallizing in a hexagonal system, space group P6 3 /m with the lattice parameters of a=9.4328Å and c=6.8842Å (JCPDS card #09-0432). Synchrotron-based XRD patterns are relatively sharp and well resolved and can be attributed to the hexagonal crystal form of hydroxyapatite. All the samples were examined with scanning electron microscope at an accelerating voltage of 15kV. The presence of large globules of different sizes is observed, in small age groups of the rat bone (8w) and lumber vertebra (LV), as distinguished from, large age groups (56 and 78w) in all samples with different magnification, reflects an amorphous phase without significant traces of crystalline phases. Scanning electron microscopy (SEM) was used to characterize the morphology and crystalline properties of Hap, for all the samples, from 2 to 100μm resolution. Copyright © 2017 Elsevier B.V. All rights reserved.

Characterization of Electrode Materials for Lithium Ion and Sodium Ion Batteries Using Synchrotron Radiation Techniques

PubMed Central

Doeff, Marca M.; Chen, Guoying; Cabana, Jordi; Richardson, Thomas J.; Mehta, Apurva; Shirpour, Mona; Duncan, Hugues; Kim, Chunjoong; Kam, Kinson C.; Conry, Thomas

2013-01-01

Intercalation compounds such as transition metal oxides or phosphates are the most commonly used electrode materials in Li-ion and Na-ion batteries. During insertion or removal of alkali metal ions, the redox states of transition metals in the compounds change and structural transformations such as phase transitions and/or lattice parameter increases or decreases occur. These behaviors in turn determine important characteristics of the batteries such as the potential profiles, rate capabilities, and cycle lives. The extremely bright and tunable x-rays produced by synchrotron radiation allow rapid acquisition of high-resolution data that provide information about these processes. Transformations in the bulk materials, such as phase transitions, can be directly observed using X-ray diffraction (XRD), while X-ray absorption spectroscopy (XAS) gives information about the local electronic and geometric structures (e.g. changes in redox states and bond lengths). In situ experiments carried out on operating cells are particularly useful because they allow direct correlation between the electrochemical and structural properties of the materials. These experiments are time-consuming and can be challenging to design due to the reactivity and air-sensitivity of the alkali metal anodes used in the half-cell configurations, and/or the possibility of signal interference from other cell components and hardware. For these reasons, it is appropriate to carry out ex situ experiments (e.g. on electrodes harvested from partially charged or cycled cells) in some cases. Here, we present detailed protocols for the preparation of both ex situ and in situ samples for experiments involving synchrotron radiation and demonstrate how these experiments are done. PMID:24300777

Characterization of electrode materials for lithium ion and sodium ion batteries using synchrotron radiation techniques.

PubMed

Doeff, Marca M; Chen, Guoying; Cabana, Jordi; Richardson, Thomas J; Mehta, Apurva; Shirpour, Mona; Duncan, Hugues; Kim, Chunjoong; Kam, Kinson C; Conry, Thomas

2013-11-11

Intercalation compounds such as transition metal oxides or phosphates are the most commonly used electrode materials in Li-ion and Na-ion batteries. During insertion or removal of alkali metal ions, the redox states of transition metals in the compounds change and structural transformations such as phase transitions and/or lattice parameter increases or decreases occur. These behaviors in turn determine important characteristics of the batteries such as the potential profiles, rate capabilities, and cycle lives. The extremely bright and tunable x-rays produced by synchrotron radiation allow rapid acquisition of high-resolution data that provide information about these processes. Transformations in the bulk materials, such as phase transitions, can be directly observed using X-ray diffraction (XRD), while X-ray absorption spectroscopy (XAS) gives information about the local electronic and geometric structures (e.g. changes in redox states and bond lengths). In situ experiments carried out on operating cells are particularly useful because they allow direct correlation between the electrochemical and structural properties of the materials. These experiments are time-consuming and can be challenging to design due to the reactivity and air-sensitivity of the alkali metal anodes used in the half-cell configurations, and/or the possibility of signal interference from other cell components and hardware. For these reasons, it is appropriate to carry out ex situ experiments (e.g. on electrodes harvested from partially charged or cycled cells) in some cases. Here, we present detailed protocols for the preparation of both ex situ and in situ samples for experiments involving synchrotron radiation and demonstrate how these experiments are done.

In-line digital holography with phase-shifting Greek-ladder sieves

NASA Astrophysics Data System (ADS)

Xie, Jing; Zhang, Junyong; Zhang, Yanli; Zhou, Shenlei; Zhu, Jianqiang

2018-04-01

Phase shifting is the key technique in in-line digital holography, but traditional phase shifters have their own limitations in short wavelength regions. Here, phase-shifting Greek-ladder sieves with amplitude-only modulation are introduced into in-line digital holography, which are essentially a kind of diffraction lens with three-dimensional array diffraction-limited foci. In the in-line digital holographic experiment, we design two kinds of sieves by lithography and verify the validity of their phase-shifting function by measuring a 1951 U.S. Air Force resolution test target and three-dimensional array foci. With advantages of high resolving power, low cost, and no limitations at shorter wavelengths, phase-shifting Greek-ladder sieves have great potential in X-ray holography or biochemical microscopy for the next generation of synchrotron light sources.

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.

In-situ synchrotron micro-diffraction study of surface, interface, grain structure, and strain/stress evolution during Sn whisker/hillock formation

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

Pei, Fei; Jadhav, Nitin; Buchovecky, Eric

2016-03-14

We have performed X-ray synchrotron micro-diffraction measurements to study the processes controlling the formation of hillocks and whiskers in Sn layers on Cu. The studies were done in real-time on Sn layers that were electro-deposited immediately before the X-ray measurements were started. This enabled a region of the sample to be monitored from the as-deposited state until after a hillock feature formed. In addition to measuring the grain orientation and deviatoric strain (via Laue diffraction), the X-ray fluorescence was monitored to quantify the evolution of the Sn surface morphology and the formation of intermetallic compound (IMC) at the Sn-Cu interface.more » The results capture the simultaneous growth of the feature and the corresponding film stress, grain orientation, and IMC formation. The observations are compared with proposed mechanisms for whisker/hillock growth and nucleation.« less

Basic design of a multi wire proportional counter using Garfield++ for ILSF

NASA Astrophysics Data System (ADS)

Ghahremani Gol, M.; Ashrafi, S.; Rahighi, J.

2016-12-01

The Iranian Light Source Facility (ILSF) is a new 3 GeV third generation synchrotron radiation facility in Middle East, which at the time being is in its design stage. An important aspect for the scientific success of this new source will be the availability of well adapted detectors. Position-sensitive X-ray detectors have played an important role in synchrotron radiation X-ray experiments for many years and are still in use. An operational one-dimensional multiwire position sensitive detector with delay line readout produced by ILSF showed a position resolution of 230 μm. In this paper, we introduce a 2-D position sensitive gas detector based on a multiwire proportional chamber which will be used in small/wide angle scattering and diffraction experiments with synchrotron radiation at the ILSF. The parameters of its components, including the gas filling, gas pressure, temperature, the geometry of anode and cathodes planes as well as the expected performance of the designed system will be described in the following. For the design and the simulation of MWPC the Elmer and Garfield++ codes have been employed. We have built and tested a MWPC as a prototype at ILSF. The results obtained so far show a good position sensing. After primary test the detector has been optimized and is now ready for test at Elettra.

Thermal phase transition behavior of lipid layers on a single human corneocyte cell.

PubMed

Imai, Tomohiro; Nakazawa, Hiromitsu; Kato, Satoru

2013-09-01

We have improved the selected area electron diffraction method to analyze the dynamic structural change in a single corneocyte cell non-invasively stripped off from human skin surface. The improved method made it possible to obtain reliable diffraction images to trace the structural change in the intercellular lipid layers on a single corneocyte cell during heating from 24°C to 100°C. Comparison of the results with those of synchrotron X-ray diffraction experiments on human stratum corneum sheets revealed that the intercellular lipid layers on a corneocyte cell exhibit essentially the same thermal phase transitions as those in a stratum corneum sheet. These results suggest that the structural features of the lipid layers are well preserved after the mechanical stripping of the corneocyte cell. Moreover, electron diffraction analyses of the thermal phase transition behaviors of the corneocyte cells that had the lipid layers with different distributions of orthorhombic and hexagonal domains at 24°C suggested that small orthorhombic domains interconnected with surrounding hexagonal domains transforms in a continuous manner into new hexagonal domains. Copyright © 2013 Elsevier Ireland 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.

Diffraction Techniques in Structural Biology

PubMed Central

Egli, Martin

2016-01-01

A detailed understanding of chemical and biological function and the mechanisms underlying the molecular activities ultimately requires atomic-resolution structural data. Diffraction-based techniques such as single-crystal X-ray crystallography, electron microscopy, and neutron diffraction are well established and they have paved the road to the stunning successes of modern-day structural biology. The major advances achieved in the last 20 years in all aspects of structural research, including sample preparation, crystallization, the construction of synchrotron and spallation sources, phasing approaches, and high-speed computing and visualization, now provide specialists and nonspecialists alike with a steady flow of molecular images of unprecedented detail. The present unit combines a general overview of diffraction methods with a detailed description of the process of a single-crystal X-ray structure determination experiment, from chemical synthesis or expression to phasing and refinement, analysis, and quality control. For novices it may serve as a stepping-stone to more in-depth treatises of the individual topics. Readers relying on structural information for interpreting functional data may find it a useful consumer guide. PMID:27248784

Diffraction Techniques in Structural Biology

PubMed Central

Egli, Martin

2010-01-01

A detailed understanding of chemical and biological function and the mechanisms underlying the activities ultimately requires atomic-resolution structural data. Diffraction-based techniques such as single-crystal X-ray crystallography, electron microscopy and neutron diffraction are well established and have paved the road to the stunning successes of modern-day structural biology. The major advances achieved in the last 20 years in all aspects of structural research, including sample preparation, crystallization, the construction of synchrotron and spallation sources, phasing approaches and high-speed computing and visualization, now provide specialists and non-specialists alike with a steady flow of molecular images of unprecedented detail. The present chapter combines a general overview of diffraction methods with a step-by-step description of the process of a single-crystal X-ray structure determination experiment, from chemical synthesis or expression to phasing and refinement, analysis and quality control. For novices it may serve as a stepping-stone to more in-depth treatises of the individual topics. Readers relying on structural information for interpreting functional data may find it a useful consumer guide. PMID:20517991

Diffraction Techniques in Structural Biology.

PubMed

Egli, Martin

2016-06-01

A detailed understanding of chemical and biological function and the mechanisms underlying the molecular activities ultimately requires atomic-resolution structural data. Diffraction-based techniques such as single-crystal X-ray crystallography, electron microscopy, and neutron diffraction are well established and they have paved the road to the stunning successes of modern-day structural biology. The major advances achieved in the last twenty years in all aspects of structural research, including sample preparation, crystallization, the construction of synchrotron and spallation sources, phasing approaches, and high-speed computing and visualization, now provide specialists and nonspecialists alike with a steady flow of molecular images of unprecedented detail. The present unit combines a general overview of diffraction methods with a detailed description of the process of a single-crystal X-ray structure determination experiment, from chemical synthesis or expression to phasing and refinement, analysis, and quality control. For novices it may serve as a stepping-stone to more in-depth treatises of the individual topics. Readers relying on structural information for interpreting functional data may find it a useful consumer guide. © 2016 by John Wiley & Sons, Inc. Copyright © 2016 John Wiley & Sons, Inc.

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.

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

Research Associate | Center for Cancer Research

Cancer.gov

PROGRAM DESCRIPTION The Basic Science Program (BSP) pursues independent, multidisciplinary research in basic and applied molecular biology, immunology, retrovirology, cancer biology, and human genetics. Research efforts and support are an integral part of the Center for Cancer Research (CCR) at the Frederick National Laboratory for Cancer Research (FNLCR). KEY ROLES/RESPONSIBILITIES - Research Associate III Dr. Zbigniew Dauter is the head investigator of the Synchrotron Radiation Research Section (SRRS) of CCR’s Macromolecular Crystallography Laboratory. The Synchrotron Radiation Research Section is located at Argonne National Laboratory, Argonne, Illinois; this is the site of the largest U.S. synchrotron facility. The SRRS uses X-ray diffraction technique to solve crystal structures of various proteins and nucleic acids of biological and medical relevance. The section is also specializing in analyzing crystal structures at extremely high resolution and accuracy and in developing methods of effective diffraction data collection and in using weak anomalous dispersion effects to solve structures of macromolecules. The areas of expertise are: Structural and molecular biology Macromolecular crystallography Diffraction data collection Dr. Dauter requires research support in these areas, and the individual will engage in the purification and preparation of samples, crystallize proteins using various techniques, and derivatize them with heavy atoms/anomalous scatterers, and establish conditions for cryogenic freezing. Individual will also participate in diffraction data collection at the Advanced Photon Source. In addition, the candidate will perform spectroscopic and chromatographic analyses of protein and nucleic acid samples in the context of their purity, oligomeric state and photophysical properties.

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.

Investigation of phase evolution of CaCu3Ti4O12 (CCTO) by in situ synchrotron high-temperature powder diffraction

NASA Astrophysics Data System (ADS)

Ouyang, Xin; Huang, Saifang; Zhang, Weijun; Cao, Peng; Huang, Zhaohui; Gao, Wei

2014-03-01

In situ synchrotron X-ray powder diffraction was used to study the high-temperature phase evolution of CaCu3Ti4O12 (CCTO) precursors prepared via solid-state and sol-gel methods. After the precursors are heated to 1225 °C, the CCTO phase is the main phase observed in the calcined powder, with the presence of some minor impurities. Comparing the two precursors, we found that the onset temperature for the CCTO phase formation is 800 °C in the sol-gel precursor, lower than that in the solid-state precursor (875 °C). Intermediate phases were only observed in the sol-gel precursor. Both precursors are able to be calcined to sub-micrometric sized powders. Based on the synchrotron data along with differential scanning calorimetry (DSC) and thermal gravimetric analysis (TGA), the phase formation sequence and mechanism during calcination are proposed in this study.

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

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.

Dislocation density evolution of AA 7020-T6 investigated by in-situ synchrotron diffraction under tensile load

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

Zhong, Z.Y., E-mail: zhengye.zhong@hzg.de; Helmholtz-Zentrum Geesthacht, Max-Planck-Straße 1, D-21502 Geesthacht; Brokmeier, H.-G.

2015-10-15

The dislocation density evolution along the loading axis of a textured AA 7020-T6 aluminum alloy during uniaxial tension was investigated by in-situ synchrotron diffraction. The highly parallel synchrotron beam at the High Energy Materials Science beamline P07 in PETRA III, DESY, offers excellent conditions to separate different influences for line broadening from which micro-strains are obtained using the modified Williamson–Hall method which is also for defect density investigations. During tensile loading the dislocation density evolution was documented from the as-received material (initial micro-strain state) to the relaxation of the strains during elastic deformation. After yield, the increasing rate of dislocationmore » density growth was relatively fast till half-way between yield and UTS. After that, the rate started to decrease and the dislocation density fluctuated as the elongation increased due to the generation and annihilation of dislocations. When dislocation generation is dominant, the correlation between the flow stress and dislocation density satisfies the Taylor equation. Besides, a method to correct the thickness effect on peak broadening is developed in the present study. - Highlights: • In-situ synchrotron diffraction was applied to characterize peak broadening. • Dislocation evolution along the loading axis during uniaxial tension was investigated. • A method to correct the sample thickness effect on peak broadening was developed. • Dislocation density and flow stress satisfy the Taylor equation at a certain range. • The texture before load and after sample fracture was analyzed.« less

In- Situ Synchrotron Diffraction Studies on Transformation Strain Development in a High-Strength Quenched and Tempered Structural Steel—Part II. Martensitic Transformation

NASA Astrophysics Data System (ADS)

Dutta, R. K.; Huizenga, R. M.; Petrov, R. H.; Amirthalingam, M.; King, A.; Gao, H.; Hermans, M. J. M.; Richardson, I. M.

2014-01-01

In-situ synchrotron diffraction studies on the kinetics of phase transformation and transformation strain development during bainitic transformation were presented in part I of the current article. In the current article, in-situ phase transformation behavior of a high-strength (830 MPa yield stress) quenched and tempered S690QL1 [Fe-0.16C-0.2Si-0.87Mn-0.33Cr-0.21Mo (wt. pct)] structural steel, during continuous cooling and under different mechanical loading conditions to promote martensitic transformation, has been studied. Time-temperature-load resolved 2D synchrotron diffraction patterns were recorded and used to calculate the phase fractions and lattice parameters of the phases during heating and cooling cycles under different loading conditions. In addition to the thermal expansion behavior, the effects of the applied stress on the elastic strains during the martensitic transformation were calculated. The results show that small tensile stresses applied at the transformation temperature do not change the kinetics of the phase transformation. The start temperature for the martensitic transformation increases with the increasing applied tensile stress. The elastic strains are not affected significantly with the increasing tensile stress. The variant selection during martensitic transformation under small applied loads (in the elastic region) is weak.

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

High-energy-resolution monochromator for nuclear resonant scattering of synchrotron radiation by Te-125 at 35.49 keV

NASA Astrophysics Data System (ADS)

Imai, Yasuhiko; Yoda, Yoshitaka; Kitao, Shinji; Masuda, Ryo; Higashitaniguchi, Satoshi; Inaba, Chika; Seto, Makoto

2007-09-01

We have developed a high-resolution monochromator (HRM) for the measurement of nuclear resonant scattering (NRS) of synchrotron radiation by Te-125 at 35.49 keV using the backscattering of sapphire (9 1 -10 68). HRMs for nuclei with excitation energies less than 30 keV have been successfully developed using high angle diffractions by silicon crystals. Nearly perfect silicon crystal, however, is not suitable for high efficient HRMs at higher energy regions because the symmetry of the crystal structure is high and the Debye-temperature is low. Therefore, we used high quality synthetic sapphire crystal, which has low symmetry of crystal structure and high Debye-temperature. The temperature of the crystal was precisely controlled around 218 K to diffract synchrotron radiation with a Bragg angle of π/2 - 0.52 mrad. Energy was tuned by changing the crystal temperature under the condition of constant diffraction angle. Energy resolution was measured by detecting nuclear forward scattering by Te-125 in enriched TeO II. The relative energy resolution of 2.1×10 -7 is achieved, that is 7.5 meV in energy bandwidth. This HRM opens studies on element-specific dynamics and electronic state of substances containing Te-125.

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.

Crystal structures of carbonates up to Mbar pressures determined by single crystal synchrotron radiation diffraction

NASA Astrophysics Data System (ADS)

Merlini, M.

2013-12-01

The recent improvements at synchrotron beamlines, currently allow single crystal diffraction experiments at extreme pressures and temperatures [1,2] on very small single crystal domains. We successfully applied such technique to determine the crystal structure adopted by carbonates at mantle pressures. The knowledge of carbon-bearing phases is in fact fundamental for any quantitative modelling of global carbon cycle. The major technical difficulty arises after first order transitions or decomposition reactions, since original crystal (apx. 10x10x5 μm3) is transformed in much smaller crystalline domains often with random orientation. The use of 3D reciprocal space visualization software and the improved resolution of new generation flat panel detectors, however, allow both identification and integration of each single crystal domain, with suitable accuracy for ab-initio structure solution, performed with direct and charge-flipping methods and successive structure refinements. The results obtained on carbonates, indicate two major crystal-chemistry trends established at high pressures. The CO32- units, planar and parallel in ambient pressure calcite and dolomite structures, becomes non parallel in calcite- and dolomite-II and III phases, allowing more flexibility in the structures with possibility to accommodate strain arising from different cation sizes (Ca and Mg in particular). Dolomite-III is therefore also observed to be thermodynamically stable at lower mantle pressures and temperatures, differently from dolomite, which undergoes decomposition into pure end-members in upper mantle. At higher pressure, towards Mbar (lowermost mantle and D'' region) in agreement with theoretical calculations [3,4] and other experimental results [5], carbon coordination transform into 4-fold CO4 units, with different polymerisation in the structure depending on carbonate composition. The second important crystal chemistry feature detected is related to Fe2+ in Fe-bearing magnesite, which spontaneously oxidises at HP/HT, forming Fe3+ carbonates, Fe3+ oxides and reduced carbon (diamonds). Single crystal diffraction approach allowed full structure determination of these phases, yielding to the discovery of few unpredicted structures, such as Mg2Fe2C4O13 and Fe13O19, which can be well reproduced in different experiments. Mg2Fe2C4O13 carbonate present truncated chain C4O13 groups, and Fe13O19 oxide, whose stoichiometry is intermediate between magnetite and hematite, is a one-layer structure, with features encountered in superconducting materials. The results fully support the ideas of unexpected complexities in the mineralogy of the lowermost mantle, and single crystal technique, once properly optimized in ad-hoc synchrotron beamlines, is fundamental for extracting accurate structural information, otherwise rarely accessible with other experimental techniques. References: [1] Merlini M., Hanfland M. (2013). Single crystal diffraction at Mbar conditions by synchrotron radiation. High Pressure Research, in press. [2] Dubrovinsky et al., (2010). High Pressure Research, 30, 620-633. [3] Arapan et al. (1997). Phys. Rev. Lett., 98, 268501. [4] Oganov et al. (2008) EPSL, 273, 38-47. [5] Boulard et al. (2011) PNAS, 108, 5184-5187.

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

Goniometer-based femtosecond crystallography with X-ray free electron lasers

DOE PAGES

Cohen, Aina E.; Soltis, S. Michael; González, Ana; ...

2014-10-31

The emerging method of femtosecond crystallography (FX) may extend the diffraction resolution accessible from small radiation-sensitive crystals and provides a means to determine catalytically accurate structures of acutely radiation-sensitive metalloenzymes. Automated goniometer-based instrumentation developed for use at the Linac Coherent Light Source enabled efficient and flexible FX experiments to be performed on a variety of sample types. In the case of rod-shaped Cpl hydrogenase crystals, only five crystals and about 30 min of beam time were used to obtain the 125 still diffraction patterns used to produce a 1.6-Å resolution electron density map. With smaller crystals, high-density grids were usedmore » to increase sample throughput; 930 myoglobin crystals mounted at random orientation inside 32 grids were exposed, demonstrating the utility of this approach. Screening results from cryocooled crystals of β 2-adrenoreceptor and an RNA polymerase II complex indicate the potential to extend the diffraction resolution obtainable from very radiation-sensitive samples beyond that possible with undulator-based synchrotron sources.« less

Goniometer-based femtosecond crystallography with X-ray free electron lasers

PubMed Central

Cohen, Aina E.; Soltis, S. Michael; González, Ana; Aguila, Laura; Alonso-Mori, Roberto; Barnes, Christopher O.; Baxter, Elizabeth L.; Brehmer, Winnie; Brewster, Aaron S.; Brunger, Axel T.; Calero, Guillermo; Chang, Joseph F.; Chollet, Matthieu; Ehrensberger, Paul; Eriksson, Thomas L.; Feng, Yiping; Hattne, Johan; Hedman, Britt; Hollenbeck, Michael; Holton, James M.; Keable, Stephen; Kobilka, Brian K.; Kovaleva, Elena G.; Kruse, Andrew C.; Lemke, Henrik T.; Lin, Guowu; Lyubimov, Artem Y.; Manglik, Aashish; Mathews, Irimpan I.; McPhillips, Scott E.; Nelson, Silke; Peters, John W.; Sauter, Nicholas K.; Smith, Clyde A.; Song, Jinhu; Stevenson, Hilary P.; Tsai, Yingssu; Uervirojnangkoorn, Monarin; Vinetsky, Vladimir; Wakatsuki, Soichi; Weis, William I.; Zadvornyy, Oleg A.; Zeldin, Oliver B.; Zhu, Diling; Hodgson, Keith O.

2014-01-01

The emerging method of femtosecond crystallography (FX) may extend the diffraction resolution accessible from small radiation-sensitive crystals and provides a means to determine catalytically accurate structures of acutely radiation-sensitive metalloenzymes. Automated goniometer-based instrumentation developed for use at the Linac Coherent Light Source enabled efficient and flexible FX experiments to be performed on a variety of sample types. In the case of rod-shaped Cpl hydrogenase crystals, only five crystals and about 30 min of beam time were used to obtain the 125 still diffraction patterns used to produce a 1.6-Å resolution electron density map. For smaller crystals, high-density grids were used to increase sample throughput; 930 myoglobin crystals mounted at random orientation inside 32 grids were exposed, demonstrating the utility of this approach. Screening results from cryocooled crystals of β2-adrenoreceptor and an RNA polymerase II complex indicate the potential to extend the diffraction resolution obtainable from very radiation-sensitive samples beyond that possible with undulator-based synchrotron sources. PMID:25362050

Microyielding of core-shell crystal dendrites in a bulk-metallic-glass matrix composite

DOE PAGES

Huang, E. -Wen; Qiao, Junwei; Winiarski, Bartlomiej; ...

2014-03-18

In-situ synchrotron x-ray experiments have been used to follow the evolution of the diffraction peaks for crystalline dendrites embedded in a bulk metallic glass matrix subjected to a compressive loading-unloading cycle. We observe irreversible diffraction-peak splitting even though the load does not go beyond half of the bulk yield strength. The chemical analysis coupled with the transmission electron microscopy mapping suggests that the observed peak splitting originates from the chemical heterogeneity between the core (major peak) and the stiffer shell (minor peak) of the dendrites. A molecular dynamics model has been developed to compare the hkl-dependent microyielding of the bulkmore » metallic-glass matrix composite. As a result, the complementary diffraction measurements and the simulation results suggest that the interfaces between the amorphous matrix and the (211) crystalline planes relax under prolonged load that causes a delay in the reload curve which ultimately catches up with the original path.« less

New Python-based methods for data processing

PubMed Central

Sauter, Nicholas K.; Hattne, Johan; Grosse-Kunstleve, Ralf W.; Echols, Nathaniel

2013-01-01

Current pixel-array detectors produce diffraction images at extreme data rates (of up to 2 TB h−1) that make severe demands on computational resources. New multiprocessing frameworks are required to achieve rapid data analysis, as it is important to be able to inspect the data quickly in order to guide the experiment in real time. By utilizing readily available web-serving tools that interact with the Python scripting language, it was possible to implement a high-throughput Bragg-spot analyzer (cctbx.spotfinder) that is presently in use at numerous synchrotron-radiation beamlines. Similarly, Python interoperability enabled the production of a new data-reduction package (cctbx.xfel) for serial femto­second crystallography experiments at the Linac Coherent Light Source (LCLS). Future data-reduction efforts will need to focus on specialized problems such as the treatment of diffraction spots on interleaved lattices arising from multi-crystal specimens. In these challenging cases, accurate modeling of close-lying Bragg spots could benefit from the high-performance computing capabilities of graphics-processing units. PMID:23793153

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

NASA Astrophysics Data System (ADS)

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

2018-03-01

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

X-ray Diffraction and Multi-Frame Phase Contrast Imaging Diagnostics for IMPULSE at the Advanced Photon Source

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

Iverson, Adam; Carlson, Carl; Young, Jason

2013-07-08

The diagnostic needs of any dynamic loading platform present unique technical challenges that must be addressed in order to accurately measure in situ material properties in an extreme environment. The IMPULSE platform (IMPact system for Ultrafast Synchrotron Experiments) at the Advanced Photon Source (APS) is no exception and, in fact, may be more challenging, as the imaging diagnostics must be synchronized to both the experiment and the 60 ps wide x-ray bunches produced at APS. The technical challenges of time-resolved x-ray diffraction imaging and high-resolution multi-frame phase contrast imaging (PCI) are described in this paper. Example data from recent IMPULSEmore » experiments are shown to illustrate the advances and evolution of these diagnostics with a focus on comparing the performance of two intensified CCD cameras and their suitability for multi-frame PCI. The continued development of these diagnostics is fundamentally important to IMPULSE and many other loading platforms and will benefit future facilities such as the Dynamic Compression Sector at APS and MaRIE at Los Alamos National Laboratory.« less

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.

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

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.

A virtual laboratory for neutron and synchrotron strain scanning

NASA Astrophysics Data System (ADS)

James, J. A.; Santisteban, J. R.; Edwards, L.; Daymond, M. R.

2004-07-01

The new generation of dedicated Engineering Strain Scanners at neutron and synchrotron facilities offer considerable improvements in both counting time and spatial resolution. In order to make full use of these advances in instrumentation, the routine tasks associated with setting up measurement runs and analysing the data need to be made as efficient as possible. Such tasks include the planning of the experiment, the alignment and positioning of the specimen, the least-squares refinement of diffraction spectra, the definition of strain in the sample coordinate system, and its visualization within a 3D model of the specimen. With this aim in mind, we have written a software providing support for most of these operations. The approach is based on a virtual lab consisting of 3D models of the sample and laboratory equipment. The system has been developed for ENGIN-X, the new engineering strain scanner recently commissioned at ISIS, but it is flexible enough to be ported to other neutron or synchrotron strain scanners. The software has been designed with visiting industrial and academic researchers in mind, users who need to be able to control the instrument after only a short period of training.

