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Sample records for in-situ synchrotron x-ray

  1. In situ synchrotron based x-ray techniques as monitoring tools for atomic layer deposition

    SciTech Connect

    Devloo-Casier, Kilian Detavernier, Christophe; Dendooven, Jolien

    2014-01-15

    Atomic layer deposition (ALD) is a thin film deposition technique that has been studied with a variety of in situ techniques. By exploiting the high photon flux and energy tunability of synchrotron based x-rays, a variety of new in situ techniques become available. X-ray reflectivity, grazing incidence small angle x-ray scattering, x-ray diffraction, x-ray fluorescence, x-ray absorption spectroscopy, and x-ray photoelectron spectroscopy are reviewed as possible in situ techniques during ALD. All these techniques are especially sensitive to changes on the (sub-)nanometer scale, allowing a unique insight into different aspects of the ALD growth mechanisms.

  2. Nitride-MBE system for in situ synchrotron X-ray measurements

    NASA Astrophysics Data System (ADS)

    Sasaki, Takuo; Ishikawa, Fumitaro; Yamaguchi, Tomohiro; Takahasi, Masamitu

    2016-05-01

    A molecular beam epitaxy (MBE) chamber dedicated to nitride growth was developed at the synchrotron radiation facility SPring-8. This chamber has two beryllium windows for incident and outgoing X-rays, and is directly connected to an X-ray diffractometer, enabling in situ synchrotron X-ray measurements during the nitride growth. Experimental results on initial growth dynamics in GaN/SiC, AlN/SiC, and InN/GaN heteroepitaxy were presented. We achieved high-speed and high-sensitivity reciprocal space mapping with a thickness resolution of atomic-layer scale. This in situ measurement using the high-brilliance synchrotron light source will be useful for evaluating structural variations in the initial growth stage of nitride semiconductors.

  3. In-situ synchrotron x-ray transmission microscopy of the sintering of multilayers

    NASA Astrophysics Data System (ADS)

    Yan, Zilin; Guillon, Olivier; Martin, Christophe L.; Wang, Steve; Lee, Chul-Seung; Bouvard, Didier

    2013-06-01

    This letter reports on in-situ characterization of the high temperature sintering of multilayer ceramic capacitors by high-resolution synchrotron x-ray imaging. Microstructural evolution was obtained in real time by a continuous recording of 2-dimensional radiographs. Anisotropic strains were measured for different layers. Quantification of defects was conducted with 3-dimensional nano-computed tomography. These in-situ observations prove that electrode discontinuities occur at the early stage of sintering and originate from initial heterogeneities linked to the particulate nature of the starting powders.

  4. In situ synchrotron radiation X-ray microspectroscopy of polymer microcontainers.

    PubMed

    Graf-Zeiler, Birgit; Fink, Rainer H; Tzvetkov, George

    2011-12-23

    Direct, real-time analytical techniques that provide high-resolution information on the chemical composition and submicrometer structure of various polymer micro- and nanoparticles are in high demand in a range of life science disciplines. Synchrotron-based scanning transmission X-ray microspectroscopy (STXM) combines both local-spot chemical information (assessed via near-edge X-ray absorption fine structure spectroscopy) and imaging with resolution of several tens of nanometers, and thus can yield new insights into the nanoscale properties of these materials. Furthermore, this method allows in situ examination of soft-matter samples in aqueous/gaseous environments and under external stimuli, such as temperature, pressure, ultrasound, and light irradiation. This Minireview highlights some recent progress in the application of the STXM technique to study the temperature-dependent behavior of polymer core-shell microcapsules and to characterize the physicochemical properties of the supporting shells of gas-filled microbubbles in their natural hydrated state.

  5. Development of a speckle-based portable device for in situ metrology of synchrotron X-ray mirrors.

    PubMed

    Kashyap, Yogesh; Wang, Hongchang; Sawhney, Kawal

    2016-09-01

    A portable device for in situ metrology of synchrotron X-ray mirrors based on the near-field speckle scanning technique has been developed. Ultra-high angular sensitivity is achieved by scanning a piece of abrasive paper or filter membrane in the X-ray beam. In addition to the compact setup and ease of implementation, a user-friendly graphical user interface has been developed to ensure that optimizing active X-ray mirrors is simple and fast. The functionality and feasibility of this device have been demonstrated by characterizing and optimizing X-ray mirrors. PMID:27577767

  6. Development of a speckle-based portable device for in situ metrology of synchrotron X-ray mirrors.

    PubMed

    Kashyap, Yogesh; Wang, Hongchang; Sawhney, Kawal

    2016-09-01

    A portable device for in situ metrology of synchrotron X-ray mirrors based on the near-field speckle scanning technique has been developed. Ultra-high angular sensitivity is achieved by scanning a piece of abrasive paper or filter membrane in the X-ray beam. In addition to the compact setup and ease of implementation, a user-friendly graphical user interface has been developed to ensure that optimizing active X-ray mirrors is simple and fast. The functionality and feasibility of this device have been demonstrated by characterizing and optimizing X-ray mirrors.

  7. Development of a speckle-based portable device for in situ metrology of synchrotron X-ray mirrors

    PubMed Central

    Kashyap, Yogesh; Wang, Hongchang; Sawhney, Kawal

    2016-01-01

    A portable device for in situ metrology of synchrotron X-ray mirrors based on the near-field speckle scanning technique has been developed. Ultra-high angular sensitivity is achieved by scanning a piece of abrasive paper or filter membrane in the X-ray beam. In addition to the compact setup and ease of implementation, a user-friendly graphical user interface has been developed to ensure that optimizing active X-ray mirrors is simple and fast. The functionality and feasibility of this device have been demonstrated by characterizing and optimizing X-ray mirrors. PMID:27577767

  8. Development of an in situ temperature stage for synchrotron X-ray spectromicroscopy

    NASA Astrophysics Data System (ADS)

    Chakraborty, R.; Serdy, J.; West, B.; Stuckelberger, M.; Lai, B.; Maser, J.; Bertoni, M. I.; Culpepper, M. L.; Buonassisi, T.

    2015-11-01

    In situ characterization of micro- and nanoscale defects in polycrystalline thin-film materials is required to elucidate the physics governing defect formation and evolution during photovoltaic device fabrication and operation. X-ray fluorescence spectromicroscopy is particularly well-suited to study defects in compound semiconductors, as it has a large information depth appropriate to study thick and complex materials, is sensitive to trace amounts of atomic species, and provides quantitative elemental information, non-destructively. Current in situ methods using this technique typically require extensive sample preparation. In this work, we design and build an in situ temperature stage to study defect kinetics in thin-film solar cells under actual processing conditions, requiring minimal sample preparation. Careful selection of construction materials also enables controlled non-oxidizing atmospheres inside the sample chamber such as H2Se and H2S. Temperature ramp rates of up to 300 °C/min are achieved, with a maximum sample temperature of 600 °C. As a case study, we use the stage for synchrotron X-ray fluorescence spectromicroscopy of CuInxGa1-xSe2 (CIGS) thin-films and demonstrate predictable sample thermal drift for temperatures 25-400 °C, allowing features on the order of the resolution of the measurement technique (125 nm) to be tracked while heating. The stage enables previously unattainable in situ studies of nanoscale defect kinetics under industrially relevant processing conditions, allowing a deeper understanding of the relationship between material processing parameters, materials properties, and device performance.

  9. Development of an in situ temperature stage for synchrotron X-ray spectromicroscopy

    SciTech Connect

    Chakraborty, R. E-mail: buonassisi@mit.edu; Serdy, J.; Culpepper, M. L.; Buonassisi, T. E-mail: buonassisi@mit.edu; West, B.; Stuckelberger, M.; Bertoni, M. I.; Lai, B.; Maser, J.

    2015-11-15

    In situ characterization of micro- and nanoscale defects in polycrystalline thin-film materials is required to elucidate the physics governing defect formation and evolution during photovoltaic device fabrication and operation. X-ray fluorescence spectromicroscopy is particularly well-suited to study defects in compound semiconductors, as it has a large information depth appropriate to study thick and complex materials, is sensitive to trace amounts of atomic species, and provides quantitative elemental information, non-destructively. Current in situ methods using this technique typically require extensive sample preparation. In this work, we design and build an in situ temperature stage to study defect kinetics in thin-film solar cells under actual processing conditions, requiring minimal sample preparation. Careful selection of construction materials also enables controlled non-oxidizing atmospheres inside the sample chamber such as H{sub 2}Se and H{sub 2}S. Temperature ramp rates of up to 300 °C/min are achieved, with a maximum sample temperature of 600 °C. As a case study, we use the stage for synchrotron X-ray fluorescence spectromicroscopy of CuIn{sub x}Ga{sub 1−x}Se{sub 2} (CIGS) thin-films and demonstrate predictable sample thermal drift for temperatures 25–400 °C, allowing features on the order of the resolution of the measurement technique (125 nm) to be tracked while heating. The stage enables previously unattainable in situ studies of nanoscale defect kinetics under industrially relevant processing conditions, allowing a deeper understanding of the relationship between material processing parameters, materials properties, and device performance.

  10. In Situ Synchrotron X-ray Study of Ultrasound Cavitation and Its Effect on Solidification Microstructures

    NASA Astrophysics Data System (ADS)

    Mi, Jiawei; Tan, Dongyue; Lee, Tung Lik

    2015-08-01

    Considerable progress has been made in studying the mechanism and effectiveness of using ultrasound waves to manipulate the solidification microstructures of metallic alloys. However, uncertainties remain in both the underlying physics of how microstructures evolve under ultrasonic waves, and the best technological approach to control the final microstructures and properties. We used the ultrafast synchrotron X-ray phase contrast imaging facility housed at the Advanced Photon Source, Argonne National Laboratory, US to study in situ the highly transient and dynamic interactions between the liquid metal and ultrasonic waves/bubbles. The dynamics of ultrasonic bubbles in liquid metal and their interactions with the solidifying phases in a transparent alloy were captured in situ. The experiments were complemented by the simulations of the acoustic pressure field, the pulsing of the bubbles, and the associated forces acting onto the solidifying dendrites. The study provides more quantitative understanding on how ultrasonic waves/bubbles influence the growth of dendritic grains and promote the grain multiplication effect for grain refinement.

  11. Dynamics of barite growth in porous media quantified by in situ synchrotron X-ray tomography

    NASA Astrophysics Data System (ADS)

    Godinho, jose; Gerke, kirill

    2016-04-01

    Current models used to formulate mineral sequestration strategies of dissolved contaminants in the bedrock often neglect the effect of confinement and the variation of reactive surface area with time. In this work, in situ synchrotron X-ray micro-tomography is used to quantify barite growth rates in a micro-porous structure as a function of time during 13.5 hours with a resolution of 1 μm. Additionally, the 3D porous network at different time frames are used to simulate the flow velocities and calculate the permeability evolution during the experiment. The kinetics of barite growth under porous confinement is compared with the kinetics of barite growth on free surfaces in the same fluid composition. Results are discussed in terms of surface area normalization and the evolution of flow velocities as crystals fill the porous structure. During the initial hours the growth rate measured in porous media is similar to the growth rate on free surfaces. However, as the thinner flow paths clog the growth rate progressively decreases, which is correlated to a decrease of local flow velocity. The largest pores remain open, enabling growth to continue throughout the structure. Quantifying the dynamics of mineral precipitation kinetics in situ in 4D, has revealed the importance of using a time dependent reactive surface area and accounting for the local properties of the porous network, when formulating predictive models of mineral precipitation in porous media.