First in-situ monitoring of CO2 delivery to the mantle followed by compression melting, using synchrotron generated X-ray diffraction.

NASA Astrophysics Data System (ADS)

Hammouda, Tahar; Chantel, Julien; Manthilake, Geeth; Guignard, Jérémy; Crichton, Wilson; Gaillard, Fabrice

2014-05-01

Melting of peridotite + CO2 upon compression has been directly monitored in situ, for the first time. We have combined high pressure experiments in the multianvil apparatus with synchrotron-generated X-ray diffraction, in order to monitor sample decarbonation upon heating, followed by melting upon compression. Experiments were performed in the model system CaO-MgO-SiO2+CO2, using dolomite and silicates contained in graphite capsules as starting material. Save Al, starting composition was aimed at reproducing peridotitic system. The sample was first compressed at room temperature, then heated. Decarbonation was observed at 2.2 GPa and 1100°C. After further heating to 1300°C, pressure was increased. Melting was observed at 2.7 GPa, while temperature was kept at 1300°C. All transformations were followed using X-ray diffraction. Starting with silicate + carbonate mixtures, we were thus able to keep CO2 fluid in the experimental sample at high P and T, up to the solidus. Concerning carbon recycling at subduction zones, it is known that CO2 is a non-wetting fluid in silicate aggregates. Therefore, any CO2 resulting from carbonate breakdown likely remains trapped at grain corners either in the subducted lithosphere or in the mantle wedge before eventually being trapped in mantle minerals as fluid inclusions, due to dynamic recrystallization. In this way, CO2 released from the slab may be spread laterally due to mantle convection. Entrainment to further depths by deep subduction or in convection cells induces CO2 introduction to depth wherein the solidus can be crossed, due to pressure increase. The solidus corresponds to the so-called carbonate ledge, beyond which carbonatitic melts are produced. Therefore, compression melting of CO2-bearing lithologies is a way to produce carbonatitic melts at depths corresponding to about 80 km. This mechanism is a viable explanation for the observed geophysical anomalies, such as those revealed by electrical conductivity measurements.

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.

Development of a synchrotron biaxial tensile device for in situ characterization of thin films mechanical response.

PubMed

Geandier, G; Thiaudière, D; Randriamazaoro, R N; Chiron, R; Djaziri, S; Lamongie, B; Diot, Y; Le Bourhis, E; Renault, P O; Goudeau, P; Bouaffad, A; Castelnau, O; Faurie, D; Hild, F

2010-10-01

We have developed on the DIFFABS-SOLEIL beamline a biaxial tensile machine working in the synchrotron environment for in situ diffraction characterization of thin polycrystalline films mechanical response. The machine has been designed to test compliant substrates coated by the studied films under controlled, applied strain field. Technological challenges comprise the sample design including fixation of the substrate ends, the related generation of a uniform strain field in the studied (central) volume, and the operations from the beamline pilot. Preliminary tests on 150 nm thick W films deposited onto polyimide cruciform substrates are presented. The obtained results for applied strains using x-ray diffraction and digital image correlation methods clearly show the full potentialities of this new setup.

Compact low power infrared tube furnace for in situ X-ray powder diffraction

NASA Astrophysics Data System (ADS)

Doran, A.; Schlicker, L.; Beavers, C. M.; Bhat, S.; Bekheet, M. F.; Gurlo, A.

2017-01-01

We describe the development and implementation of a compact, low power, infrared heated tube furnace for in situ powder X-ray diffraction experiments. Our silicon carbide (SiC) based furnace design exhibits outstanding thermal performance in terms of accuracy control and temperature ramping rates while simultaneously being easy to use, robust to abuse and, due to its small size and low power, producing minimal impact on surrounding equipment. Temperatures in air in excess of 1100 °C can be controlled at an accuracy of better than 1%, with temperature ramping rates up to 100 °C/s. The complete "add-in" device, minus power supply, fits in a cylindrical volume approximately 15 cm long and 6 cm in diameter and resides as close as 1 cm from other sensitive components of our experimental synchrotron endstation without adverse effects.

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.

Ultrahigh pressure deformation of polycrystaline hcp-cobalt

NASA Astrophysics Data System (ADS)

Merkel, S.; Antonangeli, D.; Fiquet, G.; Yagi, T.

2003-12-01

During the past few years, a novel set of methods has been developed allowing direct measurements on elasticity and rheology under static ultrahigh pressures using synchrotron x-ray diffraction and the diamond anvil cell. In particular, the analysis on the development of texture and uniaxial stress in a polycrystalline sample under ultrahigh pressure and non-hydrostatic conditions yielded to very interesting results on the microscopic deformation mechanisms and strength of MgO, silicate perovskite or ɛ -Fe [eg. Merkel et al. 2002, Merkel et al. 2003]. However, our understanding of the properties of the ɛ phase of iron remains poor. There are considerable uncertainties and disagreement on the results of various experiments or first-principles calculations. In particular, the results of the radial diffraction measurement on ɛ -Fe [Mao et al. 1998] have been highly controversial. In order to address this issue, we performed investigations on polycrystalline hcp-cobalt. Its properties such as the bulk modulus and thermal expansion are very close to those of ɛ -Fe and it is readily available under ambient conditions. Thus, it is a well known material and results from the high pressure radial diffraction experiments can be compared with those from well-established techniques. In the present analysis, we performed a new set a measurements between 0 and 20 GPa under ambient temperature conditions at the ESRF synchrotron source using amorphous boron gasket, monochromatic x-ray beam, and imaging plate techniques. From such an experiment, we are able to extract information on non-hydrostatic stress, elasticity, and preferred orientations of the sample in-situ under high pressure and compare them with results obtained previously on ɛ -Fe. Documenting the evolution of stress, elasticity and texture in hcp metals is of great interest for our understanding of the bulk properties and seismic anisotropy of the Earth's inner core. S. Merkel et al., J. Geophys. Res. 107 (2002) doi: 10.129/2001JB000920. S. Merkel et al., Earth Planet. Sci. Lett. 209 (2003) 351. H. Mao et al., Nature 396 (1998), 741

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.

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

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

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

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

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.

LAMBDA 2M GaAs—A multi-megapixel hard X-ray detector for synchrotrons

NASA Astrophysics Data System (ADS)

Pennicard, D.; Smoljanin, S.; Pithan, F.; Sarajlic, M.; Rothkirch, A.; Yu, Y.; Liermann, H. P.; Morgenroth, W.; Winkler, B.; Jenei, Z.; Stawitz, H.; Becker, J.; Graafsma, H.

2018-01-01

Synchrotrons can provide very intense and focused X-ray beams, which can be used to study the structure of matter down to the atomic scale. In many experiments, the quality of the results depends strongly on detector performance; in particular, experiments studying dynamics of samples require fast, sensitive X-ray detectors. "LAMBDA" is a photon-counting hybrid pixel detector system for experiments at synchrotrons, based on the Medipix3 readout chip. Its main features are a combination of comparatively small pixel size (55 μm), high readout speed at up to 2000 frames per second with no time gap between images, a large tileable module design, and compatibility with high-Z sensors for efficient detection of higher X-ray energies. A large LAMBDA system for hard X-ray detection has been built using Cr-compensated GaAs as a sensor material. The system is composed of 6 GaAs tiles, each of 768 by 512 pixels, giving a system with approximately 2 megapixels and an area of 8.5 by 8.5 cm2. While the sensor uniformity of GaAs is not as high as that of silicon, its behaviour is stable over time, and it is possible to correct nonuniformities effectively by postprocessing of images. By using multiple 10 Gigabit Ethernet data links, the system can be read out at the full speed of 2000 frames per second. The system has been used in hard X-ray diffraction experiments studying the structure of samples under extreme pressure in diamond anvil cells. These experiments can provide insight into geological processes. Thanks to the combination of high speed readout, large area and high sensitivity to hard X-rays, it is possible to obtain previously unattainable information in these experiments about atomic-scale structure on a millisecond timescale during rapid changes of pressure or temperature.

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.

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

Küchemann, Stefan; Mahn, Carsten; Samwer, Konrad

The investigation of short time dynamics using X-ray scattering techniques is commonly limited either by the read out frequency of the detector or by a low intensity. In this paper, we present a chopper system, which can increase the temporal resolution of 2D X-ray detectors by a factor of 13. This technique only applies to amorphous or polycrystalline samples due to their circular diffraction patterns. Using the chopper, we successfully increased the temporal resolution up to 5.1 ms during synchrotron experiments. For the construction, we provide a mathematical formalism, which, in principle, allows an even higher increase of the temporalmore » resolution.« less

High-pressure synthesis, amorphization, and decomposition of silane.

PubMed

Hanfland, Michael; Proctor, John E; Guillaume, Christophe L; Degtyareva, Olga; Gregoryanz, Eugene

2011-03-04

By compressing elemental silicon and hydrogen in a diamond anvil cell, we have synthesized polymeric silicon tetrahydride (SiH(4)) at 124 GPa and 300 K. In situ synchrotron x-ray diffraction reveals that the compound forms the insulating I4(1)/a structure previously proposed from ab initio calculations for the high-pressure phase of silane. From a series of high-pressure experiments at room and low temperature on silane itself, we find that its tetrahedral molecules break up, while silane undergoes pressure-induced amorphization at pressures above 60 GPa, recrystallizing at 90 GPa into the polymeric crystal structures.

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.

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

Synthesis and time-resolved structural characterization of framework and mineral sulfides

NASA Astrophysics Data System (ADS)

Cahill, Christopher Langley

A new class of open-framework organic/inorganic hybrid materials based on In-S chemistry has been discovered. The compounds therein exhibit unprecedented structural diversity compared to known porous sulfides, primarily due to variation in framework building units. Further, large increases in pore dimensions (vs. zeolites, for example) are observed as these materials consist of comer and edge linked clusters, e.g. In10S20, In9S17, In4S10 and In6S 15. Choice of organic structure directing agents (templates) and careful control of reaction conditions (temperature, pH) both in the In-S and Ge-S systems is shown not only to dictate which building unit will form, but also to direct the resulting framework topology. Several of the compounds described herein crystallize either as powders, or as crystals too small for standard in-house X-ray structural analysis. Diffraction experiments have thus required synchrotron based single crystal techniques for structure determination. Further, certain reaction mixture compositions result in multi-phase end products, the formation pathways of which have been studied with time resolved, in situ synchrotron powder diffraction. An extension of the applicability of the in situ techniques investigated the role of oxygen in hydrothermal systems. Oxidation state is proposed to dictate speciation in the Ni-Ge-S system and to promote phase transformations in the Fe-S mineral system.

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.

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.

Development of a synchrotron biaxial tensile device for in situ characterization of thin films mechanical response

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

Geandier, G.; Synchrotron SOLEIL, L'Orme des Merisiers, BP 48, 91192 Gif sur Yvette; LPMTM, UPR 9001 CNRS, Universite Paris-Nord, 93430 Villetaneuse

2010-10-15

We have developed on the DIFFABS-SOLEIL beamline a biaxial tensile machine working in the synchrotron environment for in situ diffraction characterization of thin polycrystalline films mechanical response. The machine has been designed to test compliant substrates coated by the studied films under controlled, applied strain field. Technological challenges comprise the sample design including fixation of the substrate ends, the related generation of a uniform strain field in the studied (central) volume, and the operations from the beamline pilot. Preliminary tests on 150 nm thick W films deposited onto polyimide cruciform substrates are presented. The obtained results for applied strains usingmore » x-ray diffraction and digital image correlation methods clearly show the full potentialities of this new setup.« less

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.

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.

Where is crystallography going?

PubMed Central

Ashton, Alun W.; Sorensen, Thomas

2018-01-01

Macromolecular crystallography (MX) has been a motor for biology for over half a century and this continues apace. A series of revolutions, including the production of recombinant proteins and cryo-crystallography, have meant that MX has repeatedly reinvented itself to dramatically increase its reach. Over the last 30 years synchrotron radiation has nucleated a succession of advances, ranging from detectors to optics and automation. These advances, in turn, open up opportunities. For instance, a further order of magnitude could perhaps be gained in signal to noise for general synchrotron experiments. In addition, X-ray free-electron lasers offer to capture fragments of reciprocal space without radiation damage, and open up the subpicosecond regime of protein dynamics and activity. But electrons have recently stolen the limelight: so is X-ray crystallography in rude health, or will imaging methods, especially single-particle electron microscopy, render it obsolete for the most interesting biology, whilst electron diffraction enables structure determination from even the smallest crystals? We will lay out some information to help you decide. PMID:29533241

Real-time data-intensive computing

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

Parkinson, Dilworth Y., E-mail: dyparkinson@lbl.gov; Chen, Xian; Hexemer, Alexander

2016-07-27

Today users visit synchrotrons as sources of understanding and discovery—not as sources of just light, and not as sources of data. To achieve this, the synchrotron facilities frequently provide not just light but often the entire end station and increasingly, advanced computational facilities that can reduce terabytes of data into a form that can reveal a new key insight. The Advanced Light Source (ALS) has partnered with high performance computing, fast networking, and applied mathematics groups to create a “super-facility”, giving users simultaneous access to the experimental, computational, and algorithmic resources to make this possible. This combination forms an efficientmore » closed loop, where data—despite its high rate and volume—is transferred and processed immediately and automatically on appropriate computing resources, and results are extracted, visualized, and presented to users or to the experimental control system, both to provide immediate insight and to guide decisions about subsequent experiments during beamtime. We will describe our work at the ALS ptychography, scattering, micro-diffraction, and micro-tomography beamlines.« less

A comparative study on the experimentally derived electron densities of three protease inhibitor model compounds.

PubMed

Grabowsky, Simon; Pfeuffer, Thomas; Morgenroth, Wolfgang; Paulmann, Carsten; Schirmeister, Tanja; Luger, Peter

2008-07-07

In order to contribute to a rational design of optimised protease inhibitors which can covalently block the nucleophilic amino acids of the proteases' active sites, we have chosen three model compounds (aziridine , oxirane and acceptor-substituted olefin ) for the examination of their electron-density distribution. Therefore, high-resolution low temperature (9, 27 and 100 K) X-ray diffraction experiments on single-crystals were carried out with synchrotron and conventional X-radiation. It could be shown by the analysis of the electron density using mainly Bader's Theory of Atoms in Molecules, Volkov's EPMM method for interaction energies, electrostatic potentials and Gatti's Source Function that aziridine is most suitable for drug design in this field. A regioselective nucleophilic attack at carbon atom C1 could be predicted and even hints about the reaction's stereoselectivity could be obtained. Moreover, the comparison between two data sets of aziridine (conventional X-ray source vs. synchrotron radiation) gave an estimate concerning the reproducibility of the quantitative results.

Strain response of thermal barrier coatings captured under extreme engine environments through synchrotron X-ray diffraction

NASA Astrophysics Data System (ADS)

Knipe, Kevin; Manero, Albert; Siddiqui, Sanna F.; Meid, Carla; Wischek, Janine; Okasinski, John; Almer, Jonathan; Karlsson, Anette M.; Bartsch, Marion; Raghavan, Seetha

2014-07-01

The mechanical behaviour of thermal barrier coatings in operation holds the key to understanding durability of jet engine turbine blades. Here we report the results from experiments that monitor strains in the layers of a coating subjected to thermal gradients and mechanical loads representing extreme engine environments. Hollow cylindrical specimens, with electron beam physical vapour deposited coatings, were tested with internal cooling and external heating under various controlled conditions. High-energy synchrotron X-ray measurements captured the in situ strain response through the depth of each layer, revealing the link between these conditions and the evolution of local strains. Results of this study demonstrate that variations in these conditions create corresponding trends in depth-resolved strains with the largest effects displayed at or near the interface with the bond coat. With larger temperature drops across the coating, significant strain gradients are seen, which can contribute to failure modes occurring within the layer adjacent to the interface.

Application of white beam synchrotron radiation topography to the analysis of twins

NASA Astrophysics Data System (ADS)

Yao, G.-D.; Dudley, M.; Hou, S.-Y.; DiSalvo, R.

1991-05-01

White beam synchrotron X-ray topography (WBSXRT) has been used to characterize room temperature twinning structures in lanthanum gallate and P-terphenyl single crystals. Both Laue and Bragg geometries are utilized to reveal the nature of twinning in LaGaO 3. The geometric relationships between the twin related domains and the directions of the corresponding diffracted beams are used to establish the presence of reflection twins on (11¯2) orth, (11¯2¯) orth and (11¯0) orth planes. Also described is the application of WBSXRT to reveal the twin law in the solution grown organic crystal p-terphenyl. The active twin plane was unambiguously determined to be (201) by determination of the orientation relationship between parent and twinned structures through Laue pattern analysis. Twin lamellae with the same twin plane were also observed. For both materials, no radiation damage was observed throughout the experiments. These results demonstrate the usefulness of WBSXRT for the study of twins.

Identification of phases in the interaction layer between U-Mo-Zr/Al and U-Mo-Zr/Al-Si

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

Varela, C.L. Komar; Arico, S.F.; Mirandou, M.

Out-of-pile diffusion experiments were performed between U-7wt.% Mo-1wt.% Zr and Al or Al A356 (7,1wt.% Si) at 550 deg. C. In this work morphological characterization and phase identification on both interaction layer are presented. They were carried out by the use of different techniques: optical and scanning electron microscopy, X-Ray diffraction and WDS microanalysis. In the interaction layer U-7wt.% Mo-1wt.% Zr/Al, the phases UAl{sub 3}, UAl{sub 4}, Al{sub 20}Mo{sub 2}U and Al{sub 43}Mo{sub 4}U{sub 6} were identified. In the interaction layer U-7wt.% Mo-1wt.% Zr/Al A356, the phases U(Al, Si) with 25at.% Si and Si{sub 5}U{sub 3} were identified. This lastmore » phase, with a higher Si concentration, was identified with XRD Synchrotron radiation performed at the National Synchrotron Light Laboratory (LNLS), Campinas, Brasil. (author)« less

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.

Time-Resolved Structural Analysis of Cation Exchange Reactions in Birnessite Using Synchrotron XRD

NASA Astrophysics Data System (ADS)

Lopano, C. L.; Heaney, P. J.; Post, J. E.; Hanson, J. C.; Lee, Y.; Komarneni, S.

2002-12-01

Birnessite ((Na,Ca,Mn2+) Mn7O142.8H2O) is a layered Mn-oxide with a 7.2Å spacing between the Mn octahedral sheets. Since birnessite is an abundant phase in soils, desert varnishes, and ocean nodules, it plays a significant role in soil and groundwater chemistry. Experiments by Golden et al. (1986,1987) have demonstrated that Na-buserite (hydrated birnessite) readily exchanges Na+ for a variety of other cations, including K+, Mg2+, Ca2+, Ba2+, Ni2+, and Sr2+. In light of its high cation exchange capacity, birnessite is industrially important for ion and molecular sieves and cathodic materials. In addition, birnessite serves as a precursor in the synthesis of todorokite, which has a 3x3 tunnel structure and is used as an octahedral sieve. We monitored cation-exchange reactions in birnessite by time-resolved X-ray powder diffraction with a simple flow-through cell at the National Synchrotron Light Source. The flow-through cell was developed by Lee and Parise at SUNY-Stony Brook, and this work represents its first application to Mn oxides. A series of synthetic Na-birnessite samples were saturated with chloride solutions containing dissolved K+, Mg2+, and Ba2+, ranging from 0.1M to 0.001M. Powder X-ray diffraction patterns were collected every ~ 3 minutes. The synchrotron experiments revealed that complete cation exchange occurs within three hours, and significant modifications of the arrangements of interlayer cations and water molecules accompany the exchange. Specifically, the replacement of Na by Mg resulted in the continuous growth of a discrete buserite-like phase with a 10Å layer spacing, while replacement of Na by K and Ba retained the 7Å spacing. K replacement of Na resulted in gradually decreasing peak intensity and peak merging. The Ba exchange yielded an abrupt decrease in diffraction intensities followed by a more gradual lattice change over the last 2 hours. Rietveld analysis led to the first determination of the structure of Ba-birnessite in space group C-1. With a final chi-squared parameter of 1.540, the refined lattice parameters were a = 5.178(2)Å, b = 2.850(3)Å, c = 7.320(5)Å, α = 89.512(1)°, β = 102.989(6)°, and γ = 89.893(6)°. However, the lattice parameters of the fully exchanged Ba-birnessite indicate that Ba substitution causes the unit cell to be more monoclinic.

High-resolution X-ray diffraction with no sample preparation

PubMed Central

Turner, S. M. R.; Degryse, P.; Shortland, A. J.

2017-01-01

It is shown that energy-dispersive X-ray diffraction (EDXRD) implemented in a back-reflection geometry is extremely insensitive to sample morphology and positioning even in a high-resolution configuration. This technique allows high-quality X-ray diffraction analysis of samples that have not been prepared and is therefore completely non-destructive. The experimental technique was implemented on beamline B18 at the Diamond Light Source synchrotron in Oxfordshire, UK. The majority of the experiments in this study were performed with pre-characterized geological materials in order to elucidate the characteristics of this novel technique and to develop the analysis methods. Results are presented that demonstrate phase identification, the derivation of precise unit-cell parameters and extraction of microstructural information on unprepared rock samples and other sample types. A particular highlight was the identification of a specific polytype of a muscovite in an unprepared mica schist sample, avoiding the time-consuming and difficult preparation steps normally required to make this type of identification. The technique was also demonstrated in application to a small number of fossil and archaeological samples. Back-reflection EDXRD implemented in a high-resolution configuration shows great potential in the crystallographic analysis of cultural heritage artefacts for the purposes of scientific research such as provenancing, as well as contributing to the formulation of conservation strategies. Possibilities for moving the technique from the synchrotron into museums are discussed. The avoidance of the need to extract samples from high-value and rare objects is a highly significant advantage, applicable also in other potential research areas such as palaeontology, and the study of meteorites and planetary materials brought to Earth by sample-return missions. PMID:28660862

Thaumatin crystallization aboard the International Space Station using liquid-liquid diffusion in the Enhanced Gaseous Nitrogen Dewar (EGN).

PubMed

Barnes, Cindy L; Snell, Edward H; Kundrot, Craig E

2002-05-01

This paper reports results from the first biological crystal-growth experiment on the International Space Station (ISS). Crystals of thaumatin were grown using liquid-liquid diffusion in Tygon tubing transported in the Enhanced Gaseous Nitrogen Dewar (EGN). Different volume ratios and concentrations of protein and precipitant were used to test different adaptations of the vapor-diffusion crystallization recipe to the liquid-liquid diffusion method. The EGN warmed up from 77 to 273 K in about 4 d, about the same time it took to warm from 273 to 293 K. The temperature within the EGN was 293-297 K for the majority of the experiment. Air gaps that blocked liquid-liquid diffusion formed in the tubes. Nonetheless, crystals were grown. Synchrotron diffraction data collected from the best space-grown crystal extended to 1.28 A, comparable to previous studies of space-grown thaumatin crystals. The resolution of the best ground-control crystal was only 1.47 A. It is not clear if the difference in diffraction limit arises from factors other than crystal size. Improvements in temperature control and the elimination of air gaps are needed, but the results show that the EGN on the ISS can be used to produce space-grown crystals that diffract to high resolution.

Thaumatin Crystallization Aboard the International Space Station Using Liquid-Liquid Diffusion in the Enhanced Gaseous Nitrogen Dewar (EGN)

NASA Technical Reports Server (NTRS)

Kundrot, Craig; Barnes, Cindy L.; Snell, Edward H.; Stinson, Thomas N. (Technical Monitor)

2002-01-01

This paper reports results from the first biological crystal growth experiment on the International Space Station (ISS). Crystals of thaumatin were grown using liquid-liquid diffusion in Tygon tubing transported in the Enhanced Gaseous Nitrogen Dewar (EGN). Different Volume ratios and concentrations of protein and precipitant were used to test different adaptations of the vapor diffusion crystallization recipe to the liquid-liquid diffusion method. The EGN warmed up from -196 C to 0 C in about four days, about the same time it took to warm from 0 C to 20 C. The temperature within the EGN was 20 - 24 C for the majority of the experiment. Air gaps that blocked liquid-liquid diffusion formed in the tubes. Nonetheless, crystals were grown. Synchrotron diffraction data collected from the best space grown crystal extended to 1.28 Angstroms, comparable to previous studies of space-grown thaumatin crystals. The resolution of the best ground control crystal was only 1.47 Angstroms. It is not clear if the difference in diffraction limit is due to factors other than crystal size. Improvements in temperature control and the elimination of air gaps are needed, but the results show that EGN on the ISS can be used to produce space grown crystals that diffract to high resolution.

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.

Through-silicon via-induced strain distribution in silicon interposer

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

Vianne, B., E-mail: benjamin.vianne@st.com; STMicroelectronics, 850 rue Jean Monnet, 38926 Crolles; Richard, M.-I.

2015-04-06

Strain in silicon induced by Through-Silicon Via (TSV) integration is of particular interest in the frame of the integration of active devices in silicon interposer. Nano-focused X-ray beam diffraction experiments were conducted using synchrotron radiation to investigate the thermally induced strain field in silicon around copper filled TSVs. Measurements were performed on thinned samples at room temperature and during in situ annealing at 400 °C. In order to correlate the 2D strain maps with finite elements analysis, an analytical model was developed, which takes into account beam absorption in the sample for a given diffraction geometry. The strain field along themore » [335] direction is found to be in the 10{sup −5} range at room temperature and around 10{sup −4} at 400 °C. Simulations support the expected plastification in some regions of the TSV during the annealing step.« less

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

PubMed Central

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

2016-01-01

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

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.

High Pressure Structure and Electrical Resistance Measurements on Cadmium Sulfide Nanoparticles

NASA Astrophysics Data System (ADS)

Montgomery, J. M.; Stemshorn, A. K.; Stanishevsky, A.; Vohra, Y. K.; Weir, S. T.

2010-03-01

Room-temperature four-probe electrical resistance and synchrotron x-ray diffraction measurements have been performed on dried and aqueous suspensions of CdS nanoparticles (25 nm in diameter) to 35 GPa. Nanoparticles used in these experiments were synthesized using the reaction between a cadmium salt and thiourea under hydrothermal conditions without using any surfactants. While the x-ray structure data confirms the irreversible wurtzite -> rocksalt transition seen at 2.5 GPa in bulk CdS, the corresponding resistance drop was not observed in the measured range, indicating that the nanoparticle boundaries may prevent electronic communication between particles. Further studies on dry and aqueous 10 nm nano-spheres and 9 nm diameter nano-rods are planned, and the results of these experiments will be presented.

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.

Using in-situ diffraction, elastic plastic self-consistent models and microstructural analysis to interpret the low strain behavior of olivine polycrystals in the D-DIA apparatus

NASA Astrophysics Data System (ADS)

Burnley, P. C.; Kaboli, S.

2016-12-01

The textbook stress strain curve has an elastic response followed by a yield point and then plastic flow. Typically in rock deformation experiments the observed `elastic' behavior deviates from the Young's modulus because the mechanical response of the loading frame and friction in the sample assembly and between moving parts of the loading frame cannot be easily corrected for. Stress strain curves generated in a D-DIA apparatus used in conjunction with synchrotron x-rays should not have these problems because the sample length is measured directly by radiography and the stress in the sample is measured from the sample itself by x-ray diffraction. However, the sample's `elastic behavior', in many instances, still deviates from what is expected. For example, in constant strain rate experiments on both polycrystalline San Carlos olivine and fayalite olivine conducted at a variety of temperatures (25 - 1200 C) and pressures (4 and 7 GPa) although we are able to use elastic plastic self-consistent (EPSC) models to describe the plastic behavior of the olivine we are not able to fit the initial elastic behavior for all but the lowest temperature experiments. To a first approximation it appears that samples are generally more compliant than their elastic properties would predict and that the degree of softening is temperature dependent. For D-DIA experiments which have been conducted at strain rates of 10-5 /sec, there are not enough data points to really clarify what is happening in the elastic portion of the experiment. Therefore, we conducted a suite of low strain experiments at 5 x 10-6/sec at temperatures ranging from 400 C to 1200 C. For each experiment we fit the diffraction data using EPSC models. We will present the results from our diffraction analysis as well as detailed microstructural analysis of the experimental samples using electron backscatter diffraction (EBSD) and electron channeling contrast imaging (ECCI). The relative degree of relaxation observed for each grain population in the diffraction data as well as to the predictions of the EPSC model combined with the microstructural data, will be used create a more comprehensive picture of how individual grains and various grain populations contribute to the low strain mechanical behavior of the polycrystal.

Real-time monitoring of laser powder bed fusion process using high-speed X-ray imaging and diffraction

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

Zhao, Cang; Fezzaa, Kamel; Cunningham, Ross W.

Here, we employ the high-speed synchrotron hard X-ray imaging and diffraction techniques to monitor the laser powder bed fusion (LPBF) process of Ti-6Al-4V in situ and in real time. We demonstrate that many scientifically and technologically significant phenomena in LPBF, including melt pool dynamics, powder ejection, rapid solidification, and phase transformation, can be probed with unprecedented spatial and temporal resolutions. In particular, the keyhole pore formation is experimentally revealed with high spatial and temporal resolutions. The solidification rate is quantitatively measured, and the slowly decrease in solidification rate during the relatively steady state could be a manifestation of the recalescencemore » phenomenon. The high-speed diffraction enables a reasonable estimation of the cooling rate and phase transformation rate, and the diffusionless transformation from β to α’ phase is evident. The data present here will facilitate the understanding of dynamics and kinetics in metal LPBF process, and the experiment platform established will undoubtedly become a new paradigm for future research and development of metal additive manufacturing.« less

Real-time monitoring of laser powder bed fusion process using high-speed X-ray imaging and diffraction

DOE PAGES

Zhao, Cang; Fezzaa, Kamel; Cunningham, Ross W.; ...

2017-06-15

Here, we employ the high-speed synchrotron hard X-ray imaging and diffraction techniques to monitor the laser powder bed fusion (LPBF) process of Ti-6Al-4V in situ and in real time. We demonstrate that many scientifically and technologically significant phenomena in LPBF, including melt pool dynamics, powder ejection, rapid solidification, and phase transformation, can be probed with unprecedented spatial and temporal resolutions. In particular, the keyhole pore formation is experimentally revealed with high spatial and temporal resolutions. The solidification rate is quantitatively measured, and the slowly decrease in solidification rate during the relatively steady state could be a manifestation of the recalescencemore » phenomenon. The high-speed diffraction enables a reasonable estimation of the cooling rate and phase transformation rate, and the diffusionless transformation from β to α’ phase is evident. The data present here will facilitate the understanding of dynamics and kinetics in metal LPBF process, and the experiment platform established will undoubtedly become a new paradigm for future research and development of metal additive manufacturing.« less

Chemical applications of synchrotron radiation: Workshop report

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

Not Available

1989-04-01

The most recent in a series of topical meetings for Advanced Photon Source user subgroups, the Workshop on Chemical Applications of Synchrotron Radiation (held at Argonne National Laboratory, October 3-4, 1988) dealt with surfaces and kinetics, spectroscopy, small-angle scattering, diffraction, and topography and imaging. The primary objectives were to provide an educational resource for the chemistry community on the scientific research being conducted at existing synchrotron sources and to indicate some of the unique opportunities that will be made available with the Advanced Photon Source. The workshop organizers were also interested in gauging the interest of chemists in the fieldmore » of synchrotron radiation. Interest expressed at the meeting has led to initial steps toward formation of a Chemistry Users Group at the APS. Individual projects are processed separately for the data bases.« less

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.

Natural Fumarolic Alteration of Fluorapatite, Olivine, and Basaltic Glass, and Implications for Habitable Environments on Mars

PubMed Central

Tschauner, Oliver

2013-01-01

Abstract Fumaroles represent a very important potential habitat on Mars because they contain water and nutrients. Global deposition of volcanic sulfate aerosols may also have been an important soil-forming process affecting large areas of Mars. Here we identify alteration from the Senator fumarole, northwest Nevada, USA, and in low-temperature environments near the fumarole to help interpret fumarolic and acid vapor alteration of rocks and soils on Mars. We analyzed soil samples and fluorapatite, olivine, and basaltic glass placed at and near the fumarole in in situ mineral alteration experiments designed to measure weathering under natural field conditions. Using synchrotron X-ray diffraction, we clearly observe hydroxyl-carbonate-bearing fluorapatite as a fumarolic alteration product of the original material, fluorapatite. The composition of apatites as well as secondary phosphates has been previously used to infer magmatic conditions as well as fumarolic conditions on Mars. To our knowledge, the observations reported here represent the first documented instance of formation of hydroxyl-carbonate-bearing apatite from fluorapatite in a field experiment. Retreat of olivine surfaces, as well as abundant NH4-containing minerals, was also characteristic of fumarolic alteration. In contrast, alteration in the nearby low-temperature environment resulted in formation of large pits on olivine surfaces, which were clearly distinguishable from the fumarolic alteration. Raman signatures of some fumarolically impacted surfaces are consistent with detection of the biological molecules chlorophyll and scytenomin, potentially useful biosignatures. Observations of altered minerals on Mars may therefore help identify the environment of formation and understand the aqueous history and potential habitability of that planet. Key Words: Fumaroles—Mars—Olivine—Acidophile—Geothermal—Search for life (biosignatures)—Synchrotron X-ray diffraction. Astrobiology 13, 1049–1064. PMID:24283927

Streaking images that appear only in the plane of diffraction in undoped GaAs single crystals: Diffraction imaging (topography) by monochromatic synchrotron radiation

NASA Technical Reports Server (NTRS)

Kuriyama, Masao; Steiner, Bruce; Dobbyn, Ronald C.; Laor, Uri; Larson, David; Brown, Margaret

1988-01-01

Streaking images restricted to the direction of the diffraction (scattering) vector have been observed on transmission through undoped GaAs. These disruption images (caused by the reduction of diffraction in the direction of observation) appear both in the forward and in Bragg diffracted directions in monochromatic synchrontron radiation diffraction imaging. This previously unobserved phenomenon can be explained in terms of planar defects (interfaces) or platelets which affects the absorption coefficient in anomalous transmission. Such regions of the crystal look perfect despite the presence of imperfections when the scattering vector is not perpendicular to the normal of the platelets. The observed crystallographic orientation of these interfaces strongly indicates that they are antiphase boundaries.

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.

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

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.

Purification, crystallization and preliminary X-ray diffraction analysis of the kinase domain of human tousled-like kinase 2

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

Garrote, Ana M.; Redondo, Pilar; Montoya, Guillermo, E-mail: gmontoya@cnio.es

2014-02-19

The C-terminal kinase domain of TLK2 (a human tousled-like kinase) has been cloned and overexpressed in Escherichia coli followed by purification to homogeneity. Crystallization experiments in the presence of ATP-γ-S yielded crystals suitable for X-ray diffraction analysis belonging to two different space groups: tetragonal I4{sub 1}22 and cubic P2{sub 1}3. Tousled-like kinases (TLKs) are an evolutionarily conserved family of serine/threonine protein kinases involved in chromatin dynamics, including DNA replication and repair, transcription and chromosome segregation. The two members of the family reported in humans, namely TLK1 and TLK2, localize to the cell nucleus and are capable of forming homo- ormore » hetero-oligomers by themselves. To characterize the role of TLK2, its C-terminal kinase domain was cloned and overexpressed in Escherichia coli followed by purification to homogeneity. Crystallization experiments in the presence of ATP-γ-S yielded crystals suitable for X-ray diffraction analysis belonging to two different space groups: tetragonal I4{sub 1}22 and cubic P2{sub 1}3. The latter produced the best diffracting crystal (3.4 Å resolution using synchrotron radiation), with unit-cell parameters a = b = c = 126.05 Å, α = β = γ = 90°. The asymmetric unit contained one protein molecule, with a Matthews coefficient of 4.59 Å{sup 3} Da{sup −1} and a solvent content of 73.23%.« less

Engineering at SLAC: Designing and constructing experimental devices for the Stanford Synchrotron Radiation Lightsource - Final Paper

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

Djang, Austin

2015-08-22

Thanks to the versatility of the beam lines at SSRL, research there is varied and benefits multiple fields. Each experiment requires a particular set of experiment equipment, which in turns requires its own particular assembly. As such, new engineering challenges arise from each new experiment. My role as an engineering intern has been to help solve these challenges, by designing and assembling experimental devices. My first project was to design a heated sample holder, which will be used to investigate the effect of temperature on a sample's x-ray diffraction pattern. My second project was to help set up an imagingmore » test, which involved designing a cooled grating holder and assembling multiple positioning stages. My third project was designing a 3D-printed pencil holder for the SSRL workstations.« less

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

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

rac-6-Hydroxy-2,5,7,8-tetramethylchroman-2-carboxamide from synchrotron data

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

Brzezinski, Krzysztof; Dauter, Zbigniew; Baj, Aneta

2012-05-29

The crystal structure of the title water-soluble analogue of vitamin E, trolox amide, C{sub 14}H{sub 19}NO{sub 3}, solved and refined against synchrotron diffraction data, contains two molecules in the asymmetric unit. In both molecules, the heterocyclic ring is in a half-chair conformation. The crystal packing features a herring-bone pattern generated by N-H...O hydrogen bonds between the hydroxy and amide groups. O-H...O hydrogen bonds also occur.

Understanding Inhomogeneous Reactions in Li‐Ion Batteries: Operando Synchrotron X‐Ray Diffraction on Two‐Layer Electrodes

PubMed Central

Villevieille, Claire; Takeuchi, Yoji

2015-01-01

To understand inhomogeneous reactions perpendicular to the current collector in an electrode for batteries, a method combining operando synchrotron X‐ray diffraction and two‐layer electrodes with different porosities is developed. The two layers are built using two different active materials (LiNi0.80Co0.15Al0.05O2 and LiMn2O4), therefore, tracing each diffraction pattern reveals which active material is reacting during the electrochemical measurement in transmission mode. The results demonstrate that the active material close to the separator is obviously more active than that one close to the current collector in the case of low porosity electrodes. This inhomogeneity should be due to the rate‐limitation and especially to low average ionic conductivity of the electrolyte in the porous electrode because the current flows first mainly into the electrode regions close to the separator. The inhomogeneity is found to be mitigated by the adjustment of the electrode density and thus porosity. Hence, the novel operando method reveals a clear inhomogeneous reaction perpendicular to the current collector. PMID:27708998

Clay pigment structure characterisation as a guide for provenance determination--a comparison between laboratory powder micro-XRD and synchrotron radiation XRD.

PubMed

Švarcová, Silvie; Bezdička, Petr; Hradil, David; Hradilová, Janka; Žižak, Ivo

2011-01-01

Application of X-ray diffraction (XRD)-based techniques in the analysis of painted artworks is not only beneficial for indisputable identification of crystal constituents in colour layers, but it can also bring insight in material crystal structure, which can be affected by their geological formation, manufacturing procedure or secondary changes. This knowledge might be helpful for art historic evaluation of an artwork as well as for its conservation. By way of example of kaolinite, we show that classification of its crystal structure order based on XRD data is useful for estimation of its provenance. We found kaolinite in the preparation layer of a Gothic wall painting in a Czech church situated near Karlovy Vary, where there are important kaolin deposits. Comparing reference kaolin materials from eight various Czech deposits, we found that these can be differentiated just according to the kaolinite crystallinity. Within this study, we compared laboratory powder X-ray micro-diffraction (micro-XRD) with synchrotron radiation X-ray diffraction analysing the same real sample. We found that both techniques led to the same results.

Structural changes induced by lattice-electron interactions: SiO2 stishovite and FeTiO3 ilmenite.

PubMed

Yamanaka, Takamitsu

2005-09-01

The bright source and highly collimated beam of synchrotron radiation offers many advantages for single-crystal structure analysis under non-ambient conditions. The structure changes induced by the lattice-electron interaction under high pressure have been investigated using a diamond anvil pressure cell. The pressure dependence of electron density distributions around atoms is elucidated by a single-crystal diffraction study using deformation electron density analysis and the maximum entropy method. In order to understand the bonding electrons under pressure, diffraction intensity measurements of FeTiO3 ilmenite and gamma-SiO2 stishovite single crystals at high pressures were made using synchrotron radiation. Both diffraction studies describe the electron density distribution including bonding electrons and provide the effective charge of the cations. In both cases the valence electrons are more localized around the cations with increasing pressure. This is consistent with molecular orbital calculations, proving that the bonding electron density becomes smaller with pressure. The thermal displacement parameters of both samples are reduced with increasing pressure.

Rastering strategy for screening and centring of microcrystal samples of human membrane proteins with a sub-10 µm size X-ray synchrotron beam

PubMed Central

Cherezov, Vadim; Hanson, Michael A.; Griffith, Mark T.; Hilgart, Mark C.; Sanishvili, Ruslan; Nagarajan, Venugopalan; Stepanov, Sergey; Fischetti, Robert F.; Kuhn, Peter; Stevens, Raymond C.

2009-01-01

Crystallization of human membrane proteins in lipidic cubic phase often results in very small but highly ordered crystals. Advent of the sub-10 µm minibeam at the APS GM/CA CAT has enabled the collection of high quality diffraction data from such microcrystals. Herein we describe the challenges and solutions related to growing, manipulating and collecting data from optically invisible microcrystals embedded in an opaque frozen in meso material. Of critical importance is the use of the intense and small synchrotron beam to raster through and locate the crystal sample in an efficient and reliable manner. The resulting diffraction patterns have a significant reduction in background, with strong intensity and improvement in diffraction resolution compared with larger beam sizes. Three high-resolution structures of human G protein-coupled receptors serve as evidence of the utility of these techniques that will likely be useful for future structural determination efforts. We anticipate that further innovations of the technologies applied to microcrystallography will enable the solving of structures of ever more challenging targets. PMID:19535414

Micron Scale Mineralogy

NASA Astrophysics Data System (ADS)

Caldwell, W. A.; Tamura, N.; Celestre, R. S.; Padmore, H. A.; Patel, J. R.

2002-12-01

Although x-ray diffraction has been used for nearly a century as the mineralogist's definitive tool in determining crystalline structures, it has proved impossible to use this technique to spatially resolve the highly heterogeneous nature of many minerals at the mesoscopic level. Due to recent revolutions in the brightness of x-ray sources and in our ability to focus x-rays, we can now carry out conventional monochromatic rotation crystallography as well as Laue diffraction with sub-micron spatial resolution and produce maps of orientation, strain, mineral type, and even chemical speciation over tens of microns in a short amount of time. We have pioneered the development of these techniques at the 3rd generation synchrotron radiation source (Advanced Light Source) in Berkeley, and will describe their application to understanding the structure of a quartz-geode. Our results show the manner in which grain structure and texture change as a function of distance from the cavity wall and are compared with models of crystal growth in such systems. This example highlights the great utility of a synchrotron based x-ray micro-diffraction beamline and the possibilities it opens to the mineralogist.

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.

Mapping the conformational landscape of a dynamic enzyme by multitemperature and XFEL crystallography

DOE PAGES

Keedy, Daniel A.; Kenner, Lillian R.; Warkentin, Matthew; ...

2015-09-30

Determining the interconverting conformations of dynamic proteins in atomic detail is a major challenge for structural biology. Conformational heterogeneity in the active site of the dynamic enzyme cyclophilin A (CypA) has been previously linked to its catalytic function, but the extent to which the different conformations of these residues are correlated is unclear. Here we compare the conformational ensembles of CypA by multitemperature synchrotron crystallography and fixed-target X-ray free-electron laser (XFEL) crystallography. The diffraction-before-destruction nature of XFEL experiments provides a radiation-damage-free view of the functionally important alternative conformations of CypA, confirming earlier synchrotron-based results. We monitored the temperature dependences ofmore » these alternative conformations with eight synchrotron datasets spanning 100-310 K. Multiconformer models show that many alternative conformations in CypA are populated only at 240 K and above, yet others remain populated or become populated at 180 K and below. These results point to a complex evolution of conformational heterogeneity between 180-–240 K that involves both thermal deactivation and solvent-driven arrest of protein motions in the crystal. The lack of a single shared conformational response to temperature within the dynamic active-site network provides evidence for a conformation shuffling model, in which exchange between rotamer states of a large aromatic ring in the middle of the network shifts the conformational ensemble for the other residues in the network. Altogether, our multitemperature analyses and XFEL data motivate a new generation of temperature- and time-resolved experiments to structurally characterize the dynamic underpinnings of protein function.« less

Mapping the conformational landscape of a dynamic enzyme by multitemperature and XFEL crystallography

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

Keedy, Daniel A.; Kenner, Lillian R.; Warkentin, Matthew

Determining the interconverting conformations of dynamic proteins in atomic detail is a major challenge for structural biology. Conformational heterogeneity in the active site of the dynamic enzyme cyclophilin A (CypA) has been previously linked to its catalytic function, but the extent to which the different conformations of these residues are correlated is unclear. Here we compare the conformational ensembles of CypA by multitemperature synchrotron crystallography and fixed-target X-ray free-electron laser (XFEL) crystallography. The diffraction-before-destruction nature of XFEL experiments provides a radiation-damage-free view of the functionally important alternative conformations of CypA, confirming earlier synchrotron-based results. We monitored the temperature dependences ofmore » these alternative conformations with eight synchrotron datasets spanning 100-310 K. Multiconformer models show that many alternative conformations in CypA are populated only at 240 K and above, yet others remain populated or become populated at 180 K and below. These results point to a complex evolution of conformational heterogeneity between 180-–240 K that involves both thermal deactivation and solvent-driven arrest of protein motions in the crystal. The lack of a single shared conformational response to temperature within the dynamic active-site network provides evidence for a conformation shuffling model, in which exchange between rotamer states of a large aromatic ring in the middle of the network shifts the conformational ensemble for the other residues in the network. Together, our multitemperature analyses and XFEL data motivate a new generation of temperature- and time-resolved experiments to structurally characterize the dynamic underpinnings of protein function.« less

Mapping the conformational landscape of a dynamic enzyme by multitemperature and XFEL crystallography

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

Keedy, Daniel A.; Kenner, Lillian R.; Warkentin, Matthew

Determining the interconverting conformations of dynamic proteins in atomic detail is a major challenge for structural biology. Conformational heterogeneity in the active site of the dynamic enzyme cyclophilin A (CypA) has been previously linked to its catalytic function, but the extent to which the different conformations of these residues are correlated is unclear. Here we compare the conformational ensembles of CypA by multitemperature synchrotron crystallography and fixed-target X-ray free-electron laser (XFEL) crystallography. The diffraction-before-destruction nature of XFEL experiments provides a radiation-damage-free view of the functionally important alternative conformations of CypA, confirming earlier synchrotron-based results. We monitored the temperature dependences ofmore » these alternative conformations with eight synchrotron datasets spanning 100-310 K. Multiconformer models show that many alternative conformations in CypA are populated only at 240 K and above, yet others remain populated or become populated at 180 K and below. These results point to a complex evolution of conformational heterogeneity between 180-–240 K that involves both thermal deactivation and solvent-driven arrest of protein motions in the crystal. The lack of a single shared conformational response to temperature within the dynamic active-site network provides evidence for a conformation shuffling model, in which exchange between rotamer states of a large aromatic ring in the middle of the network shifts the conformational ensemble for the other residues in the network. Altogether, our multitemperature analyses and XFEL data motivate a new generation of temperature- and time-resolved experiments to structurally characterize the dynamic underpinnings of protein function.« 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

Multi-element germanium detectors for synchrotron applications

NASA Astrophysics Data System (ADS)

Rumaiz, A. K.; Kuczewski, A. J.; Mead, J.; Vernon, E.; Pinelli, D.; Dooryhee, E.; Ghose, S.; Caswell, T.; Siddons, D. P.; Miceli, A.; Baldwin, J.; Almer, J.; Okasinski, J.; Quaranta, O.; Woods, R.; Krings, T.; Stock, S.

2018-04-01

We have developed a series of monolithic multi-element germanium detectors, based on sensor arrays produced by the Forschungzentrum Julich, and on Application-specific integrated circuits (ASICs) developed at Brookhaven. Devices have been made with element counts ranging from 64 to 384. These detectors are being used at NSLS-II and APS for a range of diffraction experiments, both monochromatic and energy-dispersive. Compact and powerful readout systems have been developed, based on the new generation of FPGA system-on-chip devices, which provide closely coupled multi-core processors embedded in large gate arrays. We will discuss the technical details of the systems, and present some of the results from them.

The use of radiation for the study of material of cultural heritage significance

NASA Astrophysics Data System (ADS)

Creagh, D. C.; Otieno-Alego, V.

2004-01-01

For the indigenous people of Northern Australia the expression of their experience of life, their "dreaming", is in the form of painting, usually on the bark stripped from trees growing in their tribal lands. These are often works of great beauty and the major collecting institutions in Australia and elsewhere have significant holdings of Aboriginal bark paintings. A wide range of analytical techniques (optical microscopy, FTIR microscopy, Raman microscopy, scanning electron microscopy and energy dispersive X-ray spectroscopy, and synchrotron radiation X-ray diffraction) has been used in a project to determine how best to conserve Aboriginal bark paintings.

Hirshfeld atom refinement for modelling strong hydrogen bonds.

PubMed

Woińska, Magdalena; Jayatilaka, Dylan; Spackman, Mark A; Edwards, Alison J; Dominiak, Paulina M; Woźniak, Krzysztof; Nishibori, Eiji; Sugimoto, Kunihisa; Grabowsky, Simon

2014-09-01

High-resolution low-temperature synchrotron X-ray diffraction data of the salt L-phenylalaninium hydrogen maleate are used to test the new automated iterative Hirshfeld atom refinement (HAR) procedure for the modelling of strong hydrogen bonds. The HAR models used present the first examples of Z' > 1 treatments in the framework of wavefunction-based refinement methods. L-Phenylalaninium hydrogen maleate exhibits several hydrogen bonds in its crystal structure, of which the shortest and the most challenging to model is the O-H...O intramolecular hydrogen bond present in the hydrogen maleate anion (O...O distance is about 2.41 Å). In particular, the reconstruction of the electron density in the hydrogen maleate moiety and the determination of hydrogen-atom properties [positions, bond distances and anisotropic displacement parameters (ADPs)] are the focus of the study. For comparison to the HAR results, different spherical (independent atom model, IAM) and aspherical (free multipole model, MM; transferable aspherical atom model, TAAM) X-ray refinement techniques as well as results from a low-temperature neutron-diffraction experiment are employed. Hydrogen-atom ADPs are furthermore compared to those derived from a TLS/rigid-body (SHADE) treatment of the X-ray structures. The reference neutron-diffraction experiment reveals a truly symmetric hydrogen bond in the hydrogen maleate anion. Only with HAR is it possible to freely refine hydrogen-atom positions and ADPs from the X-ray data, which leads to the best electron-density model and the closest agreement with the structural parameters derived from the neutron-diffraction experiment, e.g. the symmetric hydrogen position can be reproduced. The multipole-based refinement techniques (MM and TAAM) yield slightly asymmetric positions, whereas the IAM yields a significantly asymmetric position.

The Molecular Architecture for the Intermediate Filaments of Hard α -Keratin Based on the Superlattice Data Obtained from a Study of Mammals Using Synchrotron Fibre Diffraction

DOE PAGES

James, Veronica

2011-01-01

High- and low-angle X-ray diffraction studies of hard α -keratin have been studied, and various models have been proposed over the last 70 years. Most of these studies have been confined to one or two forms of alpha keratin. This high- and low-angle synchrotron fibre diffraction study extends the study to cover all available data for all known forms of hard α -keratin including hairs, fingernails, hooves, horn, and quills from mammals, marsupials, and a monotreme, and it confirms that the model proposed is universally acceptable for all mammals. A complete Bragg analysis of the meridional diffraction patterns, including multiple-timemore » exposures to verify any weak reflections, verified the existence of a superlattice consisting of two infinite lattices and three finite lattices. An analysis of the equatorial patterns establishes the radii of the oligomeric levels of dimers, tetramers, and intermediate filaments (IFs) together with the centre to centre distance for the IFs, thus confirming the proposed helices within helices molecular architecture for hard α -keratin. The results verify that the structure proposed by Feughelman and James meets the criteria for a valid α -keratin structure.« less

The Molecular Architecture for the Intermediate Filaments of Hard [alpha]-Keratin Based on the Superlattice Data Obtained from a Study ofMammals Using Synchrotron Fibre Diffraction

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

James, Veronica

2014-09-24

High- and low-angle X-ray diffraction studies of hard {alpha}-keratin have been studied, and various models have been proposed over the last 70 years. Most of these studies have been confined to one or two forms of alpha keratin. This high- and low-angle synchrotron fibre diffraction study extends the study to cover all available data for all known forms of hard {alpha}-keratin including hairs, fingernails, hooves, horn, and quills from mammals, marsupials, and a monotreme, and it confirms that the model proposed is universally acceptable for all mammals. A complete Bragg analysis of the meridional diffraction patterns, including multiple-time exposures tomore » verify any weak reflections, verified the existence of a superlattice consisting of two infinite lattices and three finite lattices. An analysis of the equatorial patterns establishes the radii of the oligomeric levels of dimers, tetramers, and intermediate filaments (IFs) together with the centre to centre distance for the IFs, thus confirming the proposed helices within helices molecular architecture for hard {alpha}-keratin. The results verify that the structure proposed by Feughelman and James meets the criteria for a valid {alpha}-keratin structure.« less

The Molecular Architecture for the Intermediate Filaments of Hard α -Keratin Based on the Superlattice Data Obtained from a Study of Mammals Using Synchrotron Fibre Diffraction

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

James, Veronica

High- and low-angle X-ray diffraction studies of hard α -keratin have been studied, and various models have been proposed over the last 70 years. Most of these studies have been confined to one or two forms of alpha keratin. This high- and low-angle synchrotron fibre diffraction study extends the study to cover all available data for all known forms of hard α -keratin including hairs, fingernails, hooves, horn, and quills from mammals, marsupials, and a monotreme, and it confirms that the model proposed is universally acceptable for all mammals. A complete Bragg analysis of the meridional diffraction patterns, including multiple-timemore » exposures to verify any weak reflections, verified the existence of a superlattice consisting of two infinite lattices and three finite lattices. An analysis of the equatorial patterns establishes the radii of the oligomeric levels of dimers, tetramers, and intermediate filaments (IFs) together with the centre to centre distance for the IFs, thus confirming the proposed helices within helices molecular architecture for hard α -keratin. The results verify that the structure proposed by Feughelman and James meets the criteria for a valid α -keratin structure.« less

Invited Article: Refined analysis of synchrotron radiation for NIST's SURF III facility

NASA Astrophysics Data System (ADS)

Shirley, Eric L.; Furst, Mitchell; Arp, Uwe

2018-04-01

We have developed a new method for the exact calculation of synchrotron radiation for the National Institute of Standards and Technology Synchrotron Ultraviolet Radiation Facility, SURF III. Instead of using the Schwinger formula, which is only an approximation, we develop formulae based on Graf's addition theorem for Bessel functions and accurate asymptotic expansions for Hankel functions and Bessel functions. By measuring the radiation intensity profile at two distances from the storage ring, we also confirm an apparent vertical emittance that is consistent with the vertical betatron oscillations that are intentionally introduced to extend beam lifetime by spreading the electron beam spatially. Finally, we determine how much diffraction by beamline apertures enhances the spectral irradiance at an integrating sphere entrance port at the end station. This should eliminate small but treatable components of the uncertainty budget that one should consider when using SURF III or similar synchrotrons as standard, calculable sources of ultraviolet and other radiation.