  12. In situ laser heating and radial synchrotron X-ray diffraction ina diamond anvil cell

    SciTech Connect

    Kunz, Martin; Caldwell, Wendel A.; Miyagi, Lowell; Wenk,Hans-Rudolf

    2007-06-29

    We report a first combination of diamond anvil cell radialx-ray diffraction with in situ laser heating. The laser-heating setup ofALS beamline 12.2.2 was modified to allow one-sided heating of a samplein a diamond anvil cell with an 80 W yttrium lithium fluoride laser whileprobing the sample with radial x-ray diffraction. The diamond anvil cellis placed with its compressional axis vertical, and perpendicular to thebeam. The laser beam is focused onto the sample from the top while thesample is probed with hard x-rays through an x-ray transparentboron-epoxy gasket. The temperature response of preferred orientation of(Fe,Mg)O is probed as a test experiment. Recrystallization was observedabove 1500 K, accompanied by a decrease in stress.

  13. Geological Carbon Sequestration: new insights from in-situ Synchrotron X-ray Microtomography

    NASA Astrophysics Data System (ADS)

    Voltolini, M.; Kwon, T.; Ajo Franklin, J. B.

    2012-12-01

    In a world with rapidly increasing atmospheric CO2 concentrations, a variety of scalable technologies are being considered to mitigate emissions from the combustion of fossil fuels; among these approaches, geological carbon storage (GCS) is being actively tested at a variety of subsurface sites. Despite these activities, a mechanistic understanding of multiphase flow in scCO2/brine systems at the pore scale is still being developed. The distribution of scCO2 in the pore space controls a variety of processes at the continuum scale including CO2 dissolution rate (by way of brine/CO2 contact area), capillary trapping, and residual brine fraction. Virtually no dynamic measurements of the pore-scale distribution of scCO2 in real geological samples have been made in three dimensions leaving models describing multi-phase fluid dynamics, reactive transport, and geophysical properties reliant on analog systems (often using fewer spatial dimensions, different fluids, or lower pressures) or theoretical models describing phase configurations. We present dynamic pore-scale imagery of scCO2 invasion dynamics in a 3D geological sample, in this case a quartz-rich sandstone core extracted from the Domengine Fm, a regionally extensive unit which is currently a target for future GCS operations in the Sacramento Basin. This dataset, acquired using synchrotron X-ray micro tomography (SXR-μCT) and high speed radiography, was made possible by development of a controlled P/T flow-through triaxial cell compatible with X-ray imaging in the 8-40 keV range. These experiments successfully resolved scCO2 and brine phases at a spatial resolution of 4.47 μm while the sample was kept at in situ conditions (45°C, 9 MPa pore pressure, 14 MPa hydrostatic confining stress) during drainage and imbibition cycles. Image volumes of the dry, brine saturated, and partially scCO2 saturated sample were captured and were used to correlate aspects of rock microstructure to development of the invasion front

  14. A modular reactor design for in situ synchrotron x-ray investigation of atomic layer deposition processes

    NASA Astrophysics Data System (ADS)

    Klug, Jeffrey A.; Weimer, Matthew S.; Emery, Jonathan D.; Yanguas-Gil, Angel; Seifert, Sönke; Schlepütz, Christian M.; Martinson, Alex B. F.; Elam, Jeffrey W.; Hock, Adam S.; Proslier, Thomas

    2015-11-01

    Synchrotron characterization techniques provide some of the most powerful tools for the study of film structure and chemistry. The brilliance and tunability of the Advanced Photon Source allow access to scattering and spectroscopic techniques unavailable with in-house laboratory setups and provide the opportunity to probe various atomic layer deposition (ALD) processes in situ starting at the very first deposition cycle. Here, we present the design and implementation of a portable ALD instrument which possesses a modular reactor scheme that enables simple experimental switchover between various beamlines and characterization techniques. As first examples, we present in situ results for (1) X-ray surface scattering and reflectivity measurements of epitaxial ZnO ALD on sapphire, (2) grazing-incidence small angle scattering of MnO nucleation on silicon, and (3) grazing-incidence X-ray absorption spectroscopy of nucleation-regime Er2O3 ALD on amorphous ALD alumina and single crystalline sapphire.

  15. A modular reactor design for in situ synchrotron x-ray investigation of atomic layer deposition processes

    SciTech Connect

    Klug, Jeffrey A. Emery, Jonathan D.; Martinson, Alex B. F.; Proslier, Thomas; Weimer, Matthew S.; Yanguas-Gil, Angel; Elam, Jeffrey W.; Seifert, Sönke; Schlepütz, Christian M.; Hock, Adam S.

    2015-11-15

    Synchrotron characterization techniques provide some of the most powerful tools for the study of film structure and chemistry. The brilliance and tunability of the Advanced Photon Source allow access to scattering and spectroscopic techniques unavailable with in-house laboratory setups and provide the opportunity to probe various atomic layer deposition (ALD) processes in situ starting at the very first deposition cycle. Here, we present the design and implementation of a portable ALD instrument which possesses a modular reactor scheme that enables simple experimental switchover between various beamlines and characterization techniques. As first examples, we present in situ results for (1) X-ray surface scattering and reflectivity measurements of epitaxial ZnO ALD on sapphire, (2) grazing-incidence small angle scattering of MnO nucleation on silicon, and (3) grazing-incidence X-ray absorption spectroscopy of nucleation-regime Er{sub 2}O{sub 3} ALD on amorphous ALD alumina and single crystalline sapphire.

  16. A modular reactor design for in situ synchrotron x-ray investigation of atomic layer deposition processes.

    PubMed

    Klug, Jeffrey A; Weimer, Matthew S; Emery, Jonathan D; Yanguas-Gil, Angel; Seifert, Sönke; Schlepütz, Christian M; Martinson, Alex B F; Elam, Jeffrey W; Hock, Adam S; Proslier, Thomas

    2015-11-01

    Synchrotron characterization techniques provide some of the most powerful tools for the study of film structure and chemistry. The brilliance and tunability of the Advanced Photon Source allow access to scattering and spectroscopic techniques unavailable with in-house laboratory setups and provide the opportunity to probe various atomic layer deposition (ALD) processes in situ starting at the very first deposition cycle. Here, we present the design and implementation of a portable ALD instrument which possesses a modular reactor scheme that enables simple experimental switchover between various beamlines and characterization techniques. As first examples, we present in situ results for (1) X-ray surface scattering and reflectivity measurements of epitaxial ZnO ALD on sapphire, (2) grazing-incidence small angle scattering of MnO nucleation on silicon, and (3) grazing-incidence X-ray absorption spectroscopy of nucleation-regime Er2O3 ALD on amorphous ALD alumina and single crystalline sapphire.

  17. A modular reactor design for in situ synchrotron X-ray investigation of atomic layer deposition processes

    SciTech Connect

    Klug, Jeffrey A.; Weimer, Matthew S.; Emery, Jonathan D.; Yanguas-Gil, Angel; Seifert, Sonke; Schleputz, Christian M.; Martinson, Alex B. F.; Elam, Jeffrey W.; Hock, Adam S.; Proslier, Thomas

    2015-11-01

    Synchrotron characterization techniques provide some of the most powerful tools for the study of film structure and chemistry. The brilliance and tunability of the Advanced Photon Source allow access to scattering and spectroscopic techniques unavailable with in-house laboratory setups and provide the opportunity to probe various atomic layer deposition (ALD) processes in situ starting at the very first deposition cycle. Here, we present the design and implementation of a portable ALD instrument which possesses a modular reactor scheme that enables simple experimental switchover between various beamlines and characterization techniques. As first examples, we present \\textit{in situ} results for 1.) X-ray surface scattering and reflectivity measurements of epitaxial ZnO ALD on sapphire, 2.) grazing-incidence small angle scattering of MnO nucleation on silicon, and 3.) grazing-incidence X-ray absorption spectroscopy of nucleation-regime Er2O3 ALD on amorphous ALD alumina and single crystalline sapphire.

  18. Synchrotron X-Ray Microdiffraction Reveals Intrinsic Structural Features of Amyloid Deposits In Situ

    PubMed Central

    Briki, Fatma; Vérine, Jérôme; Doucet, Jean; Bénas, Philippe; Fayard, Barbara; Delpech, Marc; Grateau, Gilles; Riès-Kautt, Madeleine

    2011-01-01

    Amyloidoses are increasingly recognized as a major public health concern in Western countries. All amyloidoses share common morphological, structural, and tinctorial properties. These consist of staining by specific dyes, a fibrillar aspect in electron microscopy and a typical cross-β folding in x-ray diffraction patterns. Most studies that aim at deciphering the amyloid structure rely on fibers generated in vitro or extracted from tissues using protocols that may modify their intrinsic structure. Therefore, the fine details of the in situ architecture of the deposits remain unknown. Here, we present to our knowledge the first data obtained on ex vivo human renal tissue sections using x-ray microdiffraction. The typical cross-β features from fixed paraffin-embedded samples are similar to those formed in vitro or extracted from tissues. Moreover, the fiber orientation maps obtained across glomerular sections reveal an intrinsic texture that is correlated with the glomerulus morphology. These results are of the highest importance to understanding the formation of amyloid deposits and are thus expected to trigger new incentives for tissue investigation. Moreover, the access to intrinsic structural parameters such as fiber size and orientation using synchrotron x-ray microdiffraction, could provide valuable information concerning in situ mechanisms and deposit formation with potential benefits for diagnostic and therapeutic purposes. PMID:21767502

  19. Phase transitions in freeze-dried systems - quantification using in situ synchrotron X-ray diffractometry

    SciTech Connect

    Varshney, Dushyant B.; Sundaramurthi, Prakash; Kumar, Satyendra; Shalaev, Evgenyi Y.; Kang, Shin-Woong; Gatlin, Larry A.; Suryanarayanan, Raj

    2009-09-02

    The purpose is: (1) To develop a synchrotron X-ray diffraction (SXRD) method to monitor phase transitions during the entire freeze-drying cycle. Aqueous sodium phosphate buffered glycine solutions with initial glycine to buffer molar ratios of 1:3 (17:50 mM), 1:1 (50 mM) and 3:1 were utilized as model systems. (2) To investigate the effect of initial solute concentration on the crystallization of glycine and phosphate buffer salt during lyophilization. Phosphate buffered glycine solutions were placed in a custom-designed sample cell for freeze-drying. The sample cell, covered with a stainless steel dome with a beryllium window, was placed on a stage capable of controlled cooling and vacuum drying. The samples were cooled to -50 C and annealed at -20 C. They underwent primary drying at -25 C under vacuum until ice sublimation was complete and secondary drying from 0 to 25 C. At different stages of the freeze-drying cycle, the samples were periodically exposed to synchrotron X-ray radiation. An image plate detector was used to obtain time-resolved two-dimensional SXRD patterns. The ice, {beta}-glycine and DHPD phases were identified based on their unique X-ray peaks. When the solutions were cooled and annealed, ice formation was followed by crystallization of disodium hydrogen phosphate dodecahydrate (DHPD). In the primary drying stage, a significant increase in DHPD crystallization followed by incomplete dehydration to amorphous disodium hydrogen phosphate was evident. Complete dehydration of DHPD occurred during secondary drying. Glycine crystallization was inhibited throughout freeze-drying when the initial buffer concentration (1:3 glycine to buffer) was higher than that of glycine. A high-intensity X-ray diffraction method was developed to monitor the phase transitions during the entire freeze-drying cycle. The high sensitivity of SXRD allowed us to monitor all the crystalline phases simultaneously. While DHPD crystallizes in frozen solution, it dehydrates

  20. Hydride reorientation in Zircaloy-4 examined by in situ synchrotron X-ray diffraction

    NASA Astrophysics Data System (ADS)

    Weekes, H. E.; Jones, N. G.; Lindley, T. C.; Dye, D.

    2016-09-01

    The phenomenon of stress-reorientation has been investigated using in situ X-ray diffraction during the thermomechanical cycling of hydrided Zircaloy-4 tensile specimens. Results have shown that loading along a sample's transverse direction (TD) leads to a greater degree of hydride reorientation when compared to rolling direction (RD)-aligned samples. The elastic lattice micro-strains associated with radially oriented hydrides have been revealed to be greater than those oriented circumferentially, a consequence of strain accommodation. Evidence of hydride redistribution after cycling, to α-Zr grains oriented in a more favourable orientation when under an applied stress, has also been observed and its behaviour has been found to be highly dependent on the loading axis. Finally, thermomechanical loading across multiple cycles has been shown to reduce the difference in terminal solid solubility of hydrogen during dissolution (TSSD,H) and precipitation (TSSP,H).

  1. Fast in situ phase and stress analysis during laser surface treatment: a synchrotron x-ray diffraction approach.

    PubMed

    Kostov, V; Gibmeier, J; Wilde, F; Staron, P; Rössler, R; Wanner, A

    2012-11-01

    An in situ stress analysis by means of synchrotron x-ray diffraction was carried out during laser surface hardening of steel. A single exposure set-up that based on a special arrangement of two fast silicon strip line detectors was established, allowing for fast stress analysis according to the sin(2)ψ x-ray analysis method. For the in situ experiments a process chamber was designed and manufactured, which is described in detail. First measurements were carried out at the HZG undulator imaging beamline (IBL, beamline P05) at the synchrotron storage ring PETRA III, DESY, Hamburg (Germany). The laser processing was carried out using a 6 kW high power diode laser system. Two different laser optics were compared, a Gaussian optic with a focus spot of ø 3 mm and a homogenizing optic with a rectangular spot dimension of 8 × 8 mm(2). The laser processing was carried out using spot hardening at a heating-/cooling rate of 1000 K/s and was controlled via pyrometric temperature measurement using a control temperature of 1150 °C. The set-up being established during the measuring campaign allowed for this first realization data collection rates of 10Hz. The data evaluation procedure applied enables the separation of thermal from elastic strains and gains unprecedented insight into the laser hardening process.

  2. High-Energy Synchrotron X-Ray Diffraction for In Situ Diffuse Scattering Studies of Bulk Single Crystals

    NASA Astrophysics Data System (ADS)

    Daniels, John E.; Jo, Wook; Donner, Wolfgang

    2012-01-01

    High-energy synchrotron x-ray scattering offers a powerful technique for investigation of single-crystal material structures. Large, mm-sized crystals can be used, allowing complex in situ sample environments to be employed. Here, we demonstrate how this technique can be applied for the collection of single-crystal diffuse scattering volumes from the electro-active material 96%Bi0.5Na0.5TiO3-4%BaTiO3 while electric fields are applied in situ. The data obtained allow correlation of the atomic and nanoscale structures with the observed macroscopic electro-active properties of interest. This article presents a recent study relating the nanoscale stacking fault structure in BNT-BT to the relaxor-ferroelectric nature of the material [Daniels et al. in Appl. Phys. Lett. 98, 252904 (2011)], and extends this study with further experimental description and analysis.

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

    NASA Astrophysics Data System (ADS)

    Chen, Xian; Tamura, Nobumichi; MacDowell, Alastair; James, Richard D.

    2016-05-01

    The alloy Cu25Au30Zn45 undergoes a huge first-order phase transformation (6% strain) and shows a high reversibility under thermal cycling and an unusual martensitc microstructure in sharp contrast to its nearby compositions. This alloy was discovered by systematically tuning the composition so that its lattice parameters satisfy the cofactor conditions (i.e., the kinematic conditions of compatibility between phases). It was conjectured that satisfaction of these conditions is responsible for the enhanced reversibility as well as the observed unusual fluid-like microstructure during transformation, but so far, there has been no direct evidence confirming that these observed microstructures are those predicted by the cofactor conditions. To verify this hypothesis, we use synchrotron X-ray Laue microdiffraction to measure the orientations and structural parameters of variants and phases near the austenite/martensite interface. The areas consisting of both austenite and multi-variants of martensite are scanned by microLaue diffraction. The cofactor conditions have been examined from the kinematic relation of lattice vectors across the interface. The continuity condition of the interface is precisely verified from the correspondent lattice vectors between two phases.

  4. Synchrotron micro-X-ray fluorescence analysis of natural diamonds: First steps in identification of mineral inclusions in situ

    SciTech Connect

    Sitepu, Husin; Kopylova, Maya G.; Quirt, David H.; Cutler, Jeffrey N.; Kotzer, Thomas G.

    2008-06-09

    Diamond inclusions are of particular research interest in mantle petrology and diamond exploration as they provide direct information about the chemical composition of upper and lower mantle and about the petrogenetic sources of diamonds in a given deposit. The objective of the present work is to develop semi-quantitative analytical tools for non-destructive in situ identification and characterization of mineral inclusions in diamonds using synchrotron micro-X-ray Fluorescence ({mu}SXRF) spectroscopy and micro-X-ray Absorption Near Edge Structure ({mu}XANES) spectroscopy at a focused spot size of 4 to 5 micrometers. The data were collected at the Pacific Northwest Consortium (PNC-CAT) 20-ID microprobe beamline at the Advanced Photon Source, located at the Argonne National Laboratory, and yielded the first high-resolution maps of Ti, Cr, Fe, Ni, Cu, and Zn for natural diamond grains, along with quantitative {mu}SXRF analysis of select chemical elements in exposed kimberlite indicator mineral grains. The distribution of diamond inclusions inside the natural diamond host, both visible and invisible using optical transmitted-light microscopy, can be mapped using synchrotron {mu}XRF analysis. Overall, the relative abundances of chemical elements determined by {mu}SXRF elemental analyses are broadly similar to their expected ratios in the mineral and therefore can be used to identify inclusions in diamonds in situ. Synchrotron {mu}XRF quantitative analysis provides accurate estimates of Cr contents of exposed polished minerals when calibrated using the concentration of Fe as a standard. Corresponding Cr K-edge {mu}XANES analyses on selected inclusions yield unique information regarding the formal oxidation state and local coordination of Cr.

  5. In situ and real-time monitoring of mechanochemical milling reactions using synchrotron X-ray diffraction.

    PubMed

    Halasz, Ivan; Kimber, Simon A J; Beldon, Patrick J; Belenguer, Ana M; Adams, Frank; Honkimäki, Veijo; Nightingale, Richard C; Dinnebier, Robert E; Friščić, Tomislav

    2013-09-01

    We describe the only currently available protocol for in situ, real-time monitoring of mechanochemical reactions and intermediates by X-ray powder diffraction. Although mechanochemical reactions (inducing transformations by mechanical forces such as grinding and milling) are normally performed in commercially available milling assemblies, such equipment does not permit direct reaction monitoring. We now describe the design and in-house modification of milling equipment that allows the reaction jars of the operating mill to be placed in the path of a high-energy (∼90 keV) synchrotron X-ray beam while the reaction is taking place. Resulting data are analyzed using conventional software, such as TOPAS. Reaction intermediates and products are identified using the Cambridge Structural Database or Inorganic Crystal Structure Database. Reactions are analyzed by fitting the time-resolved diffractograms using structureless Pawley refinement for crystalline phases that are not fully structurally characterized (such as porous frameworks with disordered guests), or the Rietveld method for solids with fully determined crystal structures (metal oxides, coordination polymers).

  6. Chromium Reaction Mechanisms for Speciation using Synchrotron in-Situ High-Temperature X-ray Diffraction.

    PubMed

    Low, Fiona; Kimpton, Justin; Wilson, Siobhan A; Zhang, Lian

    2015-07-01

    We use in situ high-temperature X-ray diffraction (HT-XRD), ex-situ XRD and synchrotron X-ray absorption near edge structure spectroscopy (XANES) to derive fundamental insights into mechanisms of chromium oxidation during combustion of solid fuels. To mimic the real combustion environment, mixtures of pure eskolaite (Cr(3+)2O3), lime (CaO) and/or kaolinite [Al2Si2O5(OH)4] have been annealed at 600-1200 °C in air versus 1% O2 diluted by N2. Our results confirm for the first time that (1) the optimum temperature for Cr(6+) formation is 800 °C for the coexistence of lime and eskolaite; (2) upon addition of kaolinite into oxide mixture, the temperature required to produce chromatite shifts to 1000 °C with a remarkable reduction in the fraction of Cr(6+). Beyond 1000 °C, transient phases are formed that bear Cr in intermediate valence states, which convert to different species other than Cr(6+) in the cooling stage; (3) of significance to Cr mobility from the waste products generated by combustion, chromatite formed at >1000 °C has a glassy disposition that prevents its water-based leaching; and (4) Increasing temperature facilitates the migration of eskolaite particles into bulk lime and enhances the extent to which Cr(3+) is oxidized, thereby completing the oxidation of Cr(3+) to Cr(6+) within 10 min. PMID:26055512

  7. In-situ X-ray Synchrotron Microtomography: Real Time Pore Structure Evolution during Olivine Carbonation

    NASA Astrophysics Data System (ADS)

    Zhu, W.; Fusseis, F.; Lisabeth, H. P.; Xiao, X.

    2013-12-01

    Mineral carbonation has been proposed as a promising method for long-term, secure sequestration of carbon dioxide. In porous rocks, fluid-rock interactions can significantly alter the pore space and thus exert important controls over the rate and extent of carbonation. We constructed an x-ray transparent pressure cell [Fusseis et al., 2013] to investigate the real time pore structure evolution during mineral carbonation in porous olivine aggregates. In each experiment, a sintered olivine sample was subjected to a confining pressure of 13 MPa and a pore pressure of 10 MPa, with a sodium bicarbonate solution (NaHCO3 at 1.5 M) as pore fluid. At these pressure conditions, the cell was heated to 473 K. Constant pressure and temperature conditions were maintained during the length of the experiments, lasting 72-120 hours. Using a polychromatic beam in the 2-BM upstream hutch at the Advanced Photon Source, 3-dimensional (3-D) microtomography data were collected in 20 seconds with 30-minute interval. A novel phase retrieval reconstruction algorithm [Paganin et al., 2002] was used to reconstruct microtomographic datasets with a voxel size of ~1.1 micron. The microtomography images at different stages of the carbonation process reveal progressive growth of new crystals in the pore space. Integration of a x-ray transparent pressure vessel with flow through capacity and 3-D microtomography provides a novel research direction of studying the coupled chemo-hydro-thermal-mechanical processes in rocks.