Serial millisecond crystallography of membrane and soluble protein microcrystals using synchrotron radiation

PubMed Central

Conrad, Chelsie E.; Nelson, Garrett; Stander, Natasha; Zatsepin, Nadia A.; Zook, James; Zhu, Lan; Geiger, James; Chun, Eugene; Kissick, David; Hilgart, Mark C.; Ogata, Craig; Ishchenko, Andrii; Nagaratnam, Nirupa; Roy-Chowdhury, Shatabdi; Coe, Jesse; Subramanian, Ganesh; Schaffer, Alexander; Ketwala, Gihan; Venugopalan, Nagarajan; Xu, Shenglan; Corcoran, Stephen; Ferguson, Dale; Weierstall, Uwe; Spence, John C. H.; Cherezov, Vadim; Fromme, Petra; Fischetti, Robert F.; Liu, Wei

2017-01-01

Crystal structure determination of biological macromolecules using the novel technique of serial femtosecond crystallography (SFX) is severely limited by the scarcity of X-ray free-electron laser (XFEL) sources. However, recent and future upgrades render microfocus beamlines at synchrotron-radiation sources suitable for room-temperature serial crystallography data collection also. Owing to the longer exposure times that are needed at synchrotrons, serial data collection is termed serial millisecond crystallography (SMX). As a result, the number of SMX experiments is growing rapidly, with a dozen experiments reported so far. Here, the first high-viscosity injector-based SMX experiments carried out at a US synchrotron source, the Advanced Photon Source (APS), are reported. Microcrystals (5–20 µm) of a wide variety of proteins, including lysozyme, thaumatin, phycocyanin, the human A2A adenosine receptor (A2AAR), the soluble fragment of the membrane lipoprotein Flpp3 and proteinase K, were screened. Crystals suspended in lipidic cubic phase (LCP) or a high-molecular-weight poly(ethylene oxide) (PEO; molecular weight 8 000 000) were delivered to the beam using a high-viscosity injector. In-house data-reduction (hit-finding) software developed at APS as well as the SFX data-reduction and analysis software suites Cheetah and CrystFEL enabled efficient on-site SMX data monitoring, reduction and processing. Complete data sets were collected for A2AAR, phycocyanin, Flpp3, proteinase K and lysozyme, and the structures of A2AAR, phycocyanin, proteinase K and lysozyme were determined at 3.2, 3.1, 2.65 and 2.05 Å resolution, respectively. The data demonstrate the feasibility of serial millisecond crystallography from 5–20 µm crystals using a high-viscosity injector at APS. The resolution of the crystal structures obtained in this study was dictated by the current flux density and crystal size, but upcoming developments in beamline optics and the planned APS-U upgrade will increase the intensity by two orders of magnitude. These developments will enable structure determination from smaller and/or weakly diffracting microcrystals. PMID:28875031

Serial millisecond crystallography of membrane and soluble protein microcrystals using synchrotron radiation.

PubMed

Martin-Garcia, Jose M; Conrad, Chelsie E; Nelson, Garrett; Stander, Natasha; Zatsepin, Nadia A; Zook, James; Zhu, Lan; Geiger, James; Chun, Eugene; Kissick, David; Hilgart, Mark C; Ogata, Craig; Ishchenko, Andrii; Nagaratnam, Nirupa; Roy-Chowdhury, Shatabdi; Coe, Jesse; Subramanian, Ganesh; Schaffer, Alexander; James, Daniel; Ketwala, Gihan; Venugopalan, Nagarajan; Xu, Shenglan; Corcoran, Stephen; Ferguson, Dale; Weierstall, Uwe; Spence, John C H; Cherezov, Vadim; Fromme, Petra; Fischetti, Robert F; Liu, Wei

2017-07-01

Crystal structure determination of biological macromolecules using the novel technique of serial femtosecond crystallography (SFX) is severely limited by the scarcity of X-ray free-electron laser (XFEL) sources. However, recent and future upgrades render microfocus beamlines at synchrotron-radiation sources suitable for room-temperature serial crystallography data collection also. Owing to the longer exposure times that are needed at synchrotrons, serial data collection is termed serial millisecond crystallography (SMX). As a result, the number of SMX experiments is growing rapidly, with a dozen experiments reported so far. Here, the first high-viscosity injector-based SMX experiments carried out at a US synchrotron source, the Advanced Photon Source (APS), are reported. Microcrystals (5-20 µm) of a wide variety of proteins, including lysozyme, thaumatin, phycocyanin, the human A 2A adenosine receptor (A 2A AR), the soluble fragment of the membrane lipoprotein Flpp3 and proteinase K, were screened. Crystals suspended in lipidic cubic phase (LCP) or a high-molecular-weight poly(ethylene oxide) (PEO; molecular weight 8 000 000) were delivered to the beam using a high-viscosity injector. In-house data-reduction (hit-finding) software developed at APS as well as the SFX data-reduction and analysis software suites Cheetah and CrystFEL enabled efficient on-site SMX data monitoring, reduction and processing. Complete data sets were collected for A 2A AR, phycocyanin, Flpp3, proteinase K and lysozyme, and the structures of A 2A AR, phycocyanin, proteinase K and lysozyme were determined at 3.2, 3.1, 2.65 and 2.05 Å resolution, respectively. The data demonstrate the feasibility of serial millisecond crystallography from 5-20 µm crystals using a high-viscosity injector at APS. The resolution of the crystal structures obtained in this study was dictated by the current flux density and crystal size, but upcoming developments in beamline optics and the planned APS-U upgrade will increase the intensity by two orders of magnitude. These developments will enable structure determination from smaller and/or weakly diffracting microcrystals.

Serial millisecond crystallography of membrane and soluble protein microcrystals using synchrotron radiation

DOE PAGES

Martin-Garcia, Jose M.; Conrad, Chelsie E.; Nelson, Garrett; ...

2017-05-24

Crystal structure determination of biological macromolecules using the novel technique of serial femtosecond crystallography (SFX) is severely limited by the scarcity of X-ray free-electron laser (XFEL) sources. However, recent and future upgrades render microfocus beamlines at synchrotron-radiation sources suitable for room-temperature serial crystallography data collection also. Owing to the longer exposure times that are needed at synchrotrons, serial data collection is termed serial millisecond crystallography (SMX). As a result, the number of SMX experiments is growing rapidly, with a dozen experiments reported so far. Here, the first high-viscosity injector-based SMX experiments carried out at a US synchrotron source, the Advancedmore » Photon Source (APS), are reported. Microcrystals (5–20 µm) of a wide variety of proteins, including lysozyme, thaumatin, phycocyanin, the human A 2A adenosine receptor (A 2AAR), the soluble fragment of the membrane lipoprotein Flpp3 and proteinase K, were screened. Crystals suspended in lipidic cubic phase (LCP) or a high-molecular-weight poly(ethylene oxide) (PEO; molecular weight 8 000 000) were delivered to the beam using a high-viscosity injector. In-house data-reduction (hit-finding) software developed at APS as well as the SFX data-reduction and analysis software suites Cheetah and CrystFEL enabled efficient on-site SMX data monitoring, reduction and processing. Complete data sets were collected for A 2AAR, phycocyanin, Flpp3, proteinase K and lysozyme, and the structures of A 2AAR, phycocyanin, proteinase K and lysozyme were determined at 3.2, 3.1, 2.65 and 2.05 Å resolution, respectively. The data demonstrate the feasibility of serial millisecond crystallography from 5–20 µm crystals using a high-viscosity injector at APS. The resolution of the crystal structures obtained in this study was dictated by the current flux density and crystal size, but upcoming developments in beamline optics and the planned APS-U upgrade will increase the intensity by two orders of magnitude. Furthermore, these developments will enable structure determination from smaller and/or weakly diffracting microcrystals.« less

Serial millisecond crystallography of membrane and soluble protein microcrystals using synchrotron radiation

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

Martin-Garcia, Jose M.; Conrad, Chelsie E.; Nelson, Garrett

Crystal structure determination of biological macromolecules using the novel technique of serial femtosecond crystallography (SFX) is severely limited by the scarcity of X-ray free-electron laser (XFEL) sources. However, recent and future upgrades render microfocus beamlines at synchrotron-radiation sources suitable for room-temperature serial crystallography data collection also. Owing to the longer exposure times that are needed at synchrotrons, serial data collection is termed serial millisecond crystallography (SMX). As a result, the number of SMX experiments is growing rapidly, with a dozen experiments reported so far. Here, the first high-viscosity injector-based SMX experiments carried out at a US synchrotron source, the Advancedmore » Photon Source (APS), are reported. Microcrystals (5–20 µm) of a wide variety of proteins, including lysozyme, thaumatin, phycocyanin, the human A 2A adenosine receptor (A 2AAR), the soluble fragment of the membrane lipoprotein Flpp3 and proteinase K, were screened. Crystals suspended in lipidic cubic phase (LCP) or a high-molecular-weight poly(ethylene oxide) (PEO; molecular weight 8 000 000) were delivered to the beam using a high-viscosity injector. In-house data-reduction (hit-finding) software developed at APS as well as the SFX data-reduction and analysis software suites Cheetah and CrystFEL enabled efficient on-site SMX data monitoring, reduction and processing. Complete data sets were collected for A 2AAR, phycocyanin, Flpp3, proteinase K and lysozyme, and the structures of A 2AAR, phycocyanin, proteinase K and lysozyme were determined at 3.2, 3.1, 2.65 and 2.05 Å resolution, respectively. The data demonstrate the feasibility of serial millisecond crystallography from 5–20 µm crystals using a high-viscosity injector at APS. The resolution of the crystal structures obtained in this study was dictated by the current flux density and crystal size, but upcoming developments in beamline optics and the planned APS-U upgrade will increase the intensity by two orders of magnitude. Furthermore, these developments will enable structure determination from smaller and/or weakly diffracting microcrystals.« 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.

The interaction of fatigue cracks with a residual stress field using thermoelastic stress analysis and synchrotron X-ray diffraction experiments

PubMed Central

Amjad, Khurram; Asquith, David; Sebastian, Christopher M.; Wang, Wei-Chung

2017-01-01

This article presents an experimental study on the fatigue behaviour of cracks emanating from cold-expanded holes utilizing thermoelastic stress analysis (TSA) and synchrotron X-ray diffraction (SXRD) techniques with the aim of resolving the long-standing ambiguity in the literature regarding potential relaxation, or modification, of beneficial compressive residual stresses as a result of fatigue crack propagation. The crack growth rates are found to be substantially lower as the crack tip moved through the residual stress zone induced by cold expansion. The TSA results demonstrated that the crack tip plastic zones were reduced in size by the presence of the residual compressive stresses induced by cold expansion. The crack tip plastic zones were found to be insignificant in size in comparison to the residual stress zone resulting from cold expansion, which implied that they were unlikely to have had a notable impact on the surrounding residual stresses induced by cold expansion. The residual stress distributions measured along the direction of crack growth, using SXRD, showed no signs of any significant stress relaxation or redistribution, which validates the conclusions drawn from the TSA data. Fractographic analysis qualitatively confirmed the influence on crack initiation of the residual stresses induced by the cold expansion. It was found that the application of single compressive overload caused a relaxation, or reduction in the residual stresses, which has wider implications for improving the fatigue life. PMID:29291095

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.

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.

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

DOE PAGES

Murray, Thomas D.; Lyubimov, Artem Y.; Ogata, Craig M.; ...

2015-08-11

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

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

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

Murray, Thomas D.; Lyubimov, Artem Y.; Ogata, Craig M.

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

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

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

Murray, Thomas D.; Lyubimov, Artem Y.; Ogata, Craig M.

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

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

PubMed Central

Murray, Thomas D.; Lyubimov, Artem Y.; Ogata, Craig M.; Vo, Huy; Uervirojnangkoorn, Monarin; Brunger, Axel T.; Berger, James M.

2015-01-01

Microcrystals present a significant impediment to the determination of macromolecular structures by X-ray diffraction methods. Although microfocus synchrotron beamlines and X-ray free-electron lasers (XFELs) can enable the collection of interpretable diffraction data from microcrystals, there is a need for efficient methods of harvesting small volumes (<2 µl) of microcrystals grown under common laboratory formats and delivering them to an X-ray beam source under native growth conditions. One approach that shows promise in overcoming the challenges intrinsic to microcrystal analysis is to pair so-called ‘fixed-target’ sample-delivery devices with microbeam-based X-ray diffraction methods. However, to record weak diffraction patterns it is necessary to fabricate devices from X-ray-transparent materials that minimize background scattering. Presented here is the design of a new micro-diffraction device consisting of three layers fabricated from silicon nitride, photoresist and polyimide film. The chip features low X-ray scattering and X-ray absorption properties, and uses a customizable blend of hydrophobic and hydrophilic surface patterns to help localize microcrystals to defined regions. Microcrystals in their native growth conditions can be loaded into the chips with a standard pipette, allowing data collection at room temperature. Diffraction data collected from hen egg-white lysozyme microcrystals (10–15 µm) loaded into the chips yielded a complete, high-resolution (<1.6 Å) data set sufficient to determine a high-quality structure by molecular replacement. The features of the chip allow the rapid and user-friendly analysis of microcrystals grown under virtually any laboratory format at microfocus synchrotron beamlines and XFELs. PMID:26457423

Investigation of phase evolution of CaCu{sub 3}Ti{sub 4}O{sub 12} (CCTO) by in situ synchrotron high-temperature powder diffraction

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

Ouyang, Xin; Huang, Saifang; School of Materials Science and Technology, China University of Geosciences

2014-03-15

In situ synchrotron X-ray powder diffraction was used to study the high-temperature phase evolution of CaCu{sub 3}Ti{sub 4}O{sub 12} (CCTO) precursors prepared via solid-state and sol–gel methods. After the precursors are heated to 1225 °C, the CCTO phase is the main phase observed in the calcined powder, with the presence of some minor impurities. Comparing the two precursors, we found that the onset temperature for the CCTO phase formation is 800 °C in the sol–gel precursor, lower than that in the solid-state precursor (875 °C). Intermediate phases were only observed in the sol–gel precursor. Both precursors are able to bemore » calcined to sub-micrometric sized powders. Based on the synchrotron data along with differential scanning calorimetry (DSC) and thermal gravimetric analysis (TGA), the phase formation sequence and mechanism during calcination are proposed in this study. -- Graphical abstract: The in situ synchrotron HT-XRD patterns of CCTO sol–gel and solid-state precursor. Highlights: • Phase formation sequence/mechanism in two CCTO precursors has been established. • Formation temperature of CCTO via sol–gel method is lower than solid-state method. • Intermediate phases are only observed in the sol–gel precursor. • Both precursors are able to be calcined into sub-micrometric sized powders.« less

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

Synchrotron Study on Crystallization Kinetics of Milk Fat under Shear Flow

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

Mazzanti, G.; Marangoni, A; Idziak, S

A detailed synchrotron X-ray diffraction study on the kinetics of crystallization of anhydrous milk fat (AMF) and milk fat triacylglycerols (MFT) was done in a Couette cell at 17 C, 17.5 C and 20 C under shear rates between 0 and 2880 s-1. We observed shear-induced acceleration of the transition from phase ? to ?? and the presence of crystalline orientation, but no effect of shear on the onset time of phase ? was observed. A two stage regime was observed for the growth of phase ??. The first stage follows a series-parallel system of differential equations describing the conversionmore » between liquid and crystalline phases. The second stage follows a diffusion-controlled regime. These mechanisms are consistent with the crystalline orientation, the growth of the crystalline domains and the observed displacement of the diffraction peak positions. The absence of the polar lipids explains the faster kinetics of MFT.« 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.

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

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

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

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.

Metrology of variable-line-spacing x-ray gratings using the APS Long Trace Profiler

NASA Astrophysics Data System (ADS)

Sheung, Janet; Qian, Jun; Sullivan, Joseph; Thomasset, Muriel; Manton, Jonathan; Bean, Sunil; Takacs, Peter; Dvorak, Joseph; Assoufid, Lahsen

2017-09-01

As resolving power targets have increased with each generation of beamlines commissioned in synchrotron radiation facilities worldwide, diffraction gratings are quickly becoming crucial optical components for meeting performance targets. However, the metrology of variable-line-spacing (VLS) gratings for high resolution beamlines is not widespread; in particular, no metrology facility at any US DOE facility is currently equipped to fully characterize such gratings. To begin to address this issue, the Optics Group at the Advanced Photon Source at Argonne, in collaboration with SOLEIL and with support from Brookhaven National Laboratory (BNL), has developed an alternative beam path addition to the Long Trace Profiler (LTP) at Argonne's Advanced Photon Source. This significantly expands the functionality of the LTP not only to measure mirrors surface slope profile at normal incidence, but also to characterize the groove density of VLS diffraction gratings in the Littrow incidence up to 79°, which covers virtually all diffraction gratings used at synchrotrons in the first order. The LTP light source is a 20mW HeNe laser, which yields enough signal for diffraction measurements to be performed on low angle blazed gratings optimized for soft X-ray wavelengths. We will present the design of the beam path, technical requirements for the optomechanics, and our data analysis procedure. Finally, we discuss challenges still to be overcome and potential limitations with use of the LTP to perform metrology on diffraction gratings.

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.

Puzzling Intergrowth in Cerium Nitridophosphate Unraveled by Joint Venture of Aberration-Corrected Scanning Transmission Electron Microscopy and Synchrotron Diffraction.

PubMed

Kloß, Simon D; Neudert, Lukas; Döblinger, Markus; Nentwig, Markus; Oeckler, Oliver; Schnick, Wolfgang

2017-09-13

Thorough investigation of nitridophosphates has rapidly accelerated through development of new synthesis strategies. Here we used the recently developed high-pressure metathesis to prepare the first rare-earth metal nitridophosphate, Ce 4 Li 3 P 18 N 35 , with a high degree of condensation >1/2. Ce 4 Li 3 P 18 N 35 consists of an unprecedented hexagonal framework of PN 4 tetrahedra and exhibits blue luminescence peaking at 455 nm. Transmission electron microscopy (TEM) revealed two intergrown domains with slight structural and compositional variations. One domain type shows extremely weak superstructure phenomena revealed by atomic-resolution scanning TEM (STEM) and single-crystal diffraction using synchrotron radiation. The corresponding superstructure involves a modulated displacement of Ce atoms in channels of tetrahedra 6-rings. The displacement model was refined in a supercell as well as in an equivalent commensurate (3 + 2)-dimensional description in superspace group P6 3 (α, β, 0)0(-α - β, α, 0)0. In the second domain type, STEM revealed disordered vacancies of the same Ce atoms that were modulated in the first domain type, leading to sum formula Ce 4-0.5x Li 3 P 18 N 35-1.5x O 1.5x (x ≈ 0.72) of the average structure. The examination of these structural intricacies may indicate the detection limit of synchrotron diffraction and TEM. We discuss the occurrence of either Ce displacements or Ce vacancies that induce the incorporation of O as necessary stabilization of the crystal structure.

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

In pursuit of the rhabdophane crystal structure: from the hydrated monoclinic LnPO{sub 4}.0.667H{sub 2}O to the hexagonal LnPO{sub 4} (Ln = Nd, Sm, Gd, Eu and Dy)

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

Mesbah, Adel, E-mail: adel.mesbah@cea.fr; Clavier, Nicolas; Elkaim, Erik

The dehydration process of the hydrated rhabdophane LnPO{sub 4}.0.667H{sub 2}O (Ln = La to Dy) was thoroughly studied over the combination of in situ high resolution synchrotron powder diffraction and TGA experiments. In the case of SmPO{sub 4}.0.667H{sub 2}O (monoclinic, C2), a first dehydration step was identified around 80 °C leading to the formation of SmPO{sub 4}.0.5H{sub 2}O (Monoclinic, C2) with Z =12 and a =17.6264(1) Å, b =6.9704(1) Å, c =12.1141(1) Å, β=133.74(1) °, V =1075.33(1) Å{sup 3}. In agreement with the TGA and dilatometry experiments, all the water molecules were evacuated above 220 °C yielding to the anhydrousmore » form, which crystallizes in the hexagonal P3{sub 1}21 space group with a =7.0389(1) Å, c =6.3702(1) Å and V =273.34(1) Å{sup 3}. This study was extended to selected LnPO{sub 4}.0.667H{sub 2}O samples (Ln= Nd, Gd, Eu, Dy) and the obtained results confirmed the existence of two dehydration steps before the stabilization of the anhydrous form, with the transitory formation of LnPO{sub 4}.0.5H{sub 2}O. - Graphical abstract: The dehydration process of the rhabdophane SmPO{sub 4}.0.667H{sub 2}O was studied over combination of in situ high resolution synchrotron powder diffraction and TGA techniques, a first dehydration was identified around 80 °C leading to the formation of SmPO{sub 4}.0.5H{sub 2}O (Monoclinic, C2). Then above 220 °C, the anhydrous form of the rhabdophane SmPO{sub 4} was stabilized and crystallizes in the hexagonal P3{sub 1}21 space group. - Highlights: • In situ synchrotron powder diffraction was carried out during the dehydration of the rhabdopahe LnPO{sub 4}.0.667H{sub 2}O. • The heat of the rhabdophane LnPO{sub 4}.0.667H{sub 2}O leads to LnPO{sub 4}.0.5H{sub 2}O then to anhydrous rhabdophane LnPO{sub 4}. • LnPO{sub 4}.0.5H{sub 2}O (monoclinic, C2) and LnPO{sub 4} (Hexagonal, P3{sub 1}21) were solved over the use of direct methods.« less

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.

Diffraction studies of the high pressure phases of GaAs and GaP

NASA Technical Reports Server (NTRS)

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

1982-01-01

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

A new XUV optical end-station to characterize compact and flexible photonic devices using synchrotron radiation

NASA Astrophysics Data System (ADS)

Marcelli, A.; Mazuritskiy, M. I.; Dabagov, S. B.; Hampai, D.; Lerer, A. M.; Izotova, E. A.; D'Elia, A.; Turchini, S.; Zema, N.; Zuccaro, F.; de Simone, M.; Javad Rezvani, S.; Coreno, M.

2018-03-01

In this contribution we present the new experimental end-station to characterize XUV diffractive optics, such as Micro Channel Plates (MCPs) and other polycapillary optics, presently under commission at the Elettra synchrotron radiation laboratory (Trieste, Italy). To show the opportunities offered by these new optical devices for 3rd and 4th generation radiation sources, in this work we present also some patterns collected at different energies of the primary XUV radiation transmitted by MCP optical devices working in the normal incidence geometry.

Acoustic emissions monitoring and synchrotron X-ray diffraction analysis of mineral dehydrations at high pressures and temperatures

NASA Astrophysics Data System (ADS)

Gasc, J.; Guillon, S.; Schubnel, A. J.; Brunet, F.; Lathe, C.; Mueller, H.

2009-12-01

We have monitored from in-situ X-ray diffraction coupled to Acoustic Emission (AE) imaging, the behavior of several materials under elevated pressures and temperatures (quartz, kaolinite, serpentinite). The samples were placed in a boron-epoxy assembly with an 8mm edge-length and loaded in the MAX80 cubic multi-anvil press installed on the German synchrotron (HASYLAB-DESY, Hamburg). AE were recorded using six piezoceramic transducers (2 MHz eigen frequency) glued on each of the six WC anvils. Full waveforms were acquired using an eight channel digital oscilloscope and a continuous acoustic recorder. Our system was first tested using quartz beads (500μm) aggregates. During cold compression performed on these samples many acoustic events were recorded and located inside the samples. These are obviously related to the fragile fracturing of the quartz due to the porosity loss. During the heating cycles performed on the same samples, the acoustic activity progressively vanishes between 300 and 400°C indicating the transition to the ductile regime towards higher temperatures. Further experiments were performed by mixing 20wt% of kaolinite to the quartz. As a result, the amount of acoustic emissions recorded during cold compression is significantly reduced. This is thought to be a result of the ductile behaviour of kaolinite even at low temperatures. This assumption has been confirmed by performing experiments on pure kaolinite which did not produce acoustic emissions during cold compression nor during heating cycles up to 1000°C (i.e. beyond the kaolinite dehydration temperature). This set of experiments clearly established that no acoustic activity is produced by the assembly and that AEs produced by the samples are accurately located by the software. The behaviour of serpentinite dehydration was then investigated under various pressure conditions (i.e. various volume changes), from ~0.6 to ~40kbars. These experiments were performed under deviatoric stress conditions by using Al2O3 waveguides. While clearly identified with the time resolved diffraction patterns, the dehydration process did not produce any AE, at least within the sensitivity and frequency ranges of our transducers. The microstructures observed on the recovered samples by SEM show features characteristic of fluid localisation and/or migration and highlight the fact that fractures were activated prior, during and after mineral dehydration. These results tend to show that the relationship between mineral dehydration, acoustic emission production, earthquakes and fracturing are not as straightforward as one could expect under high pressure and temperature conditions.

Acoustic emissions monitoring and synchrotron X-ray diffraction analysis of mineral dehydrations at high pressures and temperatures

NASA Astrophysics Data System (ADS)

Schubnel, Alexandre; Julien, Gasc; Sophie, Guillon; Fabrice, Brunet; Christian, Lathe; Hans-Joachim, Mueller

2010-05-01

We have monitored from in-situ X-ray diffraction coupled to Acoustic Emission (AE) imaging, the behavior of several materials under elevated pressures and temperatures (quartz, kaolinite, serpentinite). The samples were placed in a boron-epoxy assembly with an 8mm edge-length and loaded in the MAX80 cubic multi-anvil press installed on the German synchrotron (HASYLAB-DESY, Hamburg). AE were recorded using six piezoceramic transducers (2 MHz eigen frequency) glued on each of the six WC anvils. Full waveforms were acquired using an eight channel digital oscilloscope and a continuous acoustic recorder. Our system was first tested using quartz beads (500μm) aggregates. During cold compression performed on these samples many acoustic events were recorded and located inside the samples. These are obviously related to the fragile fracturing of the quartz due to the porosity loss. During the heating cycles performed on the same samples, the acoustic activity progressively vanishes between 300 and 400°C indicating the transition to the ductile regime towards higher temperatures. Further experiments were performed by mixing 20wt% of kaolinite to the quartz. As a result, the amount of acoustic emissions recorded during cold compression is significantly reduced. This is thought to be a result of the ductile behaviour of kaolinite even at low temperatures. This assumption has been confirmed by performing experiments on pure kaolinite which did not produce acoustic emissions during cold compression nor during heating cycles up to 1000°C (i.e. beyond the kaolinite dehydration temperature). This set of experiments clearly established that no acoustic activity is produced by the assembly and that AEs produced by the samples are accurately located by the software. The behaviour of serpentinite dehydration was then investigated under various pressure conditions (i.e. various volume changes), from ~0.6 to ~40kbars. These experiments were performed under deviatoric stress conditions by using Al2O3 waveguides. While clearly identified with the time resolved diffraction patterns, the dehydration process did not produce any AE, at least within the sensitivity and frequency ranges of our transducers. The microstructures observed on the recovered samples by SEM show features characteristic of fluid localisation and/or migration and highlight the fact that fractures were activated prior, during and after mineral dehydration. These results tend to show that the relationship between mineral dehydration, acoustic emission production, earthquakes and fracturing are not as straightforward as one could expect under high pressure and temperature conditions.

In situ synthesis studies of silicon clathrates

NASA Astrophysics Data System (ADS)

Hutchins, Peter Thomas

Solid state clathrates have shown considerable potential as a new class of materials over the past 30 years. Experimental and theoretical studies have shown that precise tuning and synthetic control of these materials, may lead to desirable properties. Very little is known about the mechanism of formation of the clathrates and so the desire to have accurate synthetic control was, until now, unrealistic. This thesis address the problem using in situ synchrotron x-ray techniques. In this study, experiments were designed to utilise time-resolved in situ diffraction techniques and high temperature 23Na NMR, in efforts to understand the mechanism of formation for this class of expanded framework materials. A complex high vacuum capillary synthesis cell was designed for loading under inert conditions and operation under high vacuum at station 6.2 of the SRS Daresbury. The cell was designed to operate in conjunction with a custom made furnace capable of temperatures in excess of 1000 C, as well as a vacuum system capable of 10"5 bar. The clathrate system was studied in situ, using rapid data collection to elucidate the mechanism of formation. The data were analysed using Rietveld methods and showed a structural link between the monoclinic, C2/c, Zintl precursors and the cubic, Pm3n, clathrate I phase. The phases were found to be linked by relation of the sodium planes in the silicide and the sodium atoms resident at cages centres in the clathrate system. This evidence suggests the guest species is instrumental in formation of the clathrate structure by templating the formation of the cages in the structure. Solid state 23Na NMR was utilised to complete specially design experiments, similar to those complete in situ using synchrotron x-ray techniques. The experiments showed increased spherical symmetry of the alkali metal sites and suggested increased mobility of the guest atoms during heating. In addition, cyclic heating experiments using in situ diffraction showed reversible reintroduction of the guest species on heating and cooling, during formation and subsequent dissipation of the clathrate structure. The realisation of the synthesis of a guest free type II clathrate and the theoretical prediction of negative thermal expansion behaviour at low temperature prompted the use of laboratory x-ray diffraction and a liquid helium cryostat to test the prediction. Careful study of the region from 20 to 200 K showed a region of zero or negative thermal expansion in the predicted region the effect observed showed good agreement with theory.

The Upgrade Programme for the Structural Biology beamlines at the European Synchrotron Radiation Facility - High throughput sample evaluation and automation

NASA Astrophysics Data System (ADS)

Theveneau, P.; Baker, R.; Barrett, R.; Beteva, A.; Bowler, M. W.; Carpentier, P.; Caserotto, H.; de Sanctis, D.; Dobias, F.; Flot, D.; Guijarro, M.; Giraud, T.; Lentini, M.; Leonard, G. A.; Mattenet, M.; McCarthy, A. A.; McSweeney, S. M.; Morawe, C.; Nanao, M.; Nurizzo, D.; Ohlsson, S.; Pernot, P.; Popov, A. N.; Round, A.; Royant, A.; Schmid, W.; Snigirev, A.; Surr, J.; Mueller-Dieckmann, C.

2013-03-01

Automation and advances in technology are the key elements in addressing the steadily increasing complexity of Macromolecular Crystallography (MX) experiments. Much of this complexity is due to the inter-and intra-crystal heterogeneity in diffraction quality often observed for crystals of multi-component macromolecular assemblies or membrane proteins. Such heterogeneity makes high-throughput sample evaluation an important and necessary tool for increasing the chances of a successful structure determination. The introduction at the ESRF of automatic sample changers in 2005 dramatically increased the number of samples that were tested for diffraction quality. This "first generation" of automation, coupled with advances in software aimed at optimising data collection strategies in MX, resulted in a three-fold increase in the number of crystal structures elucidated per year using data collected at the ESRF. In addition, sample evaluation can be further complemented using small angle scattering experiments on the newly constructed bioSAXS facility on BM29 and the micro-spectroscopy facility (ID29S). The construction of a second generation of automated facilities on the MASSIF (Massively Automated Sample Screening Integrated Facility) beam lines will build on these advances and should provide a paradigm shift in how MX experiments are carried out which will benefit the entire Structural Biology community.

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

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.

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.

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.

Application of MEMS-based x-ray optics as tuneable nanosecond choppers

NASA Astrophysics Data System (ADS)

Chen, Pice; Walko, Donald A.; Jung, Il Woong; Li, Zhilong; Gao, Ya; Shenoy, Gopal K.; Lopez, Daniel; Wang, Jin

2017-08-01

Time-resolved synchrotron x-ray measurements often rely on using a mechanical chopper to isolate a set of x-ray pulses. We have started the development of micro electromechanical systems (MEMS)-based x-ray optics, as an alternate method to manipulate x-ray beams. In the application of x-ray pulse isolation, we recently achieved a pulse-picking time window of half a nanosecond, which is more than 100 times faster than mechanical choppers can achieve. The MEMS device consists of a comb-drive silicon micromirror, designed for efficiently diffracting an x-ray beam during oscillation. The MEMS devices were operated in Bragg geometry and their oscillation was synchronized to x-ray pulses, with a frequency matching subharmonics of the cycling frequency of x-ray pulses. The microscale structure of the silicon mirror in terms of the curvature and the quality of crystallinity ensures a narrow angular spread of the Bragg reflection. With the discussion of factors determining the diffractive time window, this report showed our approaches to narrow down the time window to half a nanosecond. The short diffractive time window will allow us to select single x-ray pulse out of a train of pulses from synchrotron radiation facilities.

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.

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

The Stanford Automated Mounter: Enabling High-Throughput Protein Crystal Screening at SSRL

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

Smith, C.A.; Cohen, A.E.

2009-05-26

The macromolecular crystallography experiment lends itself perfectly to high-throughput technologies. The initial steps including the expression, purification, and crystallization of protein crystals, along with some of the later steps involving data processing and structure determination have all been automated to the point where some of the last remaining bottlenecks in the process have been crystal mounting, crystal screening, and data collection. At the Stanford Synchrotron Radiation Laboratory, a National User Facility that provides extremely brilliant X-ray photon beams for use in materials science, environmental science, and structural biology research, the incorporation of advanced robotics has enabled crystals to be screenedmore » in a true high-throughput fashion, thus dramatically accelerating the final steps. Up to 288 frozen crystals can be mounted by the beamline robot (the Stanford Auto-Mounting System) and screened for diffraction quality in a matter of hours without intervention. The best quality crystals can then be remounted for the collection of complete X-ray diffraction data sets. Furthermore, the entire screening and data collection experiment can be controlled from the experimenter's home laboratory by means of advanced software tools that enable network-based control of the highly automated beamlines.« less

Mapping the conformational landscape of a dynamic enzyme by multitemperature and XFEL crystallography

PubMed Central

Keedy, Daniel A; Kenner, Lillian R; Warkentin, Matthew; Woldeyes, Rahel A; Hopkins, Jesse B; Thompson, Michael C; Brewster, Aaron S; Van Benschoten, Andrew H; Baxter, Elizabeth L; Uervirojnangkoorn, Monarin; McPhillips, Scott E; Song, Jinhu; Alonso-Mori, Roberto; Holton, James M; Weis, William I; Brunger, Axel T; Soltis, S Michael; Lemke, Henrik; Gonzalez, Ana; Sauter, Nicholas K; Cohen, Aina E; van den Bedem, Henry; Thorne, Robert E; Fraser, James S

2015-01-01

Determining the interconverting conformations of dynamic proteins in atomic detail is a major challenge for structural biology. Conformational heterogeneity in the active site of the dynamic enzyme cyclophilin A (CypA) has been previously linked to its catalytic function, but the extent to which the different conformations of these residues are correlated is unclear. Here we compare the conformational ensembles of CypA by multitemperature synchrotron crystallography and fixed-target X-ray free-electron laser (XFEL) crystallography. The diffraction-before-destruction nature of XFEL experiments provides a radiation-damage-free view of the functionally important alternative conformations of CypA, confirming earlier synchrotron-based results. We monitored the temperature dependences of these alternative conformations with eight synchrotron datasets spanning 100-310 K. Multiconformer models show that many alternative conformations in CypA are populated only at 240 K and above, yet others remain populated or become populated at 180 K and below. These results point to a complex evolution of conformational heterogeneity between 180-–240 K that involves both thermal deactivation and solvent-driven arrest of protein motions in the crystal. The lack of a single shared conformational response to temperature within the dynamic active-site network provides evidence for a conformation shuffling model, in which exchange between rotamer states of a large aromatic ring in the middle of the network shifts the conformational ensemble for the other residues in the network. Together, our multitemperature analyses and XFEL data motivate a new generation of temperature- and time-resolved experiments to structurally characterize the dynamic underpinnings of protein function. DOI: http://dx.doi.org/10.7554/eLife.07574.001 PMID:26422513

Stress Gradient Induced Strain Localization in Metals: High Resolution Strain Cross Sectioning via Synchrotron X-Ray Diffraction (POSTPRINT)

DTIC Science & Technology

2008-04-01

DIFFRACTION (POSTPRINT) M. Croft, N. Jisrawi , Z. Zhong, K. Horvath, R.L. Holtz, M. Shepard, M. Lakshmipathy, K. Sadananda, J. Skaritka, V...5c. PROGRAM ELEMENT NUMBER 62102F 6. AUTHOR(S) M. Croft, N. Jisrawi , K. Horvath, V. Shukla, R.K. Sadangi, and T. Tsakalakos (Rutgers...Upton, NY 11973 N. Jisrawi Materials Science and Engineering Department, Rutgers University, Piscataway, NJ 08854; Department of Basic Sciences

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.

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

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

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

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

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

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.

Experiments with phase transitions at very high pressure. [compressed solidifed gases, semiconductors, superconductors, and molecular crystals

NASA Technical Reports Server (NTRS)

Spain, I. L.

1983-01-01

Diamond cells were constructed for use to 1 Mbar. A refrigerator for cooling diamond cells was adapted for studies between 15 and 300 K. A cryostat for superconductivity studies between 1.5 to 300 K was constructed. Optical equipment was constructed for fluorescence, transmission, and reflectance studies. X-ray equipment was adapted for use with diamond cells. Experimental techniques were developed for X-ray diffraction studies using synchrotron radiation. AC susceptibility techniques were developed for detecting superconducting transitions. The following materials were studied: compressed solidified gases (Xe, Ar), semiconductors (Ge, Si, GaAs), superconductors (Nb3Ge, Nb3Si, Nb3As, CuCl), molecular crystals (I).

{bold {ital In situ}} measurements of texture and phase development in (Bi,Pb){sub 2}Sr{sub 2}Ca{sub 2}Cu{sub 3}O{sub 10}{endash}Ag tapes

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

Thurston, T.R.; Haldar, P.; Wang, Y.L.

Hard x-rays from a synchrotron source were utilized in diffraction experiments performed at elevated temperatures (up to {approximately}870{degree}C) on (Bi,Pb){sub 2}Sr{sub 2}Ca{sub 2}Cu{sub 3}O{sub 10} (Bi-2223) tapes {ital completely} encased in silver. The general behavior of the phase and texture development under typical processing conditions was determined, and the effects that several variations in processing conditions had on the phase and texture development were examined. These results and their implications for improving processing conditions are discussed. {copyright} {ital 1997 Materials Research Society.}

Synchrotron radiation laboratories at the Bonn electron accelerators. a status report

NASA Astrophysics Data System (ADS)

Hormes, J.

1987-07-01

At the Physikalisches Institut of the University in Bonn experiments with synchrotron radiation were carried out ever since 1962. At the moment (June 1986) all work takes place in the SR-laboratory at the 2.5 GeV synchrotron. A 3.5 GeV stretcher ring (ELSA) is under construction and will come into operation at the end of 1986. This accelerator will also run as a storage ring for synchrotron radiation experiments and a laboratory to be used at this machine is also under consideration. The SR experiments which are carried out in Bonn try to take advantage of the fact that we are still using a high energy synchrotron for our work. Besides basic research also applied work is done using synchrotron radiation even as a production tool for X-ray lithography.

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.

Diamond anvils with a round table designed for high pressure experiments in DAC

NASA Astrophysics Data System (ADS)

Dubrovinsky, Leonid; Koemets, Egor; Bykov, Maxim; Bykova, Elena; Aprilis, Georgios; Pakhomova, Anna; Glazyrin, Konstantin; Laskin, Alexander; Prakapenka, Vitali B.; Greenberg, Eran; Dubrovinskaia, Natalia

2017-10-01

Here, we present new Diamond Anvils with a Round Table (DART-anvils) designed for applications in the diamond anvil cell (DAC) technique. The main features of the new DART-anvil design are a spherical shape of both the crown and the table of a diamond and the position of the centre of the culet exactly in the centre of the sphere. The performance of DART-anvils was tested in a number of high pressure high-temperature experiments at different synchrotron beamlines. These experiments demonstrated a number of advantages, which are unavailable with any of the hitherto known anvil designs. Use of DART-anvils enables to realise in situ single-crystal X-ray diffraction experiments with laser heating using stationary laser-heating setups; eliminating flat-plate design of conventional anvils, DART-anvils make the cell alignment easier; working as solid immersion lenses, they provide additional magnification of the sample in a DAC and improve the image resolution.

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.

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 .

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.

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.

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.

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.

High-density grids for efficient data collection from multiple crystals

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

Baxter, Elizabeth L.; Aguila, Laura; Alonso-Mori, Roberto

Higher throughput methods to mount and collect data from multiple small and radiation-sensitive crystals are important to support challenging structural investigations using microfocus synchrotron beamlines. Furthermore, efficient sample-delivery methods are essential to carry out productive femtosecond crystallography experiments at X-ray free-electron laser (XFEL) sources such as the Linac Coherent Light Source (LCLS). To address these needs, a high-density sample grid useful as a scaffold for both crystal growth and diffraction data collection has been developed and utilized for efficient goniometer-based sample delivery at synchrotron and XFEL sources. A single grid contains 75 mounting ports and fits inside an SSRL cassettemore » or uni-puck storage container. The use of grids with an SSRL cassette expands the cassette capacity up to 7200 samples. Grids may also be covered with a polymer film or sleeve for efficient room-temperature data collection from multiple samples. New automated routines have been incorporated into theBlu-Ice/DCSSexperimental control system to support grids, including semi-automated grid alignment, fully automated positioning of grid ports, rastering and automated data collection. Specialized tools have been developed to support crystallization experiments on grids, including a universal adaptor, which allows grids to be filled by commercial liquid-handling robots, as well as incubation chambers, which support vapor-diffusion and lipidic cubic phase crystallization experiments. Experiments in which crystals were loaded into grids or grown on grids using liquid-handling robots and incubation chambers are described. As a result, crystals were screened at LCLS-XPP and SSRL BL12-2 at room temperature and cryogenic temperatures.« less

High-density grids for efficient data collection from multiple crystals

PubMed Central

Baxter, Elizabeth L.; Aguila, Laura; Alonso-Mori, Roberto; Barnes, Christopher O.; Bonagura, Christopher A.; Brehmer, Winnie; Brunger, Axel T.; Calero, Guillermo; Caradoc-Davies, Tom T.; Chatterjee, Ruchira; Degrado, William F.; Fraser, James S.; Ibrahim, Mohamed; Kern, Jan; Kobilka, Brian K.; Kruse, Andrew C.; Larsson, Karl M.; Lemke, Heinrik T.; Lyubimov, Artem Y.; Manglik, Aashish; McPhillips, Scott E.; Norgren, Erik; Pang, Siew S.; Soltis, S. M.; Song, Jinhu; Thomaston, Jessica; Tsai, Yingssu; Weis, William I.; Woldeyes, Rahel A.; Yachandra, Vittal; Yano, Junko; Zouni, Athina; Cohen, Aina E.

2016-01-01

Higher throughput methods to mount and collect data from multiple small and radiation-sensitive crystals are important to support challenging structural investigations using microfocus synchrotron beamlines. Furthermore, efficient sample-delivery methods are essential to carry out productive femtosecond crystallography experiments at X-ray free-electron laser (XFEL) sources such as the Linac Coherent Light Source (LCLS). To address these needs, a high-density sample grid useful as a scaffold for both crystal growth and diffraction data collection has been developed and utilized for efficient goniometer-based sample delivery at synchrotron and XFEL sources. A single grid contains 75 mounting ports and fits inside an SSRL cassette or uni-puck storage container. The use of grids with an SSRL cassette expands the cassette capacity up to 7200 samples. Grids may also be covered with a polymer film or sleeve for efficient room-temperature data collection from multiple samples. New automated routines have been incorporated into the Blu-Ice/DCSS experimental control system to support grids, including semi-automated grid alignment, fully automated positioning of grid ports, rastering and automated data collection. Specialized tools have been developed to support crystallization experiments on grids, including a universal adaptor, which allows grids to be filled by commercial liquid-handling robots, as well as incubation chambers, which support vapor-diffusion and lipidic cubic phase crystallization experiments. Experiments in which crystals were loaded into grids or grown on grids using liquid-handling robots and incubation chambers are described. Crystals were screened at LCLS-XPP and SSRL BL12-2 at room temperature and cryogenic temperatures. PMID:26894529

High-density grids for efficient data collection from multiple crystals

DOE PAGES

Baxter, Elizabeth L.; Aguila, Laura; Alonso-Mori, Roberto; ...

2015-11-03

Higher throughput methods to mount and collect data from multiple small and radiation-sensitive crystals are important to support challenging structural investigations using microfocus synchrotron beamlines. Furthermore, efficient sample-delivery methods are essential to carry out productive femtosecond crystallography experiments at X-ray free-electron laser (XFEL) sources such as the Linac Coherent Light Source (LCLS). To address these needs, a high-density sample grid useful as a scaffold for both crystal growth and diffraction data collection has been developed and utilized for efficient goniometer-based sample delivery at synchrotron and XFEL sources. A single grid contains 75 mounting ports and fits inside an SSRL cassettemore » or uni-puck storage container. The use of grids with an SSRL cassette expands the cassette capacity up to 7200 samples. Grids may also be covered with a polymer film or sleeve for efficient room-temperature data collection from multiple samples. New automated routines have been incorporated into theBlu-Ice/DCSSexperimental control system to support grids, including semi-automated grid alignment, fully automated positioning of grid ports, rastering and automated data collection. Specialized tools have been developed to support crystallization experiments on grids, including a universal adaptor, which allows grids to be filled by commercial liquid-handling robots, as well as incubation chambers, which support vapor-diffusion and lipidic cubic phase crystallization experiments. Experiments in which crystals were loaded into grids or grown on grids using liquid-handling robots and incubation chambers are described. As a result, crystals were screened at LCLS-XPP and SSRL BL12-2 at room temperature and cryogenic temperatures.« less

Refinement of pressure calibration for multi-anvil press experiments

NASA Astrophysics Data System (ADS)

Ono, S.

2016-12-01

Accurate characterization of the pressure and temperature environment in high-pressure apparatuses is of essential importance when we apply laboratory data to the study of the Earth's interior. Recently, the synchrotron X-ray source can be used for the high-pressure experiments, and the in situ pressure calibration has been a common technique. However, this technique cannot be used in the laboratory-based experiments. Even now, the conventional pressure calibration is of great interest to understand the Earth's interior. Several high-pressure phase transitions used as the pressure calibrants in the laboratory-based multi-anvil experiments have been investigated. Precise determinations of phase boundaries of CaGeO3 [1], Fe2SiO4 [2], SiO2, and Zr [3] were performed by the multi-anvil press or the diamond anvil cell apparatuses combined with the synchrotron X-ray diffraction technique. The transition pressures in CaGeO3 (garnet-perovskite), Fe2SiO4 (alfa-gamma), and SiO2 (coesite-stishovite) were in general agreement with those reported by previous studies. However, significant discrepancies for the slopes, dP/dT, of these transitions between our and previous studies were confirmed. In the case of Zr study [3], our experimental results elucidate the inconsistency in the transition pressure between omega and beta phase in Zr observed in previous studies. [1] Ono et al. (2011) Phys. Chem. Minerals, 38, 735-740.[2] Ono et al. (2013) Phys. Chem. Minerals, 40, 811-816.[3] Ono & Kikegawa (2015) J. Solid State Chem., 225, 110-113.

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

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

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.

Facilities for small-molecule crystallography at synchrotron sources.

PubMed

Barnett, Sarah A; Nowell, Harriott; Warren, Mark R; Wilcox, Andrian; Allan, David R

2016-01-01

Although macromolecular crystallography is a widely supported technique at synchrotron radiation facilities throughout the world, there are, in comparison, only very few beamlines dedicated to small-molecule crystallography. This limited provision is despite the increasing demand for beamtime from the chemical crystallography community and the ever greater overlap between systems that can be classed as either small macromolecules or large small molecules. In this article, a very brief overview of beamlines that support small-molecule single-crystal diffraction techniques will be given along with a more detailed description of beamline I19, a dedicated facility for small-molecule crystallography at Diamond Light Source.

Inclined monochromator for high heat-load synchrotron x-ray radiation

DOEpatents

Khounsary, A.M.

1994-02-15

A double crystal monochromator is described including two identical, parallel crystals, each of which is cut such that the normal to the diffraction planes of interest makes an angle less than 90 degrees with the surface normal. Diffraction is symmetric, regardless of whether the crystals are symmetrically or asymmetrically cut, enabling operation of the monochromator with a fixed plane of diffraction. As a result of the inclination of the crystal surface, an incident beam has a footprint area which is elongated both vertically and horizontally when compared to that of the conventional monochromator, reducing the heat flux of the incident beam and enabling more efficient surface cooling. Because after inclination of the crystal only a fraction of thermal distortion lies in the diffraction plane, slope errors and the resultant misorientation of the diffracted beam are reduced. 11 figures.

Inclined monochromator for high heat-load synchrotron x-ray radiation

DOEpatents

Khounsary, Ali M.

1994-01-01

A double crystal monochromator including two identical, parallel crystals, each of which is cut such that the normal to the diffraction planes of interest makes an angle less than 90 degrees with the surface normal. Diffraction is symmetric, regardless of whether the crystals are symmetrically or asymmetrically cut, enabling operation of the monochromator with a fixed plane of diffraction. As a result of the inclination of the crystal surface, an incident beam has a footprint area which is elongated both vertically and horizontally when compared to that of the conventional monochromator, reducing the heat flux of the incident beam and enabling more efficient surface cooling. Because after inclination of the crystal only a fraction of thermal distortion lies in the diffraction plane, slope errors and the resultant misorientation of the diffracted beam are reduced.

Preparation and Delivery of Protein Microcrystals in Lipidic Cubic Phase for Serial Femtosecond Crystallography.

PubMed

Ishchenko, Andrii; Cherezov, Vadim; Liu, Wei

2016-09-20

Membrane proteins (MPs) are essential components of cellular membranes and primary drug targets. Rational drug design relies on precise structural information, typically obtained by crystallography; however MPs are difficult to crystallize. Recent progress in MP structural determination has benefited greatly from the development of lipidic cubic phase (LCP) crystallization methods, which typically yield well-diffracting, but often small crystals that suffer from radiation damage during traditional crystallographic data collection at synchrotron sources. The development of new-generation X-ray free-electron laser (XFEL) sources that produce extremely bright femtosecond pulses has enabled room temperature data collection from microcrystals with no or negligible radiation damage. Our recent efforts in combining LCP technology with serial femtosecond crystallography (LCP-SFX) have resulted in high-resolution structures of several human G protein-coupled receptors, which represent a notoriously difficult target for structure determination. In the LCP-SFX technique, LCP is recruited as a matrix for both growth and delivery of MP microcrystals to the intersection of the injector stream with an XFEL beam for crystallographic data collection. It has been demonstrated that LCP-SFX can substantially improve the diffraction resolution when only sub-10 µm crystals are available, or when the use of smaller crystals at room temperature can overcome various problems associated with larger cryocooled crystals, such as accumulation of defects, high mosaicity and cryocooling artifacts. Future advancements in X-ray sources and detector technologies should make serial crystallography highly attractive and practicable for implementation not only at XFELs, but also at more accessible synchrotron beamlines. Here we present detailed visual protocols for the preparation, characterization and delivery of microcrystals in LCP for serial crystallography experiments. These protocols include methods for conducting crystallization experiments in syringes, detecting and characterizing the crystal samples, optimizing crystal density, loading microcrystal laden LCP into the injector device and delivering the sample to the beam for data collection.

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

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.

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

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

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

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

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

DOE PAGES

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

2016-04-07

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

Diffraction-limited IR Microspectroscopy with IRENI

Treesearch

J. Sedlmair; B. Illman; M. Unger; C. Hirschmugl

2012-01-01

In a unique way, IRENI (Infrared environmental Imaging), operated at the Synchrotron Radiation Center in Madison, combines IR spectroscopy and IR imaging, revealing the chemical morphology of a sample. Most storage ring based IR confocal microscopes have to overcome a trade-off between spatial resolution versus...

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

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

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

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.

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.

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

Protein crystallography beamline BL2S1 at the Aichi synchrotron

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

Watanabe, Nobuhisa; Nagae, Takayuki; Yamada, Yusuke

The protein crystallography beamline BL2S1, constructed at one of the 5 T superconducting bending-magnet ports of the Aichi synchrotron, is available to users associated with academic and industrial organizations. The beamline is mainly intended for use in X-ray diffraction measurements of single-crystals of macromolecules such as proteins and nucleic acids. Diffraction measurements for crystals of other materials are also possible, such as inorganic and organic compounds. BL2S1 covers the energy range 7–17 keV (1.8–0.7 Å) with an asymmetric-cut curved single-crystal monochromator [Ge(111) or Ge(220)], and a platinum-coated Si mirror is used for vertical focusing and as a higher-order cutoff filter.more » The beamline is equipped with a single-axis goniometer, a CCD detector, and an open-flow cryogenic sample cooler. Lastly, high-pressure protein crystallography with a diamond anvil cell can also be performed using this beamline.« less

Protein crystallography beamline BL2S1 at the Aichi synchrotron.

PubMed

Watanabe, Nobuhisa; Nagae, Takayuki; Yamada, Yusuke; Tomita, Ayana; Matsugaki, Naohiro; Tabuchi, Masao

2017-01-01

The protein crystallography beamline BL2S1, constructed at one of the 5 T superconducting bending-magnet ports of the Aichi synchrotron, is available to users associated with academic and industrial organizations. The beamline is mainly intended for use in X-ray diffraction measurements of single-crystals of macromolecules such as proteins and nucleic acids. Diffraction measurements for crystals of other materials are also possible, such as inorganic and organic compounds. BL2S1 covers the energy range 7-17 keV (1.8-0.7 Å) with an asymmetric-cut curved single-crystal monochromator [Ge(111) or Ge(220)], and a platinum-coated Si mirror is used for vertical focusing and as a higher-order cutoff filter. The beamline is equipped with a single-axis goniometer, a CCD detector, and an open-flow cryogenic sample cooler. High-pressure protein crystallography with a diamond anvil cell can also be performed using this beamline.

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

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.

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.

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

Marçal, D.; Rego, A. T.; Fogg, M. J.

1,3-Propanediol dehydrogenase from K. pneumoniae has been overexpressed in E. coli, purified and crystallized. Diffraction data have been collected to 2.7 Å resolution. 1,3-Propanediol dehydrogenase (1,3-PD-DH), encoded by the dhaT gene, is a key enzyme in the dissimilation process for converting glycerol to 1,3-propanediol in the human pathogen Klebsiella pneumoniae. Single colourless crystals were obtained from a recombinant preparation of 1,3-propanediol dehydrogenase overexpressed in Escherichia coli. The crystals belong to space group P2{sub 1}, with unit-cell parameters a = 91.9, b = 226.6, c = 232.6 Å, β = 92.9°. The crystals probably contain two decamers in the asymmetric unit,more » with a V{sub M} value of 3.07 Å{sup 3} Da{sup −1} and an estimated solvent content of 59%. Diffraction data were collected to 2.7 Å resolution using synchrotron radiation at the ID14-4 beamline of the European Synchrotron Radiation Facility.« less

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.

Density Determination of Metallic Melts from Diffuse X-Ray Scattering

NASA Astrophysics Data System (ADS)

Brauser, N.; Davis, A.; Greenberg, E.; Prakapenka, V. B.; Campbell, A.

2017-12-01

Liquids comprise several important structural components of the deep Earth, for example, the present outer core and a hypothesized magma ocean early in Earth history. However, the physical properties of the constituent materials of these structures at high pressures and temperatures are less well constrained than their crystalline counterparts. Determination of the physical properties of these liquids can inform geophysical models of the composition and structure of the Earth, but methods for studying the physical properties of liquids at high pressure and temperatures are underdeveloped. One proposed method for direct determination of density of a melt requires analysis of the diffuse scattered X-ray signal of the liquid. Among the challenges to applying this technique to high-pressure melts within a laser heated diamond anvil cell are the low signal-to-noise ratio and overlapping diffraction peaks from the crystalline components of the sample assembly interfering with the diffuse scattering from the liquid. Recent advances in instrumentation at synchrotron X-ray sources have made this method more accessible for determination of density of melted material. In this work we present the technique and report the densities of three high-pressure melts of the FCC metals iron, nickel, and gold derived from diffuse scattered X-ray spectra collected from in situ laser-heated diamond anvil cell synchrotron experiments. The results are compared to densities derived from shock wave experiments.

GeoSoilEnviroCARS: A National User Facility for Synchrotron Radiation Research

NASA Astrophysics Data System (ADS)

Rivers, M. L.; Sutton, S. R.

2002-12-01

GeoSoilEnviroCARS (GSECARS) is a national user facility for frontier research in the earth sciences using synchrotron radiation at the Advanced Photon Source, Argonne National Laboratory. GSECARS provides earth scientists with access to the high-brilliance hard x-rays from this third-generation synchrotron light source. Both an undulator and a bending magnet beamline are available. All principal synchrotron-based analytical techniques in demand by earth scientists are being brought to bear on earth science problems: (1) high-pressure/high-temperature crystallography and spectroscopy using the diamond anvil cell; (2) high-pressure/high-temperature crystallography using the large-volume press; (3) powder, single crystal and interface diffraction; (4) inelastic x-ray scattering; (5) x-ray absorption fine structure (XAFS) spectroscopy; (6) x-ray fluorescence microprobe analysis; and (7) microtomography. The major instrumentation includes 250 and 1000 MN multianvil presses, a double-sided laser heating system, a large general-purpose 5-circle diffractometer, a focused microprobe, and a Raman laboratory. A proposal-based system for beamtime allocation, open to all earth scientists, has been in place since Fall, 1998. Since then, over 450 beamtime proposals have been received and more than 320 outside users have conducted experiments at GSECARS. The research conducted by these investigators has resulted in more than 170 publications. The unique capabilities of the APS and GSECARS have allowed groundbreaking experiments to be conducted. These include: (1) phase transformations in the Mg-Si-O system at mantle conditions; (2) structure of hydrated a-Al2O3 surfaces; (3) alloying properties of silicon in the Earth's core; (4) dynamics of iron-rich melt segregation from silicates during core formation; (5) electronic spin state of FeO at high pressure and temperature; (6) elastic wave velocities of mantle minerals at lower mantle conditions; (7) copper partitioning and speciation in natural hydrothermal fluids; and (8) mechanisms of arsenic sequestration at a Superfund site. The GSECARS mission is to provide a research environment where users receive expert assistance in planning and conducting experiments, and in analyzing data. The facility operation is funded by the NSF EAR Instrumentation and Facilities program and the DOE Geosciences program. Major instrumentation was also provided by the W.M. Keck Foundation. Information and applications for beam time can be found at http://gsecars.org.