  8. In situ synchrotron X-ray diffraction analysis of deformation behaviour in Ti-Ni-based thin films.

    PubMed

    Wang, Hong; Sun, Guangai; Wang, Xiaolin; Chen, Bo; Zu, Xiaotao; Liu, Yanping; Li, Liangbin; Pan, Guoqiang; Sheng, Liusi; Liu, Yaoguang; Fu, Yong Qing

    2015-01-01

    Deformation mechanisms of as-deposited and post-annealed Ti50.2Ni49.6, Ti50.3Ni46.2Cu3.5 and Ti48.5Ni40.8Cu7.5 thin films were investigated using the in situ synchrotron X-ray diffraction technique. Results showed that initial crystalline phases determined the deformation mechanisms of all the films during tensile loading. For the films dominated by monoclinic martensites (B19'), tensile stress induced the detwinning of 〈011〉 type-II twins and resulted in the preferred orientations of (002)B19' parallel to the loading direction (∥ LD) and (020)B19' perpendicular to the LD (⊥ LD). For the films dominated by austenite (B2), the austenite directly transformed into martensitic variants (B19') with preferred orientations of (002)B19' ∥ LD and (020)B19' ⊥ LD. For the Ti50.3Ni46.2Cu3.5 and Ti48.1Ni40.8Cu7.5 films, martensitic transformation temperatures decreased apparently after post-annealing because of the large thermal stress generated in the films due to the large differences in thermal expansion coefficients between the film and substrate. PMID:25537586

  9. In Situ Neutron and Synchrotron X-ray Diffraction Studies of Jarosite at High-Temperature High-Pressure Conditions

    NASA Astrophysics Data System (ADS)

    Xu, H.; Zhao, Y.; Hickmott, D.; Zhang, J.; Vogel, S.; Daemen, L.; Hartl, M.

    2011-03-01

    Jarosite (KFe 3 (SO4)2 (OH)6) occurs in acid mine drainage and epithermal environments and hot springs associated with volcanic activity. Jarosite is also of industrial interest as an iron-impurity extractor from zinc sulfide ores. In 2004, jarosite was detected by the Mars Exploration Rover Mössbauer spectrometer, which has been interpreted as a strong evidence for the existence of water (and possibly life) on ancient Mars. This discovery has spurred considerable interests in stability and structural behavior of jarosite and related phases at various temperature, pressure, and aqueous conditions. In this work, we have investigated the crystal structure and phase stability of jarosite at temperatures up to 900 K and/or pressures up to 9 GPa using in situ neutron and synchrotron X-ray diffraction. To avoid the large incoherent scattering of neutrons by hydrogen, a deuterated sample was synthesized and characterized. Rietveld analysis of the obtained diffraction data allowed determination of unit-cell parameters, atomic positions and atomic displacement parameters as a function of temperature and pressure. In addition, the coefficients of thermal expansion, bulk moduli and pressure-temperature stability regions of jarosite were determined.

  10. A System for Conducting Sophisticated Mechanical Tests in Situ with High Energy Synchrotron X-Rays Final Technical Report

    SciTech Connect

    Jeremy Weiss

    2012-08-02

    This is the final technical report for the SBIR Phase I project titled 'A System for Conducting Sophisticated Mechanical Tests in Situ with High Energy Synchrotron X-Rays.' Experiments using diffraction of synchrotron radiation that help scientists understand engineering material failure modes, such as fracture and fatigue, require specialized machinery. This machinery must be able to induce these failure modes in a material specimen while adhering to strict size, weight, and geometric limitations prescribed by diffraction measurement techniques. During this Phase I project, Mechanical Solutions, Inc. (MSI) developed one such machine capable of applying uniaxial mechanical loading to a material specimen in both tension and compression, with zero backlash while transitioning between the two. Engineers currently compensate for a lack of understanding of fracture and fatigue by employing factors of safety in crucial system components. Thus, mechanical and structural parts are several times bigger, thicker, and heavier than they need to be. The scientific discoveries that result from diffraction experiments which utilize sophisticated mechanical loading devices will allow for broad material, weight, fuel, and cost savings in engineering design across all industries, while reducing the number of catastrophic failures in transportation, power generation, infrastructure, and all other engineering systems. With an existing load frame as the starting point, the research focused on two main areas: (1) the design of a specimen alignment and gripping system that enables pure uniaxial tension and compression loading (and no bending, shear, or torsion), and (2) development of a feedback control system that is adaptive and thus can maintain a load set point despite changing specimen material properties (e.g. a decreasing stiffness during yield).

  11. Understanding Electrocatalytic Pathways in Low and Medium Temperature Fuel Cells: Synchrotron-based In Situ X-Ray Absorption Spectroscopy

    SciTech Connect

    Mukerjee, S.; Ziegelbauer, J; Arruda, T; Ramaker, D; Shyam, B

    2008-01-01

    Over the last few decades, researchers have made significant developments in producing more advanced electrocatalytic materials for power generation applications. For example, traditional fuel cell catalysts often involve high-priced precious metals such as Pt. However, in order for fuel cells to become commercially viable, there is a need to reduce or completely remove precious metal altogether. As a result, a myriad of novel, unconventional materials have been explored such as chalcogenides, porphyrins, and organic-metal-macrocycles for low/medium temperature fuel cells as well as enzymatic and microbial fuel cells. As these materials increasingly become more complex, researchers often find themselves in search of new characterization methods, especially those which are allow in situ and operando measurements with element specificity. One such method that has received much attention for analysis of electrocatalytic materials is X-ray absorption spectroscopy (XAS). XAS is an element specific, core level absorption technique which yields structural and electronic information. As a core electron method, XAS requires an extremely bright source, hence a synchrotron. The resulting intensity of synchrotron radiation allow for experiments to be conducted in situ, under electrochemically relevant conditions. Although a bulk-averaging technique requiring rigorous mathematical manipulation, XAS has the added benefit that it can probe materials which possess no long range order. This makes it ideal to characterize nano-scale electrocatalysts. XAS experiments are conducted by ramping the X-ray photon energy while measuring absorption of the incident beam the sample or by counting fluorescent photons released from a sample due to subsequent relaxation. Absorption mode XAS follows the Beer-Lambert Law, {mu}x = log(I{sub 0}/I{sub t}) (1) where {mu} is the absorption coefficient, x is the sample thickness and I{sub 0} and I{sub t} are the intensities of the incident and

  12. In-situ observation of nickel oxidation using synchrotron based full-field transmission X-ray microscopy

    NASA Astrophysics Data System (ADS)

    Kiss, Andrew M.; Harris, William M.; Wang, Steve; Vila-Comamala, Joan; Deriy, Alex; Chiu, Wilson K. S.

    2013-02-01

    An in situ imaging-based approach is reported to study chemical reactions using full-field transmission x-ray microscopy (TXM). Ni particles were oxidized at temperatures between 400 and 850 °C in the TXM to directly observe their morphology change while the chemical composition is monitored by x-ray absorption near edge spectroscopy. Reaction rates and activation energies are calculated from the image data. The goal of this effort is to better understand Ni oxidation in electrode materials. The approach developed will be an effective technique for directly studying chemical reactions of particles and their behavior at the nano-scale.

  13. Inhomogeneous thermal expansion of metallic glasses in atomic-scale studied by in-situ synchrotron X-ray diffraction

    SciTech Connect

    Taghvaei, Amir Hossein; Shakur Shahabi, Hamed; Bednarčik, Jozef; Eckert, Jürgen

    2015-01-28

    Numerous investigations have demonstrated that the elastic strain in metallic glasses subjected to mechanical loading could be inhomogeneous in the atomic-scale and it increases with distance from an average atom and eventually reaches the macroscopic strain at larger inter-atomic distances. We have observed a similar behavior for the thermal strain imposed by heating of Co{sub 40}Fe{sub 22}Ta{sub 8}B{sub 30} glassy particles below the glass transition temperature by analysis of the scattering data obtained by in-situ high-energy synchrotron X-ray diffraction (XRD). The results imply that the volumetric thermal strains calculated from the shift in position of the principal diffraction maximum and reduced pair correlation function (PDF) peaks are in good agreement for the length scales beyond 0.6 nm, corresponding to the atoms located over the third near-neighbor shell. However, smaller and even negative volumetric thermal strains have been calculated based on the shifts in the positions of the second and first PDF peaks, respectively. The structural changes of Co{sub 40}Fe{sub 22}Ta{sub 8}B{sub 30} glassy particles are accompanied by decreasing the average coordination number of the first near-neighbor shell, which manifests the occurrence of local changes in the short-range order upon heating. It is believed that the detected length-scale dependence of the volumetric thermal strain is correlated with the local atomic rearrangements taking place in the topologically unstable regions of the glass governed by variations in the atomic-level stresses.

  14. In-situ synchrotron x-ray spectroscopy of ruthenium nanoparticles modified with selenium for oxygen reduction reaction.

    SciTech Connect

    Inukai, J.; Cao, D.; Wieckowski, A.; Chang, K.-C.; Menzel, A.; Komanicky, V.; You, H.; Materials Science Division; Univ. of Illinois; Univ. of Yamanashi

    2007-11-15

    We used in situ Se K-edge X-ray spectroscopy to characterize Ru nanoparticles chemically modified with submonolayers of selenium (Se/Ru) [Cao et al. J. Electrochem. Soc. 2006, 153, A869]. X-ray powder diffraction verified that the Se/Ru catalyst had metallic Ru cores. The in situ X-ray absorption near edge structure taken at the open circuit potential showed that there were both elemental and oxidized selenium on the as-prepared Se/Ru samples. All selenium oxide was reduced to the elemental form of selenium by applying negative potentials. By applying positive potentials, selenium was subsequently reoxidized. The analysis of the extended X-ray absorption fine structure shows the appearance of selenium hydration (Se-OH{sub 2}) in a deaerated solution, which was not observed during the oxygen reduction reaction. We present evidence that Se-free Ru atoms play an important role in the ORR activity of the Se/Ru catalyst studied in this paper.

  15. In situ synchrotron x-ray spectroscopy of ruthenium nanoparticles modified with selenium for an oxygen reduction reaction.

    SciTech Connect

    Inukai, J.; Cao, D.; Wieckowski, A.; Chang, K.-C.; Menzel, A.; Komanicky, V.; You, H.; Univ. Illinois; Univ. Yamanashi

    2007-11-15

    We used in situ Se K-edge X-ray spectroscopy to characterize Ru nanoparticles chemically modified with submonolayers of selenium (Se/Ru) [Cao et al. J. Electrochem. Soc. 2006, 153, A869]. X-ray powder diffraction verified that the Se/Ru catalyst had metallic Ru cores. The in situ X-ray absorption near edge structure taken at the open circuit potential showed that there were both elemental and oxidized selenium on the as-prepared Se/Ru samples. All selenium oxide was reduced to the elemental form of selenium by applying negative potentials. By applying positive potentials, selenium was subsequently reoxidized. The analysis of the extended X-ray absorption fine structure shows the appearance of selenium hydration (Se-OH{sub 2}) in a deaerated solution, which was not observed during the oxygen reduction reaction. We present evidence that Se-free Ru atoms play an important role in the ORR activity of the Se/Ru catalyst studied in this paper.

  16. Effect of thermo-mechanical cycling on zirconium hydride reorientation studied in situ with synchrotron X-ray diffraction

    NASA Astrophysics Data System (ADS)

    Colas, Kimberly B.; Motta, Arthur T.; Daymond, Mark R.; Almer, Jonathan D.

    2013-09-01

    The circumferential hydrides normally present in nuclear reactor fuel cladding after reactor exposure may dissolve during drying for dry storage and re-precipitate when cooled under load into a more radial orientation, which could embrittle the fuel cladding. It is necessary to study the rates and conditions under which hydride reorientation may happen in order to assess fuel integrity in dry storage. The objective of this work is to study the effect of applied stress and thermal cycling on the hydride morphology in cold-worked stress-relieved Zircaloy-4 by combining conventional metallography and in situ X-ray diffraction techniques. Metallography is used to study the evolution of hydride morphology after several thermo-mechanical cycles. In situ X-ray diffraction performed at the Advanced Photon Source synchrotron provides real-time information on the process of hydride dissolution and precipitation under stress during several thermal cycles. The detailed study of diffracted intensity, peak position and full-width at half-maximum provides information on precipitation kinetics, elastic strains and other characteristics of the hydride precipitation process. The results show that thermo-mechanical cycling significantly increases the radial hydride fraction as well as the hydride length and connectivity. The radial hydrides are observed to precipitate at a lower temperature than circumferential hydrides. Variations in the magnitude and range of hydride strains due to reorientation and cycling have also been observed. These results are discussed in light of existing models and experiments on hydride reorientation. The study of hydride elastic strains during precipitation shows marked differences between circumferential and radial hydrides, which can be used to investigate the reorientation process. Cycling under stress above the threshold stress for reorientation drastically increases both the reoriented hydride fraction and the hydride size. The reoriented hydride

  17. In-situ and operando characterization of batteries with energy-dispersive synchrotron x-ray diffraction

    NASA Astrophysics Data System (ADS)

    Paxton, William Arthur

    Batteries play a pivotal role in the low-carbon society that is required to thwart the effects of climate change. Alternative low-carbon energy sources, such as wind and solar, are often intermittent and unreliable. Batteries are able capture their energy and deliver it later when it is needed. The implementation of battery systems in grid-level and transportation sectors is essential for efficient use of alternative energy sources. Scientists and engineers need better tools to analyze and measure the performance characteristics of batteries. One of the main hindrances in the progress of battery research is that the constituent electrode materials are inaccessible once an electrochemical cell is constructed. This leaves the researcher with a limited number of available feedback mechanisms to assess the cell's performance, e.g., current, voltage, and impedance. These data are limited in their ability to reveal the more-localized smaller-scale structural mechanisms on which the batteries' performance is so dependent. Energy-dispersive x-ray diffraction (EDXRD) is one of the few techniques that can internally probe a sealed battery. By analyzing the structural behavior of battery electrodes, one is able to gain insight to the physical properties on which the battery's performance is dependent. In this dissertation, EDXRD with ultrahigh energy synchrotron radiation is used to probe the electrodes of manufactured primary and secondary lithium batteries under in-situ and operando conditions. The technique is then applied to solve specific challenges facing lithium ion batteries. Diffraction spectra are collected from within a battery at 40 micrometer resolution. Peak-fitting is used to quantitatively estimate the abundance of lithiated and non-lithiated phases. Through mapping the distribution of phases within, structural changes are linked to the battery's galvanic response. A three-dimensional spatial analysis of lithium iron phosphate batteries suggests that evolution

  18. Multiaxial deformation of polyethylene and polyethylene/clay nanocomposites: In situ synchrotron small angle and wide angle X-ray scattering study

    SciTech Connect

    Gurun, Bilge; Bucknall, David G.; Thio, Yonathan S.; Teoh, Chin Ching; Harkin-Jones, Eileen

    2013-01-10

    A unique in situ multiaxial deformation device has been designed and built specifically for simultaneous synchrotron small angle X-ray scattering (SAXS) and wide angle X-ray scattering (WAXS) measurements. SAXS and WAXS patterns of high-density polyethylene (HDPE) and HDPE/clay nanocomposites were measured in real time during in situ multiaxial deformation at room temperature and at 55 C. It was observed that the morphological evolution of polyethylene is affected by the existence of clay platelets as well as the deformation temperature and strain rate. Martensitic transformation of orthorhombic into monoclinic crystal phases was observed under strain in HDPE, which is delayed and hindered in the presence of clay nanoplatelets. From the SAXS measurements, it was observed that the thickness of the interlamellar amorphous region increased with increasing strain, which is due to elongation of the amorphous chains. The increase in amorphous layer thickness is slightly higher for the nanocomposites compared to the neat polymer.

  19. Synchrotron-based in situ soft X-ray microscopy of Ag corrosion in aqueous chloride solution

    NASA Astrophysics Data System (ADS)

    Bozzini, B.; D'Urzo, L.; Gianoncelli, A.; Kaulich, B.; Kiskinova, M.; Prasciolu, M.; Tadjeddine, A.

    2009-09-01

    In this paper we report an in situ X-ray microscopy study of a model metal electrochemistry system, incorporating faradaic reactivity: the anodic corrosion and cathodic electrodeposition of Ag in aqueous systems. The information at sub-μm scale about morpho-chemical evolution of the electrified interface, provided by this novel electroanalytical approach fosters fundamental understanding of important issues concerning material fabrication and stability, which are crucial in developing the next generation electrochemical technologies, such as fuel cells and biosensors. The key methodology challenge faced in this pilot electrochemical experiments is combining a three-electrode configuration and wet environment, which required metal electrodes suitable for transmitting soft X-rays and a sealed cell allowing working in high vacuum. This has been solved via lithographic fabrication route fabricating 75 nm thick Ag electrodes and using Si3N4 membranes as X-ray windows and electrode support. Imaging in the STXM mode with phase contrast allowed us to monitor the corrosion morphologies and metal outgrowth features. Localised thickness variation and the build-up of reaction products of electron density different from that of the starting material have been detected with high sensitivity.

  20. Advanced Techniques for In-Situ Monitoring of Phase Transformations During Welding Using Synchrotron-Based X-Ray Diffraction

    SciTech Connect

    Elmer, J W; Palmer, T A; Zhang, W; DebRoy, T

    2005-06-05

    Understanding the evolution of microstructure in welds is an important goal of welding research because of the strong correlation between weld microstructure and weld properties. To achieve this goal it is important to develop a quantitative measure of phase transformations encountered during welding in order to ultimately develop methods for predicting weld microstructures from the characteristics of the welding process. To aid in this effort, synchrotron radiation methods have been developed at Lawrence Livermore National Laboratory (LLNL) for direct observation of microstructure evolution during welding. Using intense, highly collimated synchrotron radiation, the atomic structure of the weld heat affected and fusion zones can be probed in real time. Two synchrotron-based techniques, known as spatially resolved (SRXRD) and time resolved (TRXRD) x-ray diffraction, have been developed for these investigations. These techniques have now been used to investigate welding induced phase transformations in titanium alloys, low alloy steels, and stainless steel alloys. This paper will provide a brief overview of these methods and will discuss microstructural evolution during the welding of low carbon (AISI 1005) and medium carbon (AISI 1045) steels where the different levels of carbon influence the evolution of microstructures during welding.

  1. In situ investigation of high humidity stress corrosion cracking of 7075 aluminum alloy by three-dimensional (3D) X-ray synchrotron tomography

    DOE PAGES

    Singh, S. S.; Williams, J. J.; Lin, M. F.; Xiao, X.; De Carlo, F.; Chawla, N.

    2014-05-14

    In situ X-ray synchrotron tomography was used to investigate the stress corrosion cracking behavior of under-aged Al–Zn–Mg–Cu alloy in moisture. The discontinuous surface cracks (crack jumps) mentioned in the literature are actually a single continuous and tortuous crack when observed in three dimension (3D). Contrary to 2D measurements made at the surface which suggest non-uniform crack growth rates, 3D measurements of the crack length led to a much more accurate measurement of crack growth rates.

  2. In situ investigation of high humidity stress corrosion cracking of 7075 aluminum alloy by three-dimensional (3D) X-ray synchrotron tomography

    SciTech Connect

    Singh, S. S.; Williams, J. J.; Lin, M. F.; Xiao, X.; De Carlo, F.; Chawla, N.

    2014-05-14

    In situ X-ray synchrotron tomography was used to investigate the stress corrosion cracking behavior of under-aged Al–Zn–Mg–Cu alloy in moisture. The discontinuous surface cracks (crack jumps) mentioned in the literature are actually a single continuous and tortuous crack when observed in three dimension (3D). Contrary to 2D measurements made at the surface which suggest non-uniform crack growth rates, 3D measurements of the crack length led to a much more accurate measurement of crack growth rates.

  3. In-situ microscale through-silicon via strain measurements by synchrotron x-ray microdiffraction exploring the physics behind data interpretation

    SciTech Connect

    Liu, Xi; Thadesar, Paragkumar A.; Oh, Hanju; Bakir, Muhannad S.; Taylor, Christine L.; Sitaraman, Suresh K.; Kunz, Martin; Tamura, Nobumichi

    2014-09-15

    In-situ microscale thermomechanical strain measurements have been performed in combination with synchrotron x-ray microdiffraction to understand the fundamental cause of failures in microelectronics devices with through-silicon vias. The physics behind the raster scan and data analysis of the measured strain distribution maps is explored utilizing the energies of indexed reflections from the measured data and applying them for beam intensity analysis and effective penetration depth determination. Moreover, a statistical analysis is performed for the beam intensity and strain distributions along the beam penetration path to account for the factors affecting peak search and strain refinement procedure.

  4. Complementary Control by Additives of the Kinetics of Amorphous CaCO{sub 3} Mineralization at an Organic Interface: In-Situ Synchrotron X-Ray Observations

    SciTech Connect

    Di Masi, Elaine; Kwak, Seo-Young; Amos, Fairland F.; Olszta, Matthew J.; Lush, Debra; Gower, Laurie B.

    2006-07-28

    The kinetics of biomimetic mineralization at a fatty acid monolayer interface have been measured in situ by synchrotron x-ray reflectivity. The formation of biologically relevant amorphous calcium carbonate films is affected by soluble macromolecules, supersaturation rate of change, and Mg cations. We find that these solution conditions influence mineral film formation in a complementary fashion. Poly(sodium acrylate) extends the lifetime of metastable amorphous calcium carbonate, solution saturation controls the mineral film growth rate, and Mg cations create a longer induction time. This is the first quantification of potentially competitive biomineralization mechanisms that addresses nucleation and growth of the amorphous mineral phases, which are important in biomineralization.

  5. Characterization of Cathode Materials for Rechargeable Lithium Batteries using Synchrotron Based In Situ X-ray Techniques

    SciTech Connect

    Yang, Xiao-Qing

    2007-05-23

    not be representative for the full picture of the structural changes during charge (discharge). In other words, the important information might be missed for those charge (discharge) states which were not selected for ex situ XRD studies. Secondly, the structure of the sample may have changed after removed from the cell. Finally, it is impossible to use the ex situ XRD to study the dynamic effects during high rate charge-discharge, which is crucial for the application of lithium-ion batteries for electric vehicle. A few in situ studies have been done using conventional x-ray tube sources. All of the in situ XRD studies using conventional x-ray tube sources have been done in the reflection mode in cells with beryllium windows. Because of the weak signals, data collection takes a long time, often several hundred hours for a single charge-discharge cycle. This long time data collection is not suitable for dynamic studies at all. Furthermore, in the reflection mode, the x-ray beam probes mainly the surface layer of the cathode materials. Iri collaboration with LG Chemical Ltd., BNL group designed and constructed the cells for in situ studies. LG Chemical provided several blended samples and pouch cells to BNL for preliminary in situ study. The LG Chemical provided help on integrate the blended cathode into these cells. The BNL team carried out in situ XAS and XRD studies on the samples and pouch cells provided by LG Chemical under normal charge-discharge conditions at elevated temperature.