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

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.

Advanced Structural Analyses by Third Generation Synchrotron Radiation Powder Diffraction

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

Sakata, M.; Aoyagi, S.; Ogura, T.

2007-01-19

Since the advent of the 3rd generation Synchrotron Radiation (SR) sources, such as SPring-8, the capabilities of SR powder diffraction increased greatly not only in an accurate structure refinement but also ab initio structure determination. In this study, advanced structural analyses by 3rd generation SR powder diffraction based on the Large Debye-Scherrer camera installed at BL02B2, SPring-8 is described. Because of high angular resolution and high counting statistics powder data collected at BL02B2, SPring-8, ab initio structure determination can cope with a molecular crystals with 65 atoms including H atoms. For the structure refinements, it is found that a kindmore » of Maximum Entropy Method in which several atoms are omitted in phase calculation become very important to refine structural details of fairy large molecule in a crystal. It should be emphasized that until the unknown structure is refined very precisely, the obtained structure by Genetic Algorithm (GA) or some other ab initio structure determination method using real space structural knowledge, it is not possible to tell whether the structure obtained by the method is correct or not. In order to determine and/or refine crystal structure of rather complicated molecules, we cannot overemphasize the importance of the 3rd generation SR sources.« less

Asymmetry in serial femtosecond crystallography data.

PubMed

Sharma, Amit; Johansson, Linda; Dunevall, Elin; Wahlgren, Weixiao Y; Neutze, Richard; Katona, Gergely

2017-03-01

Serial crystallography is an increasingly important approach to protein crystallography that exploits both X-ray free-electron laser (XFEL) and synchrotron radiation. Serial crystallography recovers complete X-ray diffraction data by processing and merging diffraction images from thousands of randomly oriented non-uniform microcrystals, of which all observations are partial Bragg reflections. Random fluctuations in the XFEL pulse energy spectrum, variations in the size and shape of microcrystals, integrating over millions of weak partial observations and instabilities in the XFEL beam position lead to new types of experimental errors. The quality of Bragg intensity estimates deriving from serial crystallography is therefore contingent upon assumptions made while modeling these data. Here it is observed that serial femtosecond crystallography (SFX) Bragg reflections do not follow a unimodal Gaussian distribution and it is recommended that an idealized assumption of single Gaussian peak profiles be relaxed to incorporate apparent asymmetries when processing SFX data. The phenomenon is illustrated by re-analyzing data collected from microcrystals of the Blastochloris viridis photosynthetic reaction center and comparing these intensity observations with conventional synchrotron data. The results show that skewness in the SFX observations captures the essence of the Wilson plot and an empirical treatment is suggested that can help to separate the diffraction Bragg intensity from the background.

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).

Investigation of the Microstructure Evolution in a Fe-17Mn-1.5Al-0.3C Steel via In Situ Synchrotron X-ray Diffraction during a Tensile Test

PubMed Central

Song, Wenwen; Bleck, Wolfgang

2017-01-01

The quantitative characterization of the microstructure evolution in high-Mn steel during deformation is of great importance to understanding its strain-hardening behavior. In the current study, in situ high-energy synchrotron X-ray diffraction was employed to characterize the microstructure evolution in a Fe-17Mn-1.5Al-0.3C steel during a tensile test. The microstructure at different engineering strain levels—in terms of ε-martensite and α’-martensite volume fractions, the stacking fault probability, and the twin fault probability—was analyzed by the Rietveld refinement method. The Fe-17Mn-1.5Al-0.3C steel exhibits a high ultimate tensile strength with a superior uniform elongation and a high strain-hardening rate. The remaining high strain-hardening rate at the strain level about 0.025 to 0.35 results from ε-martensite dominant transformation-induced-plasticity (TRIP) effect. The increase in the strain-hardening rate at the strain level around 0.35 to 0.43 is attributed to the synergetic α’-martensite dominant TRIP and twinning-induced-plasticity (TWIP) effects. An evaluation of the stacking fault energy (SFE) of the Fe-17Mn-1.5Al-0.3C steel by the synchrotron measurements shows good agreement with the thermodynamic calculation of the SFE. PMID:28946692

Investigation of the Microstructure Evolution in a Fe-17Mn-1.5Al-0.3C Steel via In Situ Synchrotron X-ray Diffraction during a Tensile Test.

PubMed

Ma, Yan; Song, Wenwen; Bleck, Wolfgang

2017-09-25

The quantitative characterization of the microstructure evolution in high-Mn steel during deformation is of great importance to understanding its strain-hardening behavior. In the current study, in situ high-energy synchrotron X-ray diffraction was employed to characterize the microstructure evolution in a Fe-17Mn-1.5Al-0.3C steel during a tensile test. The microstructure at different engineering strain levels-in terms of ε-martensite and α'-martensite volume fractions, the stacking fault probability, and the twin fault probability-was analyzed by the Rietveld refinement method. The Fe-17Mn-1.5Al-0.3C steel exhibits a high ultimate tensile strength with a superior uniform elongation and a high strain-hardening rate. The remaining high strain-hardening rate at the strain level about 0.025 to 0.35 results from ε-martensite dominant transformation-induced-plasticity (TRIP) effect. The increase in the strain-hardening rate at the strain level around 0.35 to 0.43 is attributed to the synergetic α'-martensite dominant TRIP and twinning-induced-plasticity (TWIP) effects. An evaluation of the stacking fault energy (SFE) of the Fe-17Mn-1.5Al-0.3C steel by the synchrotron measurements shows good agreement with the thermodynamic calculation of the SFE.

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 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.

High-pressure structural, elastic, and electronic properties of the scintillator host material KMgF3

NASA Astrophysics Data System (ADS)

Vaitheeswaran, G.; Kanchana, V.; Kumar, Ravhi S.; Cornelius, A. L.; Nicol, M. F.; Svane, A.; Delin, A.; Johansson, B.

2007-07-01

The high-pressure structural behavior of the fluoroperovskite KMgF3 is investigated by theory and experiment. Density functional calculations were performed within the local density approximation and the generalized gradient approximation for exchange and correlation effects, as implemented within the full-potential linear muffin-tin orbital method. In situ high-pressure powder x-ray diffraction experiments were performed up to a maximum pressure of 40GPa using synchrotron radiation. We find that the cubic Pm3¯m crystal symmetry persists throughout the pressure range studied. The calculated ground state properties—the equilibrium lattice constant, bulk modulus, and elastic constants—are in good agreement with experimental results. By analyzing the ratio between the bulk and shear moduli, we conclude that KMgF3 is brittle in nature. Under ambient conditions, KMgF3 is found to be an indirect gap insulator, with the gap increasing under pressure.

From Biomass-Derived Furans to Aromatics with Ethanol over Zeolite.

PubMed

Teixeira, Ivo F; Lo, Benedict T W; Kostetskyy, Pavlo; Stamatakis, Michail; Ye, Lin; Tang, Chiu C; Mpourmpakis, Giannis; Tsang, Shik Chi Edman

2016-10-10

We report a novel catalytic conversion of biomass-derived furans and alcohols to aromatics over zeolite catalysts. Aromatics are formed via Diels-Alder cycloaddition with ethylene, which is produced in situ from ethanol dehydration. The use of liquid ethanol instead of gaseous ethylene, as the source of dienophile in this one-pot synthesis, makes the aromatics production much simpler and renewable, circumventing the use of ethylene at high pressure. More importantly, both our experiments and theoretical studies demonstrate that the use of ethanol instead of ethylene, results in significantly higher rates and higher selectivity to aromatics, due to lower activation barriers over the solid acid sites. Synchrotron-diffraction experiments and proton-affinity calculations clearly suggest that a preferred protonation of ethanol over the furan is a key step facilitating the Diels-Alder and dehydration reactions in the acid sites of the zeolite. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Titan's Lakes in a Beaker

NASA Astrophysics Data System (ADS)

Hodyss, R. P.

2017-12-01

The surface of Titan presents a complex, varied surfaced, with mountains, plains, dunes, rivers, lakes and seas, composed of a layer of organics over a water ice bedrock. Over the past 10 years, our group at JPL has developed a variety of techniques to study the chemistry of Titan's organic surface under relevant temperature and pressure conditions (90-100 K, 1.5 bar). Dissolution, precipitation, and both covalent and non-covalent chemical processes are examined using Raman and infrared spectroscopy, mass spectrometry, optical microscopy, and synchrotron X-ray powder diffraction. Despite the low temperatures, our experiments are revealing that a rich and active organic chemistry is possible on Titan's surface. Laboratory experiments like these can provide crucial insights into the geological processes occurring Titan's surface, and help explain the wealth of observational data returned by the Cassini/Huygens mission. This type of data is also critical for the development of future missions to Titan.

Auto-rickshaw: an automated crystal structure determination platform as an efficient tool for the validation of an X-ray diffraction experiment.

PubMed

Panjikar, Santosh; Parthasarathy, Venkataraman; Lamzin, Victor S; Weiss, Manfred S; Tucker, Paul A

2005-04-01

The EMBL-Hamburg Automated Crystal Structure Determination Platform is a system that combines a number of existing macromolecular crystallographic computer programs and several decision-makers into a software pipeline for automated and efficient crystal structure determination. The pipeline can be invoked as soon as X-ray data from derivatized protein crystals have been collected and processed. It is controlled by a web-based graphical user interface for data and parameter input, and for monitoring the progress of structure determination. A large number of possible structure-solution paths are encoded in the system and the optimal path is selected by the decision-makers as the structure solution evolves. The processes have been optimized for speed so that the pipeline can be used effectively for validating the X-ray experiment at a synchrotron beamline.

Do Reuss and Voigt Bounds Really Bound in High-Pressure Rheology Experiments?

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

Chen,J.; Li, L.; Yu, T.

2006-01-01

Energy dispersive synchrotron x-ray diffraction is carried out to measure differential lattice strains in polycrystalline Fe{sub 2}SiO{sub 4} (fayalite) and MgO samples using a multi-element solid state detector during high-pressure deformation. The theory of elastic modeling with Reuss (iso-stress) and Voigt (iso-strain) bounds is used to evaluate the aggregate stress and weight parameter, {alpha} (0{le}{alpha}{le}1), of the two bounds. Results under the elastic assumption quantitatively demonstrate that a highly stressed sample in high-pressure experiments reasonably approximates to an iso-stress state. However, when the sample is plastically deformed, the Reuss and Voigt bounds are no longer valid ({alpha} becomes beyond 1).more » Instead, if plastic slip systems of the sample are known (e.g. in the case of MgO), the aggregate property can be modeled using a visco-plastic self-consistent theory.« less

Correlation Between Hot Spots and 3-d Defect Structure in Single and Polycrystalline High-explosive Materials

NASA Astrophysics Data System (ADS)

Hawkins, Cameron; Tschuaner, Oliver; Fussell, Zachary; Smith, Jesse

2017-06-01

A novel approach that spatially identifies inhomogeneities from microscale (defects, con-formational disorder) to mesoscale (voids, inclusions) is developed using synchrotron x-ray methods: tomography, Lang topography, and micro-diffraction mapping. These techniques pro-vide a non-destructive method for characterization of mm-sized samples prior to shock experiments. These characterization maps can be used to correlate continuum level measurements in shock compression experiments to the mesoscale and microscale structure. Specifically examined is a sample of C4. We show extensive conformational disorder in gamma-RDX, which is the main component. Further, we observe that the minor HMX-component in C4 contains at least two different phases: alpha- and beta-HMX. This work supported by National Security Technologies, LLC, under Contract No. DE-AC52-06NA25946 with the U.S. Department of Energy and by the Site-Directed Research and Development Program. DOE/NV/25946-3071.

Optimised Combined Angular and Energy Dispersive Diffraction at the PSICHE Beam Line of the SOLEIL Synchrotron for Fast, High Q-range Structure Determination at High Pressure and Temperature.

NASA Astrophysics Data System (ADS)

King, A.; Guignot, N.; Boulard, E.; Deslandes, J. P.; Clark, A. N.; Morard, G.; Itié, J. P.

2017-12-01

Synchrotron diffraction is an ideal technique for investigating materials at high pressure and temperature, because the penetrating nature of high-energy X-rays allows measurements to be made inside pressure cells or sample environments. Wang et al. described the CAESAR acquisition strategy, in which energy and angular dispersive techniques are combined to produce an instrument particularly suitable for quantitative measurements from samples inside high-pressure apparati [1]. The PSICHE beam line of the SOLEIL Synchrotron is equipped with such a CAESAR system. Uniquely, this system allows energy dispersive diffraction spectra to be acquired at scattering angles between -5 and +30 degrees two theta, while maintaining a sphere of confusion at the measurement position in the order of 10 microns. The slits used to define the scattering angle act as Soller slits and select the diffracted volume, separating the sample from its environment. By developing an optimised acquisition strategy we are able to obtain data covering a very wide Q range (to 160nm-1 or more), while minimising the total acquisition time (one hour per complete acquisition). In addition, the 2D nature (angle and energy) of the acquired dataset enables the effective incident spectrum to be efficiently determined with no addition measurements, in order to normalise the acquired data. The resulting profile of scattered intensity as a function of Q is suitable for Fourier transform analysis of liquid or amorphous structures. PSICHE is a multi technique beam line, with a part of the beam time dedicated to parallel beam absorption and phase contrast radiography and tomography [2]. Examples will be given to show how these techniques can be combined with diffraction techniques to greatly enrich studies of materials at extreme conditions. [1] Wang, Y., Uchida, T., Von Dreele, R., Rivers, M. L., Nishiyama, N., Funakoshi, K., Nozawa, A., and Keneko, H., J. Appl. Crystallogr. 37, 947 (2004). [2] King, A., Guignot, N., Zerbino, P., Boulard, E., Desjardins, K., Bourdessoule, M., Leclerq, N., Le, S., Renaud, G., Cerato, M., Bornert, M., Lenoir, N., Delzon, S., Perrillat, J.-P., Legodec, Y., Itié, J.-P. Rev. Sci. Instrum. 87, 093704 (2016).

Synchrotron radiation study on the phase relations of KAlSi3O8

NASA Astrophysics Data System (ADS)

Urakawa, Satoru; Ohno, Hideo; Igawa, Naoki; Kondo, Tadashi; Shimomura, Osamu

1994-07-01

The equilibrium phase relations of KAlSi3O8 have been determined by in situ X-ray diffraction method using synchrotron radiation at Photon Factory, Natl. Lab. for High Energy Physics. Experiments were conducted by using the cubic type high pressure apparatus, MAX90, equipped with sintered diamond anvils. The temperature region was extended to 2000 °C up to 10 GPa in this study. Sanidine, the low pressure phase of KAlSi3O8, decomposes into three phases, the wadeite-type K2Si4O9+kyanite (Al2SiO5)+coesite (SiO2), at 6.5 GPa and 1200˜1300 °C. The hollandite-type KAlSi3O8 is made up of three phases at 9.2 GPa and 1300˜1400 °C. The melting points of sanidine and the hollandite-type KAlSi3O8 are 1600 °C at 6.7 GPa and 1800 °C at 11.2 GPa, respectively. In three phases coexisting field, wadeite-type K2Si4O9 first melts at the temperature between 1400 °C and 1500 °C.

Multi-element germanium detectors for synchrotron applications

DOE PAGES

Rumaiz, A. K.; Kuczewski, A. J.; Mead, J.; ...

2018-04-27

In this paper, we have developed a series of monolithic multi-element germanium detectors, based on sensor arrays produced by the Forschungzentrum Julich, and on Application-specific integrated circuits (ASICs) developed at Brookhaven. Devices have been made with element counts ranging from 64 to 384. These detectors are being used at NSLS-II and APS for a range of diffraction experiments, both monochromatic and energy-dispersive. Compact and powerful readout systems have been developed, based on the new generation of FPGA system-on-chip devices, which provide closely coupled multi-core processors embedded in large gate arrays. Finally, we will discuss the technical details of the systems,more » and present some of the results from them.« less

Multi-element germanium detectors for synchrotron applications

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

Rumaiz, A. K.; Kuczewski, A. J.; Mead, J.

In this paper, we have developed a series of monolithic multi-element germanium detectors, based on sensor arrays produced by the Forschungzentrum Julich, and on Application-specific integrated circuits (ASICs) developed at Brookhaven. Devices have been made with element counts ranging from 64 to 384. These detectors are being used at NSLS-II and APS for a range of diffraction experiments, both monochromatic and energy-dispersive. Compact and powerful readout systems have been developed, based on the new generation of FPGA system-on-chip devices, which provide closely coupled multi-core processors embedded in large gate arrays. Finally, we will discuss the technical details of the systems,more » and present some of the results from them.« less

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.

Purification, crystallization and preliminary X-ray analysis of Enterococcus faecium aminoglycoside-2′′-phosphotransferase-Ib [APH(2′′)-Ib

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

Walanj, Rupa; Young, Paul; Baker, Heather M.

2005-04-01

APH(2′′)-Ib is an enzyme responsible for high-level gentamicin resistance in E. faecium isolates. Native crystals of this enzyme have been prepared and preliminary X-ray diffraction experiments have been undertaken. Bacterial resistance to the aminoglycoside antibiotics is primarily the result of deactivation of the drugs. Three families of enzymes are responsible for this activity, with one such family being the aminoglycoside phosphotransferases (APHs). The gene encoding one of these enzymes, APH(2′′)-Ib, has been cloned and the protein (comprising 299 amino-acid residues) expressed in Escherichia coli, purified and crystallized in the presence of 16%(w/v) PEG 3350 and gentamicin. The crystals belong tomore » the monoclinic space group P2{sub 1}, with approximate unit-cell parameters a = 79.7, b = 58.8, c = 81.4 Å, β = 98.4°, and preliminary X-ray diffraction analysis is consistent with the presence of two molecules in the asymmetric unit. Synchrotron diffraction data to approximately 2.65 Å resolution were collected from a native APH(2′′)-Ib crystal at beamline BL9-2 at SSRL (Stanford, CA, USA). Selenium-substituted crystals have also been produced and structure determination is proceeding.« less

Acoustic emissions imaging and synchrotron X-ray diffraction analysis of calcite at high pressure and temperature

NASA Astrophysics Data System (ADS)

Gasc, J.; Brantut, N.; Schubnel, A.; Brunet, F.; Mueller, H.

2008-12-01

We have monitored from in-situ X-ray diffraction coupled to Acoustic Emission (AE) imaging, the behavior of a fine grained synthetic calcite aggregate, at 0.66 GPa and for temperatures ranging from ambient to 1200° C. The powder sample was placed in a boron-epoxy assembly with an 8 mm edge-length and loaded in the MAX80 cubic multi-anvil press installed on the German synchrotron (HASYLAB-DESY, Hamburg). AE were recorded using five piezoceramic transducers (5 MHz eigen frequency) glued on each of the five WC anvils (4 side anvils and upper one). Full waveforms were acquired using an eight channel digital oscilloscope and located using the software Insite (ASC Ltd). Beyond 600° C, calcite grains started growing as evidenced by huge changes in the relative intensity of the diffraction lines. This is correlated to a sudden burst of AE which all located within the sample volume. These AE may indicate that stress relaxation, going on as intra-crystalline plasticity mechanisms were activated, released enough acoustic energy to be recorded and located. Although the diffraction data showed that grain growth continued beyond 800° C, the acoustic activity progressively decreased to below the sensitivity of our recording device (i.e. the triggering level). However, at temperature higher than 1000° C, a large number of AE were recorded again ( 2000 events). AE location revealed that the AE front progressed inwards the sample. The complete loss of diffraction signal and the post-mortem recovery of small amounts of CaO suggest that the second AE burst may be related to calcite melting/decarbonation. Perspectives include thorough microstructural analysis of the samples using electron microscopies (SEM and TEM) as well as a statistical and mechanical analysis of the acoustic data.

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.

Crystallization and preliminary X-ray diffraction analysis of West Nile virus

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

Kaufmann, Barbel; Plevka, Pavel; Kuhn, Richard J.

2010-05-25

West Nile virus, a human pathogen, is closely related to other medically important flaviviruses of global impact such as dengue virus. The infectious virus was purified from cell culture using polyethylene glycol (PEG) precipitation and density-gradient centrifugation. Thin amorphously shaped crystals of the lipid-enveloped virus were grown in quartz capillaries equilibrated by vapor diffusion. Crystal diffraction extended at best to a resolution of about 25 {angstrom} using synchrotron radiation. A preliminary analysis of the diffraction images indicated that the crystals had unit-cell parameters a {approx_equal} b {approx_equal} 480 {angstrom}, {gamma} = 120{sup o}, suggesting a tight hexagonal packing of onemore » virus particle per unit cell.« less

Lattice preferred orientation in MnGeO3 post-perovskite at high-temperature

NASA Astrophysics Data System (ADS)

Nagaya, Y.; Hirose, K.; Sata, N.; Ohishi, Y.

2009-12-01

In the Earth’s lowermost mantle which is called D” layer, shear-wave splitting is often observed. The velocity of horizontally polarized S-waves are faster than polarized S-waves in many areas of the D” layer. The D” layer is now recognized as being made up with the post-perovskite (PPv)-type MgSiO3 phase. MgSiO3 PPv has a strong elastic anisotropy because of its layered crystal structure. Therefore, it is expected that a lattice preferred orientation (LPO) of PPv may explain the observed seismic anisotropy. LPOs of PPv have been investigated by the high-pressure experiments using a diamond anvil cell (DAC) (Merkel et al., 2006; 2007; Okada et al., 2009). However, the reported experiments using the DAC were made only at the room temperature. In order to understand the nature of PPv deformation under the lower mantle conditions, it is necessary to operate the deformation experiments at high-temperature (~2500 K). In this study, so as to examine the LPO and the dominant slip plane of PPv at simultaneously high P-T conditions, we conducted the high-temperature plastic deformation experiments in a laser-heated diamond anvil cell (LHDAC) using synchrotron radial X-ray diffraction techniques at the beamline BL10XU, SPring-8. In the radial X-ray diffraction experiments, X-ray was irradiated to the sample perpendicular to the compression axis through gasket. LPO was investigated on the basis of the variations of diffraction intensity. We adopted a cubic boron nitride and beryllium composite gasket to obtain a radial X-ray diffraction pattern. In order to deform a sample at high temperature, we had newly developed a membrane system for the deformation experiments. We are able to regulate the gas pressure in the membrane of the DAC, and therefore compress the sample at high temperature during the laser heating. Starting material was orthopyroxene (OPx) with a composition of MnGeO3, which is an analogue of MgSiO3. First, MnGeO3 PPv was synthesized directly from OPx around 60 GPa in the LHDAC. Subsequently, PPv was plastically deformed by further compression at high-temperature during the laser heating. We also conducted the room-temperature deformation experiments. We will discuss the deformation mechanism of the PPv at high P-T conditions.

High speed systems for time-resolved experiments with synchrotron radiation

NASA Astrophysics Data System (ADS)

Koziol, Anna; Maj, Piotr

2018-02-01

The UFXC32k is a single photon counting hybrid pixel detector with 75 μm pixel pitch. It was designed to cope with high X-ray intensities and therefore it is a very good candiate for synchrotron applications. In order to use this detector in an application, a dedicated setup must be designed and built allowing proper operation of the detector within the experiment. The paper presents two setups built for the purpose of Pump-Probe-Probe experiments at the Synchrotron SOLEIL and XPCS experiments at the APS.

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

NASA Astrophysics Data System (ADS)

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

2016-04-01

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

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.

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.

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

Gargarella, P., E-mail: piter@ufscar.br; Departamento de Engenharia de Materiais, Universidade Federal de São Carlos, Rodovia Washington Luiz, Km 235, 13565-905 São Carlos, São Paulo; Pauly, S.

The structural evolution of Ti{sub 50}Cu{sub 43}Ni{sub 7} and Ti{sub 55}Cu{sub 35}Ni{sub 10} metallic glasses during heating was investigated by in-situ synchrotron X-ray diffraction. The width of the most intense diffraction maximum of the glassy phase decreases slightly during relaxation below the glass transition temperature. Significant structural changes only occur above the glass transition manifesting in a change in the respective peak positions. At even higher temperatures, nanocrystals of the shape memory B2-Ti(Cu,Ni) phase precipitate, and their small size hampers the occurrence of a martensitic transformation.

{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.}

Metastable and equilibrium phase formation in sputter-deposited Ti/Al multilayer thin films

NASA Astrophysics Data System (ADS)

Lucadamo, G.; Barmak, K.; Lavoie, C.; Cabral, C., Jr.; Michaelsen, C.

2002-06-01

The sequence and kinetics of metastable and equilibrium phase formation in sputter deposited multilayer thin films was investigated by combining in situ synchrotron x-ray diffraction (XRD) with ex situ electron diffraction and differential scanning calorimetry (DSC). The sequence included both cubic and tetragonal modifications of the equilibrium TiAl3 crystal structure. Values for the formation activation energies of the various phases in the sequence were determined using the XRD and DSC data obtained here, as well as activation energy data reported in the literature.

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

Beam Size Measurement by Optical Diffraction Radiation and Laser System for Compton Polarimeter (in Chinese)

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

Liu, Chuyu

2012-12-31

Beam diagnostics is an essential constituent of any accelerator, so that it is named as "organs of sense" or "eyes of the accelerator." Beam diagnostics is a rich field. A great variety of physical effects or physical principles are made use of in this field. Some devices are based on electro-magnetic influence by moving charges, such as faraday cups, beam transformers, pick-ups; Some are related to Coulomb interaction of charged particles with matter, such as scintillators, viewing screens, ionization chambers; Nuclear or elementary particle physics interactions happen in some other devices, like beam loss monitors, polarimeters, luminosity monitors; Some measuremore » photons emitted by moving charges, such as transition radiation, synchrotron radiation monitors and diffraction radiation-which is the topic of the first part of this thesis; Also, some make use of interaction of particles with photons, such as laser wire and Compton polarimeters-which is the second part of my thesis. Diagnostics let us perceive what properties a beam has and how it behaves in a machine, give us guideline for commissioning, controlling the machine and indispensable parameters vital to physics experiments. In the next two decades, the research highlight will be colliders (TESLA, CLIC, JLC) and fourth-generation light sources (TESLA FEL, LCLS, Spring 8 FEL) based on linear accelerator. These machines require a new generation of accelerator with smaller beam, better stability and greater efficiency. Compared with those existing linear accelerators, the performance of next generation linear accelerator will be doubled in all aspects, such as 10 times smaller horizontal beam size, more than 10 times smaller vertical beam size and a few or more times higher peak power. Furthermore, some special positions in the accelerator have even more stringent requirements, such as the interaction point of colliders and wigglor of free electron lasers. Higher performance of these accelerators increases the difficulty of diagnostics. For most cases, intercepting measurements are no longer acceptable, and nonintercepting method like synchrotron radiation monitor can not be applied to linear accelerators. The development of accelerator technology asks for simutanous diagnostics innovations, to expand the performance of diagnostic tools to meet the requirements of the next generation accelerators. Diffraction radiation and inverse Compton scattering are two of the most promising techniques, their nonintercepting nature avoids perturbance to the beam and damage to the instrumentation. This thesis is divided into two parts, beam size measurement by optical diffraction radiation and Laser system for Compton polarimeter. Diffraction radiation, produced by the interaction between the electric field of charged particles and the target, is related to transition radiation. Even though the theory of diffraction radiation has been discussed since 1960s, there are only a few experimental studies in recent years. The successful beam size measurement by optical diffraction radiation at CEBAF machine is a milestone: First of all, we have successfully demonstrated diffraction radiation as an effective nonintercepting diagnostics; Secondly, the simple linear relationship between the diffraction radiation image size and the actual beam size improves the reliability of ODR measurements; And, we measured the polarized components of diffraction radiation for the first time and I analyzed the contribution from edge radiation to diffraction radiation.« less

Direct Visualization of Orbital Flipping in Volborthite by Charge Density Analysis Using Detwinned Data

NASA Astrophysics Data System (ADS)

Sugawara, Kento; Sugimoto, Kunihisa; Fujii, Tatsuya; Higuchi, Takafumi; Katayama, Naoyuki; Okamoto, Yoshihiko; Sawa, Hiroshi

2018-02-01

The distribution of d-orbital valence electrons in volborthite [Cu3V2O7(OH)2 • 2H2O] was investigated by charge density analysis of the multipole model refinement. Diffraction data were obtained by synchrotron radiation single-crystal X-ray diffraction experiments. Data reduction by detwinning of the multiple structural domains was performed using our developed software. In this study, using high-quality data, we demonstrated that the water molecules in volborthite can be located by the hydrogen bonding in cavities that consist of Kagome lattice layers of CuO4(OH)2 and pillars of V2O7. Final multipole refinements before and after the structural phase transition directly visualized the deformation electron density of the valence electrons. We successfully directly visualized the orbital flipping of the d-orbital dx2-y2, which is the highest level of 3d orbitals occupied by d9 electrons in volborthite. The developed techniques and software can be employed for investigations of structural properties of systems with multiple structural domains.