  6. Repeated crack healing in MAX-phase ceramics revealed by 4D in situ synchrotron X-ray tomographic microscopy

    PubMed Central

    Sloof, Willem G.; Pei, Ruizhi; McDonald, Samuel A.; Fife, Julie L.; Shen, Lu; Boatemaa, Linda; Farle, Ann-Sophie; Yan, Kun; Zhang, Xun; van der Zwaag, Sybrand; Lee, Peter D.; Withers, Philip J.

    2016-01-01

    MAX phase materials are emerging as attractive engineering materials in applications where the material is exposed to severe thermal and mechanical conditions in an oxidative environment. The Ti2AlC MAX phase possesses attractive thermomechanical properties even beyond a temperature of 1000 K. An attractive feature of this material is its capacity for the autonomous healing of cracks when operating at high temperatures. Coupling a specialized thermomechanical setup to a synchrotron X-ray tomographic microscopy endstation at the TOMCAT beamline, we captured the temporal evolution of local crack opening and healing during multiple cracking and autonomous repair cycles at a temperature of 1500 K. For the first time, the rate and position dependence of crack repair in pristine Ti2AlC material and in previously healed cracks has been quantified. Our results demonstrate that healed cracks can have sufficient mechanical integrity to make subsequent cracks form elsewhere upon reloading after healing. PMID:26972608

  7. Repeated crack healing in MAX-phase ceramics revealed by 4D in situ synchrotron X-ray tomographic microscopy.

    PubMed

    Sloof, Willem G; Pei, Ruizhi; McDonald, Samuel A; Fife, Julie L; Shen, Lu; Boatemaa, Linda; Farle, Ann-Sophie; Yan, Kun; Zhang, Xun; van der Zwaag, Sybrand; Lee, Peter D; Withers, Philip J

    2016-01-01

    MAX phase materials are emerging as attractive engineering materials in applications where the material is exposed to severe thermal and mechanical conditions in an oxidative environment. The Ti2AlC MAX phase possesses attractive thermomechanical properties even beyond a temperature of 1000 K. An attractive feature of this material is its capacity for the autonomous healing of cracks when operating at high temperatures. Coupling a specialized thermomechanical setup to a synchrotron X-ray tomographic microscopy endstation at the TOMCAT beamline, we captured the temporal evolution of local crack opening and healing during multiple cracking and autonomous repair cycles at a temperature of 1500 K. For the first time, the rate and position dependence of crack repair in pristine Ti2AlC material and in previously healed cracks has been quantified. Our results demonstrate that healed cracks can have sufficient mechanical integrity to make subsequent cracks form elsewhere upon reloading after healing. PMID:26972608

  8. Phase transition in Ba{sub 2}In{sub 2}O{sub 5} studied by in situ high temperature X-ray diffraction using synchrotron radiation

    SciTech Connect

    Rey, J. F. Q.; Ferreira, F. F.; Muccillo, E. N. S.

    2009-01-29

    The order-disorder phase transition in Ba{sub 2}In{sub 2}O{sub 5} high-temperature ionic conductor was systematically studied by in situ high-temperature X-ray diffraction using synchrotron radiation and electrical conductivity. Pure barium indate was prepared by solid state reactions at 1300 deg. C. The room-temperature structural characterization showed a high degree of phase homogeneity in the prepared material. The reduction of the order-disorder phase transition temperature was verified by electrical conductivity and high-temperature X-ray diffraction. The observed features were explained based on Fourier-transform infrared spectroscopy results that revealed the presence of hydroxyl species in the crystal lattice. The increase of the intensity of few diffraction peaks near the phase transition temperature suggests the formation of a superstructure before the orthorhombic-to-tetragonal phase transition.

  9. In Situ Synchrotron Based X-ray Fluorescence and Scattering Measurements During Atomic Layer Deposition: Initial Growth of HfO2 on Si and Ge Substrates

    SciTech Connect

    K Devloo-Casier; J Dendooven; K Ludwig; G Lekens; J DHaen; C Detavernier

    2011-12-31

    The initial growth of HfO{sub 2} was studied by means of synchrotron based in situ x-ray fluorescence (XRF) and grazing incidence small angle x-ray scattering (GISAXS). HfO{sub 2} was deposited by atomic layer deposition (ALD) using tetrakis(ethylmethylamino)hafnium and H{sub 2}O on both oxidized and H-terminated Si and Ge surfaces. XRF quantifies the amount of deposited material during each ALD cycle and shows an inhibition period on H-terminated substrates. No inhibition period is observed on oxidized substrates. The evolution of film roughness was monitored using GISAXS. A correlation is found between the inhibition period and the onset of surface roughness.

  10. 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.

  11. Quantitative analysis by in situ synchrotron X-ray radiography of the evolution of the mushy zone in a fixed temperature gradient

    NASA Astrophysics Data System (ADS)

    Salloum-Abou-Jaoude, G.; Reinhart, G.; Combeau, H.; Založnik, M.; Lafford, T. A.; Nguyen-Thi, H.

    2015-02-01

    This paper deals with a series of experiments dedicated to the analysis of the time evolution of a mushy zone in a fixed temperature gradient, carried out on the BM05 beamline at the European Synchrotron Radiation Facility (ESRF) on Al-Cu alloy. Because most of phenomena involved in this evolution are dynamic, in situ and real time investigation is essential for conducting a thorough analysis as a function of time. Synchrotron X-ray radiography is a non-invasive visualization technique, perfectly suited to such a study since it is able to reveal the microstructural changes of the mushy zone during the holding stage. In addition, we extended our analysis by performing advanced image processing of synchrotron X-ray radiographs to characterize the solute distribution in the liquid phase. These measurements gave us crucial information for understanding the competition between the diffusion processes in the bulk and the mushy zone. Moreover, combining these data with mass balance equations at the two boundaries of the mushy zone enables us to demonstrate the major role of solute diffusion in the dynamics of the mushy zone, from the early instants to the final state of the holding stage.

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

    SciTech Connect

    Meng, Yue; Hrubiak, Rostislav; Rod, Eric; Shen, Guoyin; Boehler, Reinhard

    2015-07-15

    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 areas including high-pressure melting, pressure-temperature-volume equations of state, chemical reaction, and time resolved studies.

  13. Dynamics of mineral crystallization from precipitated slab-derived fluid phase: first in situ synchrotron X-ray measurements

    NASA Astrophysics Data System (ADS)

    Malaspina, Nadia; Alvaro, Matteo; Campione, Marcello; Wilhelm, Heribert; Nestola, Fabrizio

    2015-03-01

    Remnants of the fluid phase at ultrahigh pressure (UHP) in subduction environments may be preserved as primary multiphase inclusions in UHP minerals. The mode of crystallization of daughter minerals during precipitation within the inclusion and/or the mechanism of interaction between the fluid at supercritical conditions and the host mineral are still poorly understood from a crystallographic point of view. A case study is represented by garnet-orthopyroxenites from the Maowu Ultramafic Complex (China) deriving from harzburgite precursors metasomatized at ~4 GPa, 750 °C by a silica- and incompatible trace element-rich fluid phase. This metasomatism produced poikilitic orthopyroxene and inclusion-rich garnet porphyroblasts. Solid multiphase primary inclusions in garnet display a size within a few tens of micrometres and negative crystal shapes. Infilling minerals (spinel: 10-20 vol%; amphibole, chlorite, talc, mica: 80-90 vol%) occur with constant volume proportions and derive from trapped solute-rich aqueous fluids. To constrain the possible mode of precipitation of daughter minerals, we performed for the first time a single-crystal X-ray diffraction experiment by synchrotron radiation at Diamond Light Source. In combination with electron probe microanalyses, this measurement allowed the unique identification of each mineral phase and reciprocal orientations. We demonstrated the epitaxial relationship between spinel and garnet and between some hydrous minerals. Such information is discussed in relation to the physico-chemical aspects of nucleation and growth, shedding light on the mode of mineral crystallization from a fluid phase trapped at supercritical conditions.

  14. Direct Observation of Austenitization in 1005 C-Mn Steel during Continuous Heating Using In Situ Synchrotron X-Ray Diffraction

    SciTech Connect

    Palmer, T. A.; Elmer, J. W.; Mayr, Peter; Specht, Eliot D

    2011-01-01

    The austenitization ( ) transformation in a 1005 C-Mn steel is monitored in real time at continuous heating rates between 1 C/sec to 10 C/sec using in situ synchrotron x-ray diffraction. Both dilatometry and the in situ x-ray diffraction experiments show that the austenitization transformation proceeds through multiple mechanisms from initiation through completion. Unlike the dilatometry experiments, the in situ x-ray diffraction experiments provide direct evidence for the phases present at specific times during the transformation. Thus, experimental validation is provided for models based on the differing kinetics of the austenitization transformation starting from a heterogeneous microstructure containing pearlite and ferrite. Beginning at temperatures below the A1 transformation temperature, the starting microstructure undergoes a recovery and recrystallization process to relieve stress imparted during the initial thermomechanical treatment of the steel. The austenitization transformation follows, beginning at temperatures above the A1 temperature, with the initial transformation proceeding as the pearlite in the microstructure is dissolved and high carbon concentration austenite is formed. Since the carbon present in the steel is localized near the original pearlite colonies, there is a pronounced heating rate dependant delay before the remaining ferrite grains begin to transform. As temperatures reach 850 C at all heating rates, the remaining ferrite transforms to austenite, since the equilibrium phase diagram indicates that higher temperatures are required to drive the transformation at these lower carbon concentrations. The transformation reaches completion at temperatures above the A3 temperature, and the last ferrite to be transformed is nearly pure iron.

  15. Tensile testing of materials at high temperatures above 1700 °C with in situ synchrotron X-ray micro-tomography

    SciTech Connect

    Haboub, Abdel; Nasiatka, James R.; MacDowell, Alastair A.; Bale, Hrishikesh A.; Cox, Brian N.; Marshall, David B.; Ritchie, Robert O.

    2014-08-15

    A compact ultrahigh temperature tensile testing instrument has been designed and fabricated for in situ x-ray micro-tomography using synchrotron radiation at the Advanced Light Source, Lawrence Berkeley National Laboratory. It allows for real time x-ray micro-tomographic imaging of test materials under mechanical load at temperatures up to 2300 °C in controlled environments (vacuum or controlled gas flow). Sample heating is by six infrared halogen lamps with ellipsoidal reflectors arranged in a confocal configuration, which generates an approximately spherical zone of high heat flux approximately 5 mm in diameter. Samples are held between grips connected to a motorized stage that loads the samples in tension or compression with forces up to 2.2 kN. The heating chamber and loading system are water-cooled for thermal stability. The entire instrument is mounted on a rotation stage that allows stepwise recording of radiographs over an angular range of 180°. A thin circumferential (360°) aluminum window in the wall of the heating chamber allows the x-rays to pass through the chamber and the sample over the full angular range. The performance of the instrument has been demonstrated by characterizing the evolution of 3D damage mechanisms in ceramic composite materials under tensile loading at 1750 °C.

  16. Direct Observations of Sigma Phase Formation in Duplex Stainless Steels Using In Situ Synchrotron X-Ray Diffraction

    SciTech Connect

    Elmer, J. W.; Palmer, T. A.; Specht, Eliot D

    2007-01-01

    The formation and growth of sigma ( ) phase in 2205 duplex stainless steel (DSS) was observed and measured in real time using synchrotron radiation during 10 hour isothermal heat treatments at temperatures between 700 C and 850 C. Sigma formed in near-equilibrium quantities during the isothermal holds, starting from a microstructure which contained a balanced mixture of metastable ferrite and austenite. In-situ synchrotron diffraction continuously monitored the transformation, and these results were compared to those predicted by thermodynamic calculations. The data were further analyzed using a modified Johnson-Mehl-Avrami-Kolmogrov (JMAK) approach to determine kinetic parameters for sigma formation over this temperature range. The initial JMAK exponent, n, at low fractions of sigma was found to be approximately 7.0; however, toward the end of the transformation, n decreased to values of approximately 0.75. The change in the JMAK exponent was attributed to a change in the transformation mechanism from discontinuous precipitation with increasing nucleation rate, to growth of the existing sigma phase after nucleation site saturation occurred. Because of this change in mechanism, it was not possible to determine reliable values for the activation energy and pre-exponential terms for the JMAK equation. While cooling back to room temperature, the partial transformation of austenite resulted in a substantial increase in the ferrite content, but sigma retained its high-temperature value to room temperature.

  17. Direct Observations of Sigma Phase Formation in Duplex Stainless Steels using In Situ Synchrotron X-Ray Diffraction

    SciTech Connect

    Elmer, J W; Palmer, T A; Specht, E D

    2006-07-03

    The formation and growth of sigma phase in 2205 duplex stainless steel was observed and measured in real time using synchrotron radiation during 10 hr isothermal heat treatments at temperatures between 700 C and 850 C. Sigma formed in near-equilibrium quantities during the isothermal holds, starting from a microstructure which contained a balanced mixture of metastable ferrite and austenite. In situ synchrotron diffraction continuously monitored the transformation, and these results were compared to those predicted by thermodynamic calculations. Differences between the calculated and measured amounts of sigma, ferrite and austenite suggest that the thermodynamic calculations underpredict the sigma dissolution temperature by approximately 50 C. The data were further analyzed using a modified Johnson-Mehl-Avrami (JMA) approach to determine kinetic parameters for sigma formation over this temperature range. The initial JMA exponent, n, at low fractions of sigma was found to be approximately 7.0, however, towards the end of the transformation, n decreased to values of approximately 0.75. The change in the JMA exponent was attributed to a change in the transformation mechanism from discontinuous precipitation with increasing nucleation rate, to growth of the existing sigma phase after nucleation site saturation occurred. Because of this change in mechanism, it was not possible to determine reliable values for the activation energy and pre-exponential terms for the JMA equation. While cooling back to room temperature, the partial transformation of austenite resulted in a substantial increase in the ferrite content, but sigma retained its high temperature value to room temperature.

  18. Evidence for Degradation of the Chrome Yellows in Van Gogh's Sunflowers: A Study Using Noninvasive In Situ Methods and Synchrotron-Radiation-Based X-ray Techniques.

    PubMed

    Monico, Letizia; Janssens, Koen; Hendriks, Ella; Vanmeert, Frederik; Van der Snickt, Geert; Cotte, Marine; Falkenberg, Gerald; Brunetti, Brunetto Giovanni; Miliani, Costanza

    2015-11-16

    This paper presents firm evidence for the chemical alteration of chrome yellow pigments in Van Gogh's Sunflowers (Van Gogh Museum, Amsterdam). Noninvasive in situ spectroscopic analysis at several spots on the painting, combined with synchrotron-radiation-based X-ray investigations of two microsamples, revealed the presence of different types of chrome yellow used by Van Gogh, including the lightfast PbCrO4 and the sulfur-rich PbCr1-x Sx O4 (x≈0.5) variety that is known for its high propensity to undergo photoinduced reduction. The products of this degradation process, i.e., Cr(III) compounds, were found at the interface between the paint and the varnish. Selected locations of the painting with the highest risk of color modification by chemical deterioration of chrome yellow are identified, thus calling for careful monitoring in the future. PMID:26482035

  19. Strength Measurement of Boron Suboxide B6O at High Pressure and Temperature Using in situ Synchrotron X-ray Diffraction

    SciTech Connect

    Chen, J.; Yang, Y; Yu, T; Zhang, J; Zhao, Y; Wang, L

    2008-01-01

    The strength of boron suboxide (B6O) was measured at high pressure and temperature up to 8 GPa and 800 C using diffraction peak broadening analysis. The sample was synthesized at 6 GPa and 1750 C. In situ energy dispersive X-ray diffraction was conducted at the X17B2 beamline of the National Synchrotron Light Source. The differential stress in the powdered sample was derived through deconvolution of peak broadening of diffraction lines (0 2 1) and (1 1 3) during the compression and heating. The sample shows anisotropic yielding along the two orientations. The (0 2 1) orientation does not show yielding within the investigated pressure range (8 GPa) whereas the (1 1 3) orientation yields at 5 GPa. Upon heating, significant weakening (yielding) was observed at temperatures above 400 C. The yield temperature of boron suboxide is much lower than that of diamond, 1200 C, but similar to that observed in moissanite (SiC).

  20. In situ measurement of electromigration-induced transient stress in Pb-free Sn-Cu solder joints by synchrotron radiation based X-ray polychromatic microdiffraction

    SciTech Connect

    Chen, Kai; Tamura, Nobumichi; Kunz, Martin; Tu, King-Ning; Lai, Yi-Shao

    2009-12-01

    Electromigration-induced hydrostatic elastic stress in Pb-free SnCu solder joints was studied by in situ synchrotron X-ray white beam microdiffraction. The elastic stresses in two different grains with similar crystallographic orientation, one located at the anode end and the other at the cathode end, were analyzed based on the elastic anisotropy of the Beta-Sn crystal structure. The stress in the grain at the cathode end remained constant except for temperature fluctuations, while the compressive stress in the grain at the anode end was built-up as a function of time during electromigration until a steady state was reached. The measured compressive stress gradient between the cathode and the anode is much larger than what is needed to initiate Sn whisker growth. The effective charge number of Beta-Sn derived from the electromigration data is in good agreement with the calculated value.

  1. Formation of delta ferrite in 9 wt.% Cr steel investigated by in-situ X-ray diffraction using synchrotron radiation

    SciTech Connect

    Mayr, Peter; Palmer, T. A.; Elmer, J. W.; Specht, Eliot D; Allen, S M

    2010-01-01

    In situ X-ray diffraction measurements using high energy synchrotron radiation were performed to monitor in real time the formation of delta ferrite in a martensitic 9 wt.% chromium steel under simulated weld thermal cycles. Volume fractions of martensite, austenite and delta ferrite were measured as a function of temperature at a 10 C s-1 heating rate to 1300 C and subsequent cooling to room temperature. At the peak temperature, the delta ferrite concentration rose to a level of 19%, of which 17% transformed back to austenite on subsequent cooling. The final microstructure after this single thermal cycle consisted of newly formed martensite with 4% of retained austenite and 2% of retained delta ferrite.

  2. 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.

  3. In situ measurement of electromigration-induced transient stress in Pb-free Sn-Cu solder joints by synchrotron radiation based X-ray polychromatic microdiffraction

    SciTech Connect

    Chen, Kai; Tamura, Nobumichi; Kunz, Martin; Tu, King-Ning; Lai, Yi-Shao

    2009-05-15

    Electromigration-induced hydrostatic elastic stress in Pb-free SnCu solder joints was studied by in situ synchrotron X-ray white beam microdiffraction. The elastic stresses in two different grains with similar crystallographic orientation, one located at the anode end and the other at the cathode end, were analyzed based on the elastic anisotropy of the {beta}-Sn crystal structure. The stress in the grain at the cathode end remained constant except for temperature fluctuations, while the compressive stress in the grain at the anode end was built-up as a function of time during electromigration until a steady state was reached. The measured compressive stress gradient between the cathode and the anode is much larger than what is needed to initiate Sn whisker growth. The effective charge number of {beta}-Sn derived from the electromigration data is in good agreement with the calculated value.

  4. In situ synchrotron X-ray diffraction study of deformation behavior and load transfer in a Ti{sub 2}Ni-NiTi composite

    SciTech Connect

    Zhang, Junsong; Hao, Shijie; Yu, Cun; Shao, Yang; Ru, Yadong; Jiang, Daqiang; Cui, Lishan; Liu, Yinong; Ren, Yang; Huan, Yong

    2014-07-28

    The deformation behavior and load transfer of a dual-phase composite composed of martensite NiTi embedded in brittle Ti{sub 2}Ni matrices were investigated by using in situ synchrotron x-ray diffraction during compression. The composite exhibits a stage-wise deformation feature and a double-yielding phenomenon, which were caused by the interaction between Ti{sub 2}Ni and NiTi with alternative microscopic deformation mechanism. No load transfer occurs from the soft NiTi dendrites to the hard Ti{sub 2}Ni matrices during the pseudoplastic deformation (detwinning) of NiTi, which is significantly different from that previously reported in bulk metallic glasses matrices composites.

  5. Evidence for Degradation of the Chrome Yellows in Van Gogh's Sunflowers: A Study Using Noninvasive In Situ Methods and Synchrotron-Radiation-Based X-ray Techniques.

    PubMed

    Monico, Letizia; Janssens, Koen; Hendriks, Ella; Vanmeert, Frederik; Van der Snickt, Geert; Cotte, Marine; Falkenberg, Gerald; Brunetti, Brunetto Giovanni; Miliani, Costanza

    2015-11-16

    This paper presents firm evidence for the chemical alteration of chrome yellow pigments in Van Gogh's Sunflowers (Van Gogh Museum, Amsterdam). Noninvasive in situ spectroscopic analysis at several spots on the painting, combined with synchrotron-radiation-based X-ray investigations of two microsamples, revealed the presence of different types of chrome yellow used by Van Gogh, including the lightfast PbCrO4 and the sulfur-rich PbCr1-x Sx O4 (x≈0.5) variety that is known for its high propensity to undergo photoinduced reduction. The products of this degradation process, i.e., Cr(III) compounds, were found at the interface between the paint and the varnish. Selected locations of the painting with the highest risk of color modification by chemical deterioration of chrome yellow are identified, thus calling for careful monitoring in the future.

  6. (De)lithiation mechanism of Li/SeS(x) (x = 0-7) batteries determined by in situ synchrotron X-ray diffraction and X-ray absorption spectroscopy.

    PubMed

    Cui, Yanjie; Abouimrane, Ali; Lu, Jun; Bolin, Trudy; Ren, Yang; Weng, Wei; Sun, Chengjun; Maroni, Victor A; Heald, Steve M; Amine, Khalil

    2013-05-29

    Electrical energy storage for transportation has gone beyond the limit of converntional lithium ion batteries currently. New material or new battery system development is an alternative approach to achieve the goal of new high-energy storage system with energy densities 5 times or more greater. A series of SeSx-carbon (x = 0-7) composite materials has been prepared and evaluated as the positive electrodes in secondary lithium cells with ether-based electrolyte. In situ synchrotron high-energy X-ray diffraction was utilized to investigate the crystalline phase transition during cell cycling. Complementary, in situ Se K-edge X-ray absorption near edge structure analysis was used to track the evolution of the Se valence state for both crystalline and noncrystalline phases, including amorphous and electrolyte-dissolved phases in the (de)lithiation process. On the basis of these results, a mechanism for the (de)lithiation process is proposed, where Se is reduced to the polyselenides, Li2Sen (n ≥ 4), Li2Se2, and Li2Se sequentially during the lithiation and Li2Se is oxidized to Se through Li2Sen (n ≥ 4) during the delithiation. In addition, X-ray photoelectron spectroscopy and electrochemical impedance spectroscopy demonstrated the reversibility of the Li/Se system in ether-based electrolyte and the presence of side products in the carbonate-based electrolytes. For Li/SeS2 and Li/SeS7 cells, Li2Se and Li2S are the discharged products with the presence of Se only as the crystalline phase in the end of charge.

  7. (De)lithiation mechanism of Li/SeS(x) (x = 0-7) batteries determined by in situ synchrotron X-ray diffraction and X-ray absorption spectroscopy.

    PubMed

    Cui, Yanjie; Abouimrane, Ali; Lu, Jun; Bolin, Trudy; Ren, Yang; Weng, Wei; Sun, Chengjun; Maroni, Victor A; Heald, Steve M; Amine, Khalil

    2013-05-29

    Electrical energy storage for transportation has gone beyond the limit of converntional lithium ion batteries currently. New material or new battery system development is an alternative approach to achieve the goal of new high-energy storage system with energy densities 5 times or more greater. A series of SeSx-carbon (x = 0-7) composite materials has been prepared and evaluated as the positive electrodes in secondary lithium cells with ether-based electrolyte. In situ synchrotron high-energy X-ray diffraction was utilized to investigate the crystalline phase transition during cell cycling. Complementary, in situ Se K-edge X-ray absorption near edge structure analysis was used to track the evolution of the Se valence state for both crystalline and noncrystalline phases, including amorphous and electrolyte-dissolved phases in the (de)lithiation process. On the basis of these results, a mechanism for the (de)lithiation process is proposed, where Se is reduced to the polyselenides, Li2Sen (n ≥ 4), Li2Se2, and Li2Se sequentially during the lithiation and Li2Se is oxidized to Se through Li2Sen (n ≥ 4) during the delithiation. In addition, X-ray photoelectron spectroscopy and electrochemical impedance spectroscopy demonstrated the reversibility of the Li/Se system in ether-based electrolyte and the presence of side products in the carbonate-based electrolytes. For Li/SeS2 and Li/SeS7 cells, Li2Se and Li2S are the discharged products with the presence of Se only as the crystalline phase in the end of charge. PMID:23631402

  8. Quantitative study of particle size distribution in an in-situ grown Al–TiB{sub 2} composite by synchrotron X-ray diffraction and electron microscopy

    SciTech Connect

    Tang, Y.; Chen, Z.; Borbély, A.; Ji, G.; Zhong, S.Y.; Schryvers, D.; Ji, V.

    2015-04-15

    Synchrotron X-ray diffraction and transmission electron microscopy (TEM) were applied to quantitatively characterize the average particle size and size distribution of free-standing TiB{sub 2} particles and TiB{sub 2} particles in an in-situ grown Al–TiB{sub 2} composite. The detailed evaluations were carried out by X-ray line profile analysis using the restricted moment method and multiple whole profile fitting procedure (MWP). Both numerical methods indicate that the formed TiB{sub 2} particles are well crystallized and free of crystal defects. The average particle size determined from different Bragg reflections by the restricted moment method ranges between 25 and 55 nm, where the smallest particle size is determined using the 110 reflection suggesting the highest lateral-growth velocity of (110) facets. The MWP method has shown that the in-situ grown TiB{sub 2} particles have a very low dislocation density (~ 10{sup 11} m{sup −} {sup 2}) and their size distribution can be described by a log-normal distribution. Good agreement was found between the results obtained from the restricted moment and MWP methods, which was further confirmed by TEM. - Highlights: • Accurate quantitative characterization of in-situ grown T{sub i}B{sub 2} particles has been achieved. • Particle size anisotropy was revealed indicating 110 facets being largest during T{sub i}B{sub 2} growth. • A wide size distribution was observed for T{sub i}B{sub 2} particles with a dominant size smaller than 100 nm.

  9. In Situ Synchrotron X-Ray Diffraction and Small Angle X-Ray Scattering Studies on Rapidly Heated and Cooled Ti-Al and Al-Cu-Mg Alloys Using Laser-Based Heating

    NASA Astrophysics Data System (ADS)

    Kenel, C.; Schloth, P.; Van Petegem, S.; Fife, J. L.; Grolimund, D.; Menzel, A.; Van Swygenhoven, H.; Leinenbach, C.

    2016-03-01

    Beam-based additive manufacturing (AM) typically involves high cooling rates in a range of 103-104 K/s. Therefore, new techniques are required to understand the non-equilibrium evolution of materials at appropriate time scales. Most technical alloys have not been optimized for such rapid solidification, and microstructural, phase, and elemental solubility behavior can be very different. In this work, the combination of complementary in situ synchrotron micro-x-ray diffraction (microXRD) and small angle x-ray scattering (SAXS) studies with laser-based heating and rapid cooling is presented as an approach to study alloy behavior under processing conditions similar to AM techniques. In rapidly solidified Ti-48Al, the full solidification and phase transformation sequences are observed using microXRD with high temporal resolution. The high cooling rates are achieved by fast heat extraction. Further, the temperature- and cooling rate-dependent precipitation of sub-nanometer clusters in an Al-Cu-Mg alloy can be studied by SAXS. The sensitivity of SAXS on the length scales of the newly formed phases allows their size and fraction to be determined. These techniques are unique tools to help provide a deeper understanding of underlying alloy behavior and its influence on resulting microstructures and properties after AM. Their availability to materials scientists is crucial for both in-depth investigations of novel alloys and also future production of high-quality parts using AM.

  10. In-situ mechanical testing during X-ray diffraction

    SciTech Connect

    Van Swygenhoven, Helena Van Petegem, Steven

    2013-04-15

    Deforming metals during recording X-ray diffraction patterns is a useful tool to get a deeper understanding of the coupling between microstructure and mechanical behaviour. With the advances in flux, detector speed and focussing techniques at synchrotron facilities, in-situ mechanical testing is now possible during powder diffraction and Laue diffraction. The basic principle is explained together with illustrative examples.

  11. Early age hydration and pozzolanic reaction in natural zeolite blended cements: Reaction kinetics and products by in situ synchrotron X-ray powder diffraction

    SciTech Connect

    Snellings, R.; Mertens, G.; Cizer, O.; Elsen, J.

    2010-12-15

    The in situ early-age hydration and pozzolanic reaction in cements blended with natural zeolites were investigated by time-resolved synchrotron X-ray powder diffraction with Rietveld quantitative phase analysis. Chabazite and Na-, K-, and Ca-exchanged clinoptilolite materials were mixed with Portland cement in a 3:7 weight ratio and hydrated in situ at 40 {sup o}C. The evolution of phase contents showed that the addition of natural zeolites accelerates the onset of C{sub 3}S hydration and precipitation of CH and AFt. Kinetic analysis of the consumption of C{sub 3}S indicates that the enveloping C-S-H layer is thinner and/or less dense in the presence of alkali-exchanged clinoptilolite pozzolans. The zeolite pozzolanic activity is interpreted to depend on the zeolite exchangeable cation content and on the crystallinity. The addition of natural zeolites alters the structural evolution of the C-S-H product. Longer silicate chains and a lower C/S ratio are deduced from the evolution of the C-S-H b-cell parameter.

  12. In situ synchrotron X-ray imaging on morphological evolution of dendrites in Sn-Bi hypoeutectic alloy under electric currents

    NASA Astrophysics Data System (ADS)

    Wang, Tongmin; Zhu, Jing; Kang, Huijun; Chen, Zongning; Fu, Yanan; Huang, Wanxia; Xiao, Tiqiao

    2014-06-01

    The growth behavior and morphological evolution of dendrites in solidifying Sn-Bi alloy under electric currents [e.g., direct current (DC) and electric current pulse (ECP)] are in situ studied using synchrotron radiation X-ray imaging technique. The suppression of dendrite growth, floating and rotation of dendrites, refinement and remelting of dendrites are investigated by analyzing a series of animated images captured during the experiments. The modification mechanisms of dendrite morphology by electric fields are discussed based on the in situ and real-time observations. When DC is imposed on the samples, the growth of dendrites is significantly suppressed due to the effect of Joule heat, and a small dendrite freely flows up and rotates due to the common effect of natural convection. When ECP is imposed in the whole solidification process, the outset of solidification is delayed by Joule heat. And due to the accumulation of undercooling, dendrites suddenly nucleate, grow and finally become fine primary dendrite arm spacing. When ECP is imposed during the crystal growth stage only, the dendrites are remelted at first and then reappear along the original growing trajectories, showing the hereditary feature.

  13. 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

  14. Integrating in situ high pressure small and wide angle synchrotron x-ray scattering for exploiting new physics of nanoparticle supercrystals

    PubMed Central

    Wang, Zhongwu; Chen, Ou; Cao, Charles Y.; Finkelstein, Ken; Smilgies, Detlef-M.; Lu, Xianmao; Bassett, William A.

    2010-01-01

    Combined small and wide angle synchrotron x-ray scattering (SAXS and WAXS) techniques have been developed for in situ high pressure samples, enabling exploration of the atomic structure and nanoscale superstructure phase relations. These studies can then be used to find connections between nanoparticle surfaces and internal atomic arrangements. We developed a four-axis control system for the detector, which we then employed for the study of two supercrystals assembled from 5 nm Fe3O4 and 10 nm Au nanoparticles. We optimized the x-ray energy and the sample-to-detector distance to facilitate simultaneous collection of both SAXS and WAXS. We further performedin situ high pressure SAXS and WAXS on a cubic supercrystal assembled from 4 nm wurtzite-structure CdSe nanoparticles. While wurtzite-structure CdSe nanoparticles transform into a rocksalt structure at 6.2 GPa, the cubic superstructure develops into a lamellarlike mesostructure at 9.6 GPa. Nanoparticle coupling and interaction could be enhanced, thus reducing the compressibility of the interparticle spacing above ∼3 GPa. At ∼6.2 GPa, the wurtzite-to-rocksalt phase transformation results in a noticeable drop of interparticle spacing. Above 6.2 GPa, a combined effect from denser CdSe nanoparticle causes the interparticle spacing to expand. These findings could be related to a series of changes including the surface structure, electronic and mechanical properties, and strain distribution of CdSe under pressure. This technique opens the way for exploring the new physics of nanoparticles and self-assembled superlattices. PMID:20886989

  15. In situ apparatus for the study of clathrate hydrates relevant to solar system bodies using synchrotron X-ray diffraction and Raman spectroscopy

    NASA Astrophysics Data System (ADS)

    Day, Sarah J.; Thompson