In situ X-ray diffraction and the evolution of polarization during the growth of ferroelectric superlattices

DOE PAGES

Bein, Benjamin; Hsing, Hsiang-Chun; Callori, Sara J.; ...

2015-12-04

In the epitaxially strained ferroelectric thin films and superlattices, the ferroelectric transition temperature can lie above the growth temperature. Ferroelectric polarization and domains should then evolve during the growth of a sample, and electrostatic boundary conditions may play an important role. In this work, ferroelectric domains, surface termination, average lattice parameter and bilayer thickness are simultaneously monitored using in situ synchrotron X-ray diffraction during the growth of BaTiO 3/SrTiO 3 superlattices on SrTiO 3 substrates by off-axis radio frequency magnetron sputtering. The technique used allows for scan times substantially faster than the growth of a single layer of material. Effectsmore » of electric boundary conditions are investigated by growing the same superlattice alternatively on SrTiO 3 substrates and 20 nm SrRuO 3 thin films on SrTiO 3 substrates. Our experiments provide important insights into the formation and evolution of ferroelectric domains when the sample is ferroelectric during the growth process.« less

Magnetic properties of transition metal fluorides MF2 (M=Mn, Fe, Co, Ni) via high-energy photon diffraction

NASA Astrophysics Data System (ADS)

Strempfer, J.; Rütt, U.; Bayrakci, S.; Brückel, Th.; Jauch, W.

2004-01-01

We present an overview of recent results from nonresonant magnetic diffraction experiments on the antiferromagnetic compounds MnF2, FeF2, CoF2, and NiF2 using high-energy synchrotron radiation of photon energies above 100 keV. New results are presented on the determination of the spin and of the L/S ratio for CoF2 and NiF2. For CoF2, the saturation value of the long-range-ordered pure spin Sz component Sz=1.11(1) is considerably lower than the value Sz=3/2 for the free Co2+ ion. This is in contrast to our results for NiF2, where the full spin of the free transition-metal ion was found, Sz=0.98(1). The temperature dependence of the magnetization in the critical region as well as in the low-temperature region is also presented. For all compounds, Ising behavior is found in the critical regime, whereas the crossover to the low-temperature spin-wave behavior varies. We attribute this to different anisotropies in this series of compounds.

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.

National Synchrotron Light Source annual report 1988

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

Hulbert, S.; Lazarz, N.; Williams, G.

1988-01-01

This report discusses the experiment done at the National Synchrotron Light Source. Most experiments discussed involves the use of the x-ray beams to study physical properties of solid materials. (LSP)

Crystallization and preliminary X-ray diffraction analysis of the peripheral light-harvesting complex LH2 from Marichromatium purpuratum.

PubMed

Cranston, Laura J; Roszak, Aleksander W; Cogdell, Richard J

2014-06-01

LH2 from the purple photosynthetic bacterium Marichromatium (formerly known as Chromatium) purpuratum is an integral membrane pigment-protein complex that is involved in harvesting light energy and transferring it to the LH1-RC `core' complex. The purified LH2 complex was crystallized using the sitting-drop vapour-diffusion method at 294 K. The crystals diffracted to a resolution of 6 Å using synchrotron radiation and belonged to the tetragonal space group I4, with unit-cell parameters a=b=109.36, c=80.45 Å. The data appeared to be twinned, producing apparent diffraction symmetry I422. The tetragonal symmetry of the unit cell and diffraction for the crystals of the LH2 complex from this species reveal that this complex is an octamer.

Crystallization and preliminary X-ray diffraction analysis of the peripheral light-harvesting complex LH2 from Marichromatium purpuratum

PubMed Central

Cranston, Laura J.; Roszak, Aleksander W.; Cogdell, Richard J.

2014-01-01

LH2 from the purple photosynthetic bacterium Marichromatium (formerly known as Chromatium) purpuratum is an integral membrane pigment–protein complex that is involved in harvesting light energy and transferring it to the LH1–RC ‘core’ complex. The purified LH2 complex was crystallized using the sitting-drop vapour-diffusion method at 294 K. The crystals diffracted to a resolution of 6 Å using synchrotron radiation and belonged to the tetragonal space group I4, with unit-cell parameters a = b = 109.36, c = 80.45 Å. The data appeared to be twinned, producing apparent diffraction symmetry I422. The tetragonal symmetry of the unit cell and diffraction for the crystals of the LH2 complex from this species reveal that this complex is an octamer. PMID:24915099

Zigzag spin structure in layered honeycomb L i3N i2Sb O6 : A combined diffraction and antiferromagnetic resonance study

NASA Astrophysics Data System (ADS)

Kurbakov, A. I.; Korshunov, A. N.; Podchezertsev, S. Yu.; Malyshev, A. L.; Evstigneeva, M. A.; Damay, F.; Park, J.; Koo, C.; Klingeler, R.; Zvereva, E. A.; Nalbandyan, V. B.

2017-07-01

The magnetic structure of L i3N i2Sb O6 has been determined by low-temperature neutron diffraction, and the crystal structure has been refined by a combination of synchrotron and neutron powder diffraction. The monoclinic (C 2 /m ) symmetry, assigned previously to this pseudohexagonal layered structure, has been unambiguously proven by peak splitting in the synchrotron diffraction pattern. The structure is based on essentially hexagonal honeycomb-ordered N i2Sb O6 layers alternating with L i3 layers, all cations and anions being in an octahedral environment. The compound orders antiferromagnetically below TN=15 K , with the magnetic supercell being a 2 a ×2 b multiple of the crystal cell. The magnetic structure within the honeycomb layer consists of zigzag ferromagnetic spin chains coupled antiferromagnetically. The ordered magnetic moment amounts to 1.62 (2 ) μB/Ni , which is slightly lower than the full theoretical value. Upon cooling below TN, the spins tilt from the c axis, with a maximum tilting angle of 15 .6∘ at T =1.5 K . Our data imply non-negligible ferromagnetic interactions between the honeycomb layers. The observed antiferromagnetic resonance modes are in agreement with the two-sublattice model derived from the neutron data. Orthorhombic anisotropy shows up in zero-field splitting of Δ =198 ±4 and 218 ±4 GHz . Above TN, the electron spin resonance data imply short-range antiferromagnetic order up to about 80 K.

Pump-probe experiments at the TEMPO beamline using the low-α operation mode of Synchrotron SOLEIL.

PubMed

Silly, Mathieu G; Ferté, Tom; Tordeux, Marie Agnes; Pierucci, Debora; Beaulieu, Nathan; Chauvet, Christian; Pressacco, Federico; Sirotti, Fausto; Popescu, Horia; Lopez-Flores, Victor; Tortarolo, Marina; Sacchi, Maurizio; Jaouen, Nicolas; Hollander, Philippe; Ricaud, Jean Paul; Bergeard, Nicolas; Boeglin, Christine; Tudu, Bharati; Delaunay, Renaud; Luning, Jan; Malinowski, Gregory; Hehn, Michel; Baumier, Cédric; Fortuna, Franck; Krizmancic, Damjan; Stebel, Luigi; Sergo, Rudi; Cautero, Giuseppe

2017-07-01

The SOLEIL synchrotron radiation source is regularly operated in special filling modes dedicated to pump-probe experiments. Among others, the low-α mode operation is characterized by shorter pulse duration and represents the natural bridge between 50 ps synchrotron pulses and femtosecond experiments. Here, the capabilities in low-α mode of the experimental set-ups developed at the TEMPO beamline to perform pump-probe experiments with soft X-rays based on photoelectron or photon detection are presented. A 282 kHz repetition-rate femtosecond laser is synchronized with the synchrotron radiation time structure to induce fast electronic and/or magnetic excitations. Detection is performed using a two-dimensional space resolution plus time resolution detector based on microchannel plates equipped with a delay line. Results of time-resolved photoelectron spectroscopy, circular dichroism and magnetic scattering experiments are reported, and their respective advantages and limitations in the framework of high-time-resolution pump-probe experiments compared and discussed.

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

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

Zou, Yongtao; Zhang, Wei; Li, Xuefei

2018-01-01

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

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

NASA Technical Reports Server (NTRS)

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

2016-01-01

The petrographic study of Itokawa particle, RA-QD02-0127 has been performed by SEM-EDS and optical microscope observations. The purpose of this study is to understand better the metamorphic and impact shock history of asteroid Itokawa, and other S-class asteroids.

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

Anomalous Thermal Expansion of HoCo0.5Cr0.5O3 Probed by X-ray Synchrotron Powder Diffraction.

PubMed

Hreb, Vasyl; Vasylechko, Leonid; Mykhalichko, Vitaliya; Prots, Yurii

2017-12-01

Mixed holmium cobaltite-chromite HoCo 0.5 Cr 0.5 O 3 with orthorhombic perovskite structure (structure type GdFeO 3 , space group Pbnm) was obtained by solid state reaction of corresponding oxides in air at 1373 K. Room- and high-temperature structural parameters were derived from high-resolution X-ray synchrotron powder diffraction data collected in situ in the temperature range of 300-1140 K. Analysis of the results obtained revealed anomalous thermal expansion of HoCo 0.5 Cr 0.5 O 3 , which is reflected in a sigmoidal temperature dependence of the unit cell parameters and in abnormal increase of the thermal expansion coefficients with a broad maxima near 900 K. Pronounced anomalies are also observed for interatomic distances and angles within Co/CrO 6 octahedra, tilt angles of octahedra and atomic displacement parameters. The observed anomalies are associated with the changes of spin state of Co 3+ ions and insulator-metal transition occurring in HoCo 0.5 Cr 0.5 O 3 .

Anomalous Thermal Expansion of HoCo0.5Cr0.5O3 Probed by X-ray Synchrotron Powder Diffraction

NASA Astrophysics Data System (ADS)

Hreb, Vasyl; Vasylechko, Leonid; Mykhalichko, Vitaliya; Prots, Yurii

2017-07-01

Mixed holmium cobaltite-chromite HoCo0.5Cr0.5O3 with orthorhombic perovskite structure (structure type GdFeO3, space group Pbnm) was obtained by solid state reaction of corresponding oxides in air at 1373 K. Room- and high-temperature structural parameters were derived from high-resolution X-ray synchrotron powder diffraction data collected in situ in the temperature range of 300-1140 K. Analysis of the results obtained revealed anomalous thermal expansion of HoCo0.5Cr0.5O3, which is reflected in a sigmoidal temperature dependence of the unit cell parameters and in abnormal increase of the thermal expansion coefficients with a broad maxima near 900 K. Pronounced anomalies are also observed for interatomic distances and angles within Co/CrO6 octahedra, tilt angles of octahedra and atomic displacement parameters. The observed anomalies are associated with the changes of spin state of Co3+ ions and insulator-metal transition occurring in HoCo0.5Cr0.5O3.

A highly modular beamline electrostatic levitation facility, optimized for in situ high-energy x-ray scattering studies of equilibrium and supercooled liquids

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

Mauro, N.A.; Kelton, K.F.

2011-10-27

High-energy x-ray diffraction studies of metallic liquids provide valuable information about structural evolution on the atomic length scale, leading to insights into the origin of the nucleation barrier and the processes of supercooling and glass formation. The containerless processing of the beamline electrostatic levitation (BESL) facility allows coordinated thermophysical and structural studies of equilibrium and supercooled liquids to be made in a contamination-free, high-vacuum ({approx}10{sup -8} Torr) environment. To date, the incorporation of electrostatic levitation facilities into synchrotron beamlines has been difficult due to the large footprint of the apparatus and the difficulties associated with its transportation and implementation. Here,more » we describe a modular levitation facility that is optimized for diffraction studies of high-temperature liquids at high-energy synchrotron beamlines. The modular approach used in the apparatus design allows it to be easily transported and quickly setup. Unlike most previous electrostatic levitation facilities, BESL can be operated by a single user instead of a user team.« less

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

Protein nanocrystallography: growth mechanism and atomic structure of crystals induced by nanotemplates.

PubMed

Pechkova, E; Vasile, F; Spera, R; Fiordoro, S; Nicolini, C

2005-11-01

Protein nanocrystallography, a new technology for crystal growth based on protein nanotemplates, has recently been shown to produce diffracting, stable and radiation-resistant lysozyme crystals. This article, by computing these lysozyme crystals' atomic structures, obtained by the diffraction patterns of microfocused synchrotron radiation, provides a possible mechanism for this increased stability, namely a significant decrease in water content accompanied by a minor but significant alpha-helix increase. These data are shown to be compatible with the circular dichroism and two-dimensional Fourier transform spectra of high-resolution H NMR of proteins dissolved from the same nanotemplate-based crystal versus those from a classical crystal. Finally, evidence for protein direct transfer from the nanotemplate to the drop and the participation of the template proteins in crystal nucleation and growth is provided by high-resolution NMR spectrometry and mass spectrometry. Furthermore, the lysozyme nanotemplate appears stable up to 523 K, as confirmed by a thermal denaturation study using spectropolarimetry. The overall data suggest that heat-proof lysozyme presence in the crystal provides a possible explanation of the crystal's resistance to synchrotron radiation.

Size–strain separation in diffraction line profile analysis

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

Scardi, P.; Ermrich, M.; Fitch, A.

Separation of size and strain effects on diffraction line profiles has been studied in a round robin involving laboratory instruments and synchrotron radiation beamlines operating with different radiation, optics, detectors and experimental configurations. The studied sample, an extensively ball milled iron alloy powder, provides an ideal test case, as domain size broadening and strain broadening are of comparable size. The high energy available at some synchrotron radiation beamlines provides the best conditions for an accurate analysis of the line profiles, as the size–strain separation clearly benefits from a large number of Bragg peaks in the pattern; high counts, reliable intensitymore » values in low-absorption conditions, smooth background and data collection at different temperatures also support the possibility to include diffuse scattering in the analysis, for the most reliable assessment of the line broadening effect. However, results of the round robin show that good quality information on domain size distribution and microstrain can also be obtained using standard laboratory equipment, even when patterns include relatively few Bragg peaks, provided that the data are of good quality in terms of high counts and low and smooth background.« less

Combined Synchrotron X-ray Diffraction and Digital Image Correlation Technique for Measurement of Austenite Transformation with Strain in TRIP-assisted Steels

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

Poling, Whitney A.; Savic, Vesna; Hector, Louis G.

2016-04-05

The strain-induced, diffusionless shear transformation of retained austenite to martensite during straining of transformation induced plasticity (TRIP) assisted steels increases strain hardening and delays necking and fracture leading to exceptional ductility and strength, which are attractive for automotive applications. A novel technique that provides the retained austenite volume fraction variation with strain in TRIP-assisted steels with improved precision is presented. Digital images of the gauge section of tensile specimens were first recorded up to selected plastic strains with a stereo digital image correlation (DIC) system. The austenite volume fraction was measured by synchrotron X-ray diffraction from small squares cut frommore » the gage section. Strain fields in the squares were then computed by localizing the strain measurement to the corresponding region of a given square during DIC post-processing of the images recorded during tensile testing. Results obtained for a QP980 steel are used to study the influence of initial volume fraction of austenite and the austenite transformation with strain on tensile mechanical behavior.« less

Relationships Between the Phase Transformation Kinetics, Texture Evolution, and Microstructure Development in a 304L Stainless Steel Under Biaxial Loading Conditions: Synchrotron X-ray and Electron Backscatter Diffraction Studies

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

Cakmak, Ercan; Choo, Hahn; Kang, Jun-Yun

2015-02-11

The relationships between the martensitic phase transformation kinetics, texture evolution, and the microstructure development in the parent austenite phase were studied for a 304L stainless steel that exhibits the transformation-induced plasticity effect under biaxial loading conditions at ambient temperature. The applied loading paths included: pure torsion, simultaneous biaxial torsion/tension, simultaneous biaxial torsion/compression, and stepwise loading of tension followed by torsion (i.e., first loading by uniaxial tension and then by pure torsion in sequence). Synchrotron X-ray and electron backscatter diffraction techniques were used to measure the evolution of the phase fractions, textures, and microstructures as a function of the applied strains.more » The influence of loading character and path on the changes in martensitic phase transformation kinetics is discussed in the context of (1) texture-transformation relationship and the preferred transformation of grains belonging to certain texture components over the others, (2) effects of axial strains on shear band evolutions, and (3) volume changes associated with martensitic transformation.« less

Structure and stability of solid Xe(H 2) n

DOE PAGES

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

2015-03-10

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

Size–strain separation in diffraction line profile analysis

DOE PAGES

Scardi, P.; Ermrich, M.; Fitch, A.; ...

2018-05-29

Separation of size and strain effects on diffraction line profiles has been studied in a round robin involving laboratory instruments and synchrotron radiation beamlines operating with different radiation, optics, detectors and experimental configurations. The studied sample, an extensively ball milled iron alloy powder, provides an ideal test case, as domain size broadening and strain broadening are of comparable size. The high energy available at some synchrotron radiation beamlines provides the best conditions for an accurate analysis of the line profiles, as the size–strain separation clearly benefits from a large number of Bragg peaks in the pattern; high counts, reliable intensitymore » values in low-absorption conditions, smooth background and data collection at different temperatures also support the possibility to include diffuse scattering in the analysis, for the most reliable assessment of the line broadening effect. However, results of the round robin show that good quality information on domain size distribution and microstrain can also be obtained using standard laboratory equipment, even when patterns include relatively few Bragg peaks, provided that the data are of good quality in terms of high counts and low and smooth background.« 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.

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.

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.

Interactions Between Snow-Adapted Organisms, Minerals and Snow in a Mars-Analog Environment, and Implications for the Possible Formation of Mineral Biosignatures

NASA Astrophysics Data System (ADS)

Hausrath, E.; Bartlett, C. L.; Garcia, A. H.; Tschauner, O. D.; Murray, A. E.; Raymond, J. A.

2015-12-01

Increasing evidence suggests that icy environments on bodies such as Mars, Europa, and Enceladus may be important potential habitats in our solar system. Life in icy environments faces many challenges, including water limitation, temperature extremes, and nutrient limitation. Understanding how life has adapted to withstand these challenges on Earth may help understand potential life on other icy worlds, and understanding the interactions of such life with minerals may help shed light on the detection of possible mineral biosignatures. Snow environments, being particularly nutrient limited, may require specific adaptations by the microbiota living there. Previous observations have suggested that associated minerals and microorganisms play an important role in snow algae micronutrient acquisition. Here, in order to interpret micronutrient uptake by snow algae, and potential formation of mineral biosignatures, we present observations of interactions between snow algae and associated microorganisms and minerals in both natural, Mars-analog environments, and laboratory experiments. Samples of snow, dust, snow algae, and microorganisms were collected from Mount Anderson Ridge, CA. Some samples were DAPI-stained and analyzed by epifluorescent microscopy, and others were freeze-dried and examined by scanning electron microscopy, synchrotron X-ray diffraction (XRD) and synchrotron X-ray fluorescence (XRF). Xenic cultures of the snow alga Chloromonas brevispina were also grown under Fe-limiting conditions with and without the Fe-containing mineral nontronite to determine impacts of the mineral on algal growth. Observations from epifluorescent microscopy show bacteria closely associated with the snow algae, consistent with a potential role in micronutrient acquisition. Particles are also present on the algal cell walls, and synchrotron-XRD and XRF observations indicate that they are Fe-rich, and may therefore be a micronutrient source. Laboratory experiments indicated enhanced algal growth in the presence of nontronite, as well as a close physical association between the snow alga and mineral surfaces. We are presently examining the role of minerals and microorganisms in nutrient acquisition, and attempting to identify mineral biosignatures.

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.

Expression, crystallization and preliminary X-ray diffraction studies of recombinant Clostridium perfringens β2-toxin

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

Gurjar, Abhijit A.; Yennawar, Neela H.; Yennawar, Hemant P.

2007-06-01

The cloning, expression, purification and crystallization of recombinant Clostridium perfringens β2-toxin is described. The crystals diffracted to 2.9 Å resolution. Clostridium perfringens is a Gram-positive sporulating anaerobic bacterium that is responsible for a wide spectrum of diseases in animals, birds and humans. The virulence of C. perfringens is associated with the production of several enterotoxins and exotoxins. β2-toxin is a 28 kDa exotoxin produced by C. perfringens. It is implicated in necrotic enteritis in animals and humans, a disease characterized by a sudden acute onset with lethal hemorrhagic mucosal ulceration. The recombinant expression, purification and crystallization of β2-toxin using themore » batch-under-oil technique are reported here. Native X-ray diffraction data were obtained to 2.9 Å resolution on a synchrotron beamline at the F2 station at Cornell High Energy Synchrotron Source (CHESS) using an ADSC Quantum-210 CCD detector. The crystals belong to space group R3, with a dimer in the asymmetric unit; the unit-cell parameters are a = b = 103.71, c = 193.48 Å, α = β = 90, γ = 120° using the hexagonal axis setting. A self-rotation function shows that the two molecules are related by a noncrystallographic twofold axis with polar angles ω = 90.0, ϕ = 210.3°.« less

Synchrotron powder diffraction on Aztec blue pigments

NASA Astrophysics Data System (ADS)

Sánchez Del Río, M.; Gutiérrez-León, A.; Castro, G. R.; Rubio-Zuazo, J.; Solís, C.; Sánchez-Hernández, R.; Robles-Camacho, J.; Rojas-Gaytán, J.

2008-01-01

Some samples of raw blue pigments coming from an archaeological rescue mission in downtown Mexico City have been characterized using different techniques. The samples, some recovered as a part of a ritual offering, could be assigned to the late Aztec period (XVth century). The striking characteristic of these samples is that they seem to be raw pigments prior to any use in artworks, and it was possible to collect a few μg of pigment after manual grain selection under a microscopy monitoring. All pigments are made of indigo, an organic colorant locally known as añil or xiuhquilitl. The colorant is always found in combination with an inorganic matrix, studied by powder diffraction. In one case the mineral base is palygorskite, a rare clay mineral featuring micro-channels in its structure, well known as the main ingredient of the Maya blue pigment. However, other samples present the minerals sepiolite (a clay mineral of the palygorskite family) and calcite. Another sample contains barite, a mineral never reported in prehispanic paints. We present the results of characterization using high resolution powder diffraction recorded at the European Synchrotron Radiation Facility (BM25A, SpLine beamline) complemented with other techniques. All of them gave consistent results on the composition. A chemical test on resistance to acids was done, showing a high resistance for the palygorskite and eventually sepiolite compounds, in good agreement with the excellent resistance of the Maya blue.

Melting-solidification transition of Zn nanoparticles embedded in SiO2: Observation by synchrotron x-ray and ultraviolet-visible-near-infrared light

NASA Astrophysics Data System (ADS)

Amekura, H.; Tanaka, M.; Katsuya, Y.; Yoshikawa, H.; Ohnuma, M.; Matsushita, Y.; Kobayashi, K.; Kishimoto, N.

2010-11-01

Melting-solidification transition of Zn nanoparticles (NPs) with the mean diameter of 11.5 nm, embedded in silica glass, was investigated by glancing incident x-ray diffraction (GIXRD) at high temperatures using synchrotron radiation (SR). With increasing temperature, 101Zn diffraction peak gradually decreases up to ˜360 °C and then steeply decreases. This is due to the melting of Zn NPs, which completes around 420 °C. With decreasing temperature, the solidification of the NPs begins around ˜310 °C. The temperature hysteresis with a width of ˜110 °C was observed. With temperature, the diffraction angle shows a shift without hysteresis, which is ascribed to thermal expansion of Zn NP lattice. Thermal expansion coefficient of Zn NPs was determined as 24.4×10-6 K-1 along the ⟨101⟩ direction. Optical absorption spectroscopy shows a broad ultraviolet (UV) peak which was observed at even higher temperatures than the melting temperature but shifts to the low-energy side with the melting. The energy shift in the UV peak also shows the temperature hysteresis which resembles with the melting-solidification hysteresis recorded by SR-GIXRD. The melting-solidification transition is also detectable by the optical absorption spectroscopy in the UV-visible-near-infrared region.

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.

Synchrotron X-ray diffraction and Raman spectroscopy of Ln{sub 3}NbO{sub 7} (Ln=La, Pr, Nd, Sm-Lu) ceramics obtained by molten-salt synthesis

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

Siqueira, K.P.F.; Soares, J.C.; Granado, E.

2014-01-15

Ln{sub 3}NbO{sub 7} (Ln=La, Pr, Nd, Sm, Eu, Gd, Tb, Dy, Ho, Er, Tm, Yb, and Lu) ceramics were obtained by molten-salt synthesis and their structures were systematically investigated by synchrotron X-ray diffraction (SXRD), second harmonic generation (SHG) and Raman spectroscopy. It was observed that ceramics with the largest ionic radii (La, Pr, Nd) crystallized into the Pmcn space group, while the ceramics with intermediate ionic radii (Sm-Gd) exhibited a different crystal structure belonging to the Ccmm space group. For this last group of ceramics, this result was corroborated by SHG and Raman scattering and ruled out any possibility formore » the non-centrosymmetric C 222{sub 1} space group, solving a recent controversy in the literature. Finally, according to SXRD, Tb-Lu containing samples exhibited an average defect fluorite structure (Fm3{sup ¯}m space group). Nonetheless, broad scattering at forbidden Bragg reflections indicates the presence of short-range domains with lower symmetry. Vibrational spectroscopy showed the presence of six Raman-active modes, inconsistent with the average cubic fluorite structure, and in line with the existence of lower-symmetry nano-domains immersed in the average fluorite structure of these ceramics. - Graphical abstract: Raman spectrum for Sm{sub 3}NbO{sub 7} ceramics showing their 27 phonon modes adjusted through Lorentzian lines. According to synchrotron X-ray diffraction and Raman scattering, this material belongs to the space group Cmcm. Display Omitted - Highlights: • Ln{sub 3}NbO{sub 7} ceramics were obtained by molten-salt synthesis. • SXRD, SHG and Raman scattering confirmed orthorhombic and cubic structures. • Ccmm instead of C222{sub 1} is the correct structure for Sm–Gd ceramics. • Pmcn space group was confirmed for La-, Pr- and Nd-based ceramics. • For Tb–Lu ceramics, ordered domains of a pyrochlore structure were observed.« less

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

Casco, Mirian E.; Silvestre-Albero, Joaquín; Ramírez-Cuesta, Anibal J.

Natural methane hydrates are believed to be the largest source of hydrocarbons on Earth. These structures are formed in specific locations such as deep-sea sediments and the permafrost based on demanding conditions of high pressure and low temperature. We report that, by taking advantage of the confinement effects on nanopore space, synthetic methane hydrates grow under mild conditions (3.5 MPa and 2 degrees C), with faster kinetics (within minutes) than nature, fully reversibly and with a nominal stoichiometry that mimics nature. Furthermore, the formation of the hydrate structures in nanospace and their similarity to natural hydrates is confirmed using inelasticmore » neutron scattering experiments and synchrotron X-ray powder diffraction. Our findings may be a step towards the application of a smart synthesis of methane hydrates in energy-demanding applications (for example, transportation).« less

Residual stress relief due to fatigue in tetragonal lead zirconate titanate ceramics

NASA Astrophysics Data System (ADS)

Hall, D. A.; Mori, T.; Comyn, T. P.; Ringgaard, E.; Wright, J. P.

2013-07-01

High energy synchrotron XRD was employed to determine the lattice strain ɛ{111} and diffraction peak intensity ratio R{200} in tetragonal PZT ceramics, both in the virgin poled state and after a bipolar fatigue experiment. It was shown that the occurrence of microstructural damage during fatigue was accompanied by a reduction in the gradient of the ɛ{111}-cos2 ψ plot, indicating a reduction in the level of residual stress due to poling. In contrast, the fraction of oriented 90° ferroelectric domains, quantified in terms of R{200}, was not affected significantly by fatigue. The change in residual stress due to fatigue is interpreted in terms of a change in the average elastic stiffness of the polycrystalline matrix due to the presence of inter-granular microcracks.

Aqueous Nucleation and Growth of Titanium Oxides Using Time-Resolved Synchrotron X- ray Diffraction

NASA Astrophysics Data System (ADS)

Hummer, D. R.; Heaney, P. J.; Post, J. E.

2006-05-01

The inorganic precipitation of oxide minerals in soil environments has profound effects on a variety of geochemical processes. These include the removal of metals from the aqueous phase, the production of coatings that reduce the reactive surface area of pre-existing mineral grains, and the generation of feedstocks for microbial metabolic reactions. Recent observations of transient, metastable phases during the growth of oxide crystallites has raised questions about their role in crystallization mechanisms, and created a need for more detailed structural measurements. To better understand the process of nucleation and growth, we investigated the crystallization of Ti oxides from aqueous 0.5 M TiCl4 solutions using synchrotron X-ray diffraction at temperatures of 100 and 150 °C. Solutions were heated in a 1.0 mm internal diameter quartz glass capillary sealed with epoxy. Powder diffraction patterns of the growing crystallites were collected using image plate technology with a time step of ~ 4 minutes, providing high resolution in situ measurements of structural changes during the crystallization process. The data indicate a co-precipitation of the two crystalline phases anatase and rutile within the first 30 minutes of heating, followed by a gradual phase transition from anatase to rutile during particle coarsening throughout the 10 hour duration of an experiment. The co-existence of anatase and rutile at the onset of crystallization lends additional support to the assertion of nearly identical free energies for anatase and rutile at the nanoscale, believed to be due to the prominence of surface energy effects (Ranade et al., 2001). Whole pattern analyses using the Rietveld refinement method also documented previously unobserved changes in lattice parameters of both phases during growth, on the order of 0.2-0.3 % expansion for each axis. The trends in lattice parameters are observed to be temperature dependent, generally having lower values at higher crystallization temperature. In addition to increased surface energy, these small but measurable structural changes may be partially responsible for the observed reversals in thermodynamic stability between crystalline Ti oxide phases at very small particle sizes.

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

NASA Astrophysics Data System (ADS)

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

2012-12-01

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

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

Tetragonal deformation of the hexagonal myofilament matrix in single skinned skeletal muscle fibres owing to change in sarcomere length.

PubMed

Schiereck, P; de Beer, E L; Grundeman, R L; Manussen, T; Kylstra, N; Bras, W

1992-10-01

Single skinned skeletal muscle fibres were immersed in solutions containing two different levels of activator calcium (pCa: 4.4; 6.0). Sarcomere length was varied from 1.6 to 3.5 microns and recorded by laser diffraction. Slack length was 2.0 microns. Small-angle equatorial X-ray diffraction patterns of relaxed and activated fibres at different sarcomere lengths were recorded using synchrotron radiation. The position and amplitude of the diffraction peaks were calculated from the spectra based on the hexagonal arrangement of the myofilament matrix, relating the position of the (1.0)- and (1.1)-diffraction peaks in this model by square root of 3. The diffraction peaks were fitted by five Gaussian functions (1.0, 1.1, 2.0, 2.1 and Z-line) and residual background was corrected by means of a hyperbola. The coupling of the position of the (1.0)- and (1.1)-peak was expressed as a factor: FAC = [d(1.0)/d(1.1)]/square root 3. In the relaxed state this coupling factor decreased at increasing sarcomere length (0.9880 +/- 0.002 at 2.0 microns; 0.900 +/- 0.01 at 3.5 microns). The coupling factor tends toward the one that will be obtained from the squared structure of actin filaments near the Z-discs. At shorter sarcomere lengths a decrease of the coupling factor has also been seen (0.9600 +/- 0.005 at 1.6 microns), giving rise to an increased uniform deformation of the hexagonal matrix, when sarcomere length is changed from slack length. From these experiments we conclude that a change in sarcomere length (from slack length) increases the deformation of the actin-myosin matrix to a tetragonal lattice.

Evaluation of the UFXC32k photon-counting detector for pump-probe experiments using synchrotron radiation.

PubMed

Koziol, Anna; Bordessoule, Michel; Ciavardini, Alessandra; Dawiec, Arkadiusz; Da Silva, Paulo; Desjardins, Kewin; Grybos, Pawel; Kanoute, Brahim; Laulhe, Claire; Maj, Piotr; Menneglier, Claude; Mercere, Pascal; Orsini, Fabienne; Szczygiel, Robert

2018-03-01

This paper presents the performance of a single-photon-counting hybrid pixel X-ray detector with synchrotron radiation. The camera was evaluated with respect to time-resolved experiments, namely pump-probe-probe experiments held at SOLEIL. The UFXC camera shows very good energy resolution of around 1.5 keV and allows the minimum threshold setting to be as low as 3 keV keeping the high-count-rate capabilities. Measurements of a synchrotron characteristic filling mode prove the proper separation of an isolated bunch of photons and the usability of the detector in time-resolved experiments.

High resolution diffraction imaging of crystals grown in microgravity and closely related terrestrial crystals

NASA Technical Reports Server (NTRS)

Steiner, B.; Dobbyn, R.; Black, D.; Burdette, H.; Kuriyama, M.; Spal, R.; Vandenberg, L.; Fripp, A.; Simchick, R.; Lal, R.

1991-01-01

Irregularities found in three crystals grown in space, in four crystals grown entirely on the ground were examined and compared. Irregularities were observed in mercuric iodide, lead tin telluride, triglycine sulfate, and gallium arsenide by high resolution synchrotron x radiation diffraction imaging. Radiation detectors made from mercuric iodide crystals grown in microgravity were reported to perform far better than conventional detectors grown from the same material under full gravity. Effort is now underway to reproduce these 'space' crystals, optimize their properties, and extend comparable superiority to other types of materials.

Temperature dependence of helium-implantation-induced lattice swelling in polycrystalline tungsten: X-ray micro-diffraction and Eigenstrain modelling

DOE PAGES

de Broglie, I.; Beck, C. E.; Liu, W.; ...

2015-05-30

Using synchrotron X-ray micro-diffraction and Eigenstrain analysis the distribution of lattice swelling near grain boundaries in helium-implanted polycrystalline tungsten is quantified. Samples heat-treated at up to 1473 K after implantation show less uniform lattice swelling that varies significantly from grain to grain compared to as-implanted samples. An increase in lattice swelling is found in the vicinity of some grain boundaries, even at depths beyond the implanted layer. As a result, these findings are discussed in terms of the evolution of helium-ion-implantation-induced defects.

Temperature dependence of helium-implantation-induced lattice swelling in polycrystalline tungsten: X-ray micro-diffraction and Eigenstrain modelling

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

de Broglie, I.; Beck, C. E.; Liu, W.

Using synchrotron X-ray micro-diffraction and Eigenstrain analysis the distribution of lattice swelling near grain boundaries in helium-implanted polycrystalline tungsten is quantified. Samples heat-treated at up to 1473 K after implantation show less uniform lattice swelling that varies significantly from grain to grain compared to as-implanted samples. An increase in lattice swelling is found in the vicinity of some grain boundaries, even at depths beyond the implanted layer. As a result, these findings are discussed in terms of the evolution of helium-ion-implantation-induced defects.

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.

Exploring Jupiter's icy moons with old techniques and big facilities - new insights on sulfuric acid hydrates

NASA Astrophysics Data System (ADS)

Maynard-Casely, H. E.; Avdeev, M.; Brand, H.; Wallwork, K.

2013-12-01

Sulfuric acid hydrates have been proposed to be abundant on the surface of Europa [1], and hence would be important planetary forming materials for this moon and its companions Ganymede and Callisto. Understanding of the surface features and subsurface of these moons could be advanced by firmer knowledge of the icy materials that comprise them [2], insight into which can be drawn from firmer knowledge of physical properties and phase behaviour of the candidate materials. We wish to present results from a study that started with the question ';What form of sulfuric acid hydrate would form on the surface of Europa'. The intrinsic hydrogen-domination of planetary ices, makes studying these materials with laboratory powder diffraction very challenging. Insights into their crystalline phase behavior and the extraction of a number of thermal and mechanical properties is often only accessible with high-flux synchrotron x-ray diffraction and utilization of the large scattering cross section with neutron diffraction. We have used the Powder Diffraction beamline at Australian synchrotron [4] and the Echidna (High-resolution neutron powder diffraction) instrument of the Australian Nuclear Science and Technology Organization, [5] to obtain an number of new insights into the crystalline phases formed from sulfruic acid and water mixtures. These instruments have enabled the discovery a new water-rich sulfuric acid hydrate form [6], improved structural characterisation of existing forms [7] and a charting the phase diagram of this fundamental binary system [8]. This has revealed exciting potential for understanding more about the surface of Europa from space, perhaps even providing a window into its past. [1] Carlson, R.W., R.E. Johnson, and M.S. Anderson, Science, 1999. 286(5437): p. 97-99. [2] Fortes, A.D. and M. Choukroun. Space Sci Rev, 2010. 153(1-4): p. 185-218. [3] Blake, D., et al., Space Sci Rev,, 2012. 170(1-4): p. 341-399. [4] Wallwork, K.S., Kennedy B. J. and Wang, D., AIP Conf Proc, 2007. 879: p. 879-882. [5] Liss, K.D., et al., Phys B-Cond Mat, 2006. 385-86: p. 1010-1012. [6] Maynard-Casely, H.E., K.S. Wallwork, and M. Avdeev, (In review). [7] Maynard-Casely, H.E., H.E.A. Brand, and K.S. Wallwork, J.of App.Cryst, 2012. 45: p.1198-1207. [8] Maynard-Casely, H.E., K.S. Wallwork, and H.E.A. Brand, (In Preparation). Stages of the crystal structure determination of sulfruic acid octahydrate a) the oxygen and sulfur postions were determined from the synchrotron x-ray data b) Once neutron diffraction data was collected Fourier difference methods were used to locate hydrogen positions to determine c) the full structure of sulfuric acid octahydrate.

Examination of Short- and Long-Range Atomic Order Nanocrystalline SiC and Diamond by Powder Diffraction Methods

NASA Technical Reports Server (NTRS)

Palosz, B.; Grzanka, E.; Stelmakh, S.; Gierlotka, S.; Weber, H.-P.; Proffen, T.; Palosz, W.

2002-01-01

The real atomic structure of nanocrystals determines unique, key properties of the materials. Determination of the structure presents a challenge due to inherent limitations of standard powder diffraction techniques when applied to nanocrystals. Alternate methodology of the structural analysis of nanocrystals (several nanometers in size) based on Bragg-like scattering and called the "apparent lattice parameter" (alp) is proposed. Application of the alp methodology to examination of the core-shell model of nanocrystals will be presented. The results of application of the alp method to structural analysis of several nanopowders were complemented by those obtained by determination of the Atomic Pair Distribution Function, PDF. Based on synchrotron and neutron diffraction data measured in a large diffraction vector of up to Q = 25 Angstroms(exp -1), the surface stresses in nanocrystalline diamond and SiC were evaluated.

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.

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.

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.

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.

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.

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.

Predicting In-Situ X-ray Diffraction for the SrTiO3/Liquid Interface from First Principles

NASA Astrophysics Data System (ADS)

Letchworth-Weaver, Kendra; Gunceler, Deniz; Sundararaman, Ravishankar; Huang, Xin; Brock, Joel; Arias, T. A.

2013-03-01

Recent advances in experimental techniques, such as in-situ x-ray diffraction, allow researchers to probe the solid-liquid interface in electrochemical systems under operating conditions. These advances offer an unprecedented opportunity for theory to predict properties of electrode materials in aqueous environments and inform the design of energy conversion and storage devices. To compare with experiment, these theoretical studies require microscopic details of both the liquid and the electrode surface. Joint Density Functional Theory (JDFT), a computationally efficient alternative to molecular dynamics, couples a classical density-functional, which captures molecular structure of the liquid, to a quantum-mechanical functional for the electrode surface. We present a JDFT exploration of SrTiO3, which can catalyze solar-driven water splitting, in an electrochemical environment. We determine the geometry of the polar SrTiO3 surface and the equilibrium structure of the contacting liquid, as well as the influence of the liquid upon the electronic structure of the surface. We then predict the effect of the fluid environment on x-ray diffraction patterns and compare our predictions to in-situ measurements performed at the Cornell High Energy Synchrotron Source (CHESS). This material is based upon work supported by the Energy Materials Center at Cornell (EMC2), an Energy Frontier Research Center funded by the U.S. Department of Energy.

WavePropaGator: interactive framework for X-ray free-electron laser optics design and simulations.

PubMed

Samoylova, Liubov; Buzmakov, Alexey; Chubar, Oleg; Sinn, Harald

2016-08-01

This article describes the WavePropaGator ( WPG ) package, a new interactive software framework for coherent and partially coherent X-ray wavefront propagation simulations. The package has been developed at European XFEL for users at the existing and emerging free-electron laser (FEL) facilities, as well as at the third-generation synchrotron sources and future diffraction-limited storage rings. The WPG addresses the needs of beamline scientists and user groups to facilitate the design, optimization and improvement of X-ray optics to meet their experimental requirements. The package uses the Synchrotron Radiation Workshop ( SRW ) C/C++ library and its Python binding for numerical wavefront propagation simulations. The framework runs reliably under Linux, Microsoft Windows 7 and Apple Mac OS X and is distributed under an open-source license. The available tools allow for varying source parameters and optics layouts and visualizing the results interactively. The wavefront history structure can be used for tracking changes in every particular wavefront during propagation. The batch propagation mode enables processing of multiple wavefronts in workflow mode. The paper presents a general description of the package and gives some recent application examples, including modeling of full X-ray FEL beamlines and start-to-end simulation of experiments.

Synchronizing flash-melting in a diamond cell with synchrotron X ray diffraction (XRD)

NASA Astrophysics Data System (ADS)

Karandikar, Amol; Boehler, Reinhard; Meng, Yue; Rod, Eric; Shen, Guoyin

2013-06-01

The major challenges in measuring melting temperatures in laser heated diamond cells are sample instability, thermal runaway and chemical reactions. To circumvent these problems, we developed a ``flash heating'' method using a modulated CW fiber laser and fast X ray detection capability at APS (Pilatus 1M detector). As an example, Pt spheres of 5 micron diameter were loaded in a single crystal sapphire encapsulation in the diamond cell at 65 GPa and heated in a single flash heating event for 20 ms to reach a desired temperature. A CCD spectrometer and the Pilatus were synchronized to measure the temperature and the XRD signal, respectively, when the sample reached the thermal steady state. Each successive flash heating was done at a higher temperature. The integrated XRD pattern, collected during and after (300 K) each heating, showed no chemical reaction up to 3639 K, the highest temperature reached in the experiment. Pt111 and 200 peak intensity variation showed gradual recrystalization and complete diminishing at about 3600 K, indicating melting. Thus, synchronized flash heating with novel sample encapsulation circumvents previous notorious problems and enables accurate melting temperature measurement in the diamond cell using synchrotron XRD probe. Affiliation 2: Geowissenschaeften, Goethe-Universitaet, Altenhoeferallee 1, D-60438 Frankfurt a.M., Germany.

Pargasite at high pressure and temperature

NASA Astrophysics Data System (ADS)

Comboni, Davide; Lotti, Paolo; Gatta, G. Diego; Merlini, Marco; Liermann, Hanns-Peter; Frost, Daniel J.

2017-08-01

The P-T phase stability field, the thermoelastic behavior and the P-induced deformation mechanisms at the atomic scale of pargasite crystals, from the "phlogopite peridotite unit" of the Finero mafic-ultramafic complex (Ivrea-Verbano Formation, Italy), have been investigated by a series of in situ experiments: (a) at high pressure (up to 20.1 GPa), by single-crystal synchrotron X-ray diffraction with a diamond anvil cell, (b) at high temperature (up to 823 K), by powder synchrotron X-ray diffraction using a hot air blower device, and (c) at simultaneous HP-HT conditions, by single-crystal synchrotron X-ray diffraction with a resistive-heated diamond anvil cell (P max = 16.5 GPa, T max = 1200 K). No phase transition has been observed within the P-T range investigated. At ambient T, the refined compressional parameters, calculated by fitting a second-order Birch-Murnaghan Equation of State (BM-EoS), are: V 0 = 915.2(8) Å3 and K P0,T0 = 95(2) GPa (β P0,T0 = 0.0121(2) GPa-1) for the unit-cell volume; a 0 = 9.909(4) Å and K(a) P0,T0 = 76(2) GPa for the a-axis; b 0 = 18.066(7) Å and K(b) P0,T0 = 111(2) GPa for the b-axis; c 0 = 5.299(5) Å and K(c) P0,T0 = 122(12) GPa for the c-axis [K(c) P0,T0 K(b) P0,T0 > K(a) P0,T0]. The high-pressure structure refinements (at ambient T) show a moderate contraction of the TO4 double chain and a decrease of its bending in response to the hydrostatic compression, along with a pronounced compressibility of the A- and M(4)-polyhedra [K P0, T0(A) = 38(2) GPa, K P0, T0(M4) = 79(5) GPa] if compared to the M(1)-, M(2)-, M(3)-octahedra [K P0, T0(M1,2,3) ≤ 120 GPa] and to the rigid tetrahedra [K P0, T0(T1,T2) 300 GPa]. The thermal behavior, at ambient pressure up to 823 K, was modelled with Berman's formalism, which gives: V 0 = 909.1(2) Å3, α0 = 2.7(2)·10-5 K-1 and α1 = 1.4(6)·10-9 K-2 [with α0(a) = 0.47(6)·10-5 K-1, α0(b) = 1.07(4)·10-5 K-1, and α0(c) = 0.97(7)·10-5 K-1]. The petrological implications for the experimental findings of this study are discussed.

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.

Determination of the occurrence of gold in an unoxidized Carlin-type ore sample using synchrotron radiation

USGS Publications Warehouse

Chen, J.R.; Chao, E.C.T.; Minkin, J.A.; Back, J.M.; Bagby, W.C.; Rivers, M.L.; Sutton, S.R.; Gordon, B.M.; Hanson, A.L.; Jones, K.W.

1987-01-01

The occurrence of the so-called invisible gold in two unoxidized Carlin-type gold samples from Nevada has been determined using synchrotron X-ray fluorescence (SXRF) analysis at the National Synchrotron Light Source, Brookhaven National Laboratory. A bedded sample from the East ore zone of the Carlin deposit and a breccia sample from Horse Canyon were analyzed. Preliminary results show that gold is found only in the Horse Canyon breccia sample. Experimental details including other X-ray line and diffraction peak interferences, standards used, and minimum detection limits (MDLs) are discussed. Gold, with a MDL range of 0.8 to 3 ppm, was not detected in euhedral pyrite crystals except in the interior porous portion of one grain. Gold was detected in some parts of the matrix. The phase which contains gold has not yet been identified. The highest content of gold so far analyzed is about 40 ppm. There are interesting implications of these new findings. ?? 1987.

Chemical mapping of paleontological and archeological artifacts with synchrotron X-rays.

PubMed

Bergmann, Uwe; Manning, Phillip L; Wogelius, Roy A

2012-01-01

The application of the recently developed synchrotron rapid scanning X-ray fluorescence (SRS-XRF) technique to the mapping of large objects is the focus of this review. We discuss the advantages of SRS-XRF over traditional systems and the use of other synchrotron radiation (SR) techniques to provide corroborating spectroscopic and diffraction analyses during the same analytical session. After reviewing routine techniques used to analyze precious specimens, we present several case studies that show how SR-based methods have been successfully applied in archeology and paleontology. For example, SRS-XRF imaging of a seventh-century Qur'ān palimpsest and an overpainted original opera score from Luigi Cherubini is described. We also review the recent discovery of soft-tissue residue in fossils of Archaeopteryx and an ancient reptile, as well as work that has successfully resolved the remnants of pigment in Confuciusornis sanctus, a 120-million-year-old fossil of the oldest documented bird with a fully derived avian beak.

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

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

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

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

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

Combined resistive and laser heating technique for in situ radial X-ray diffraction in the diamond anvil cell at high pressure and temperature

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

Miyagi, Lowell; Department of Earth Sciences, Montana State University, Bozeman, Montana 59717; Kanitpanyacharoen, Waruntorn

2013-02-15

To extend the range of high-temperature, high-pressure studies within the diamond anvil cell, a Liermann-type diamond anvil cell with radial diffraction geometry (rDAC) was redesigned and developed for synchrotron X-ray diffraction experiments at beamline 12.2.2 of the Advanced Light Source. The rDAC, equipped with graphite heating arrays, allows simultaneous resistive and laser heating while the material is subjected to high pressure. The goals are both to extend the temperature range of external (resistive) heating and to produce environments with lower temperature gradients in a simultaneously resistive- and laser-heated rDAC. Three different geomaterials were used as pilot samples to calibrate andmore » optimize conditions for combined resistive and laser heating. For example, in Run1, FeO was loaded in a boron-mica gasket and compressed to 11 GPa then gradually resistively heated to 1007 K (1073 K at the diamond side). The laser heating was further applied to FeO to raise temperature to 2273 K. In Run2, Fe-Ni alloy was compressed to 18 GPa and resistively heated to 1785 K (1973 K at the diamond side). The combined resistive and laser heating was successfully performed again on (Mg{sub 0.9}Fe{sub 0.1})O in Run3. In this instance, the sample was loaded in a boron-kapton gasket, compressed to 29 GPa, resistive-heated up to 1007 K (1073 K at the diamond side), and further simultaneously laser-heated to achieve a temperature in excess of 2273 K at the sample position. Diffraction patterns obtained from the experiments were deconvoluted using the Rietveld method and quantified for lattice preferred orientation of each material under extreme conditions and during phase transformation.« less

An instrument for in situ coherent x-ray studies of metal-organic vapor phase epitaxy of III-nitrides.

PubMed

Ju, Guangxu; Highland, Matthew J; Yanguas-Gil, Angel; Thompson, Carol; Eastman, Jeffrey A; Zhou, Hua; Brennan, Sean M; Stephenson, G Brian; Fuoss, Paul H

2017-03-01

We describe an instrument that exploits the ongoing revolution in synchrotron sources, optics, and detectors to enable in situ studies of metal-organic vapor phase epitaxy (MOVPE) growth of III-nitride materials using coherent x-ray methods. The system includes high-resolution positioning of the sample and detector including full rotations, an x-ray transparent chamber wall for incident and diffracted beam access over a wide angular range, and minimal thermal sample motion, giving the sub-micron positional stability and reproducibility needed for coherent x-ray studies. The instrument enables surface x-ray photon correlation spectroscopy, microbeam diffraction, and coherent diffraction imaging of atomic-scale surface and film structure and dynamics during growth, to provide fundamental understanding of MOVPE processes.

An instrument for in situ coherent x-ray studies of metal-organic vapor phase epitaxy of III-nitrides

NASA Astrophysics Data System (ADS)

Ju, Guangxu; Highland, Matthew J.; Yanguas-Gil, Angel; Thompson, Carol; Eastman, Jeffrey A.; Zhou, Hua; Brennan, Sean M.; Stephenson, G. Brian; Fuoss, Paul H.

2017-03-01

We describe an instrument that exploits the ongoing revolution in synchrotron sources, optics, and detectors to enable in situ studies of metal-organic vapor phase epitaxy (MOVPE) growth of III-nitride materials using coherent x-ray methods. The system includes high-resolution positioning of the sample and detector including full rotations, an x-ray transparent chamber wall for incident and diffracted beam access over a wide angular range, and minimal thermal sample motion, giving the sub-micron positional stability and reproducibility needed for coherent x-ray studies. The instrument enables surface x-ray photon correlation spectroscopy, microbeam diffraction, and coherent diffraction imaging of atomic-scale surface and film structure and dynamics during growth, to provide fundamental understanding of MOVPE processes.

Pressure, stress, and strain distribution in the double-stage diamond anvil cell

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

Lobanov, Sergey S., E-mail: slobanov@carnegiescience.edu; V.S. Sobolev Institute of Geology and Mineralogy SB RAS, Novosibirsk 630090; Prakapenka, Vitali B.

Double stage diamond anvil cells (DACs) of two designs have been assembled and tested. We used a standard symmetric DAC with flat or beveled culets as a primary stage and CVD microanvils machined by a focused ion beam as a second. We evaluated pressure, stress, and strain distributions in gold and a mixture of gold and iron as well as in secondary anvils using synchrotron x-ray diffraction with a micro-focused beam. A maximum pressure of 240 GPa was reached independent of the first stage anvil culet size. We found that the stress field generated by the second stage anvils is typicalmore » of conventional DAC experiments. The maximum pressures reached are limited by strains developing in the secondary anvil and by cupping of the first stage diamond anvil in the presented experimental designs. Also, our experiments show that pressures of several megabars may be reached without sacrificing the first stage diamond anvils.« less

Parallel ptychographic reconstruction

DOE PAGES

Nashed, Youssef S. G.; Vine, David J.; Peterka, Tom; ...

2014-12-19

Ptychography is an imaging method whereby a coherent beam is scanned across an object, and an image is obtained by iterative phasing of the set of diffraction patterns. It is able to be used to image extended objects at a resolution limited by scattering strength of the object and detector geometry, rather than at an optics-imposed limit. As technical advances allow larger fields to be imaged, computational challenges arise for reconstructing the correspondingly larger data volumes, yet at the same time there is also a need to deliver reconstructed images immediately so that one can evaluate the next steps tomore » take in an experiment. Here we present a parallel method for real-time ptychographic phase retrieval. It uses a hybrid parallel strategy to divide the computation between multiple graphics processing units (GPUs) and then employs novel techniques to merge sub-datasets into a single complex phase and amplitude image. Results are shown on a simulated specimen and a real dataset from an X-ray experiment conducted at a synchrotron light source.« less

Mechanical behavior of cellulose microfibrils in tension wood, in relation with maturation stress generation.

PubMed

Clair, Bruno; Alméras, Tancrède; Yamamoto, Hiroyuki; Okuyama, Takashi; Sugiyama, Junji

2006-08-01

A change in cellulose lattice spacing can be detected during the release of wood maturation stress by synchrotron x-ray diffraction experiment. The lattice strain was found to be the same order of magnitude as the macroscopic strain. The fiber repeat distance, 1.033 nm evaluated for tension wood after the release of maturation stress was equal to the conventional wood values, whereas the value before stress release was larger, corresponding to a fiber repeat of 1.035 nm, nearly equal to that of cotton and ramie. Interestingly, the fiber repeat varied from 1.033 nm for wood to 1.040 nm for algal cellulose, with an increasing order of lateral size of cellulose microfibrils so far reported. These lines of experiments demonstrate that, before the stress release, the cellulose was in a state of tension, which is, to our knowledge, the first experimental evidence supporting the assumption that tension is induced in cellulose microfibrils.

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

Structural studies on Pax-8 Prd domain/DNA complex.

PubMed

Campagnolo, M; Pesaresi, A; Zelezetsky, I; Geremia, S; Randaccio, L; Bisca, A; Tell, G

2007-04-01

Pax-8 is a member of the Pax family of transcription factors and is essential in the development of thyroid follicular cells. Pax-8 has two DNA-binding domains: the paired domain and the homeo domain. In this study, a preliminary X-ray diffraction analysis of the mammalian Pax-8 paired domain in complex with the C-site of the thyroglobulin promoter was achieved. The Pax-8 paired domain was crystallized by the hanging-drop vapor-diffusion method in complex with both a blunt-ended 26 bp DNA fragment and with a sticky-ended 24 bp DNA fragment with two additional overhanging bases. Crystallization experiments make clear that the growth of transparent crystals with large dimensions and regular shape is particularly influenced by ionic strength. The crystals of Pax-8 complex with blunt-ended and sticky-ended DNA, diffracted synchrotron radiation to 6.0 and 8.0 A resolution and belongs both to the C centered monoclinic system with cell dimensions: a = 89.88 A, b = 80.05 A, c = 67.73 A, and beta = 124.3 degrees and a = 256.56, b = 69.07, c = 99.32 A, and beta = 98.1 degrees , respectively. Fluorescence experiments suggest that the crystalline disorder, deduced by the poor diffraction, can be attributed to the low homogeneity of the protein-DNA sample. The theoretical comparative model of the Pax-8 paired domain complexed with the C-site of the thyroglobulin promoter shows the probable presence of some specific protein-DNA interactions already observed in other Pax proteins and the important role of the cysteine residues of PAI subdomain in the redox control of the DNA recognition.

Support for Synchrotron Access by Environmental Scientists

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

Daly, Michael; Madden, Andrew; Palumbo, Anthony

2006-06-01

To support ERSP-funded scientists in all aspects of synchrotron-based research at the Advanced Photon Source (APS). This support comes in one or more of the following forms: (1) writing proposals to the APS General User (GU) program, (2) providing time at MRCAT/EnviroCAT beamlines via the membership of the Molecular Environmental Science (MES) Group in MRCAT/EnviroCAT, (3) assistance in experimental design and sample preparation, (4) support at the beamline during the synchrotron experiment, (5) analysis and interpretation of the synchrotron data, and (6) integration of synchrotron experimental results into manuscripts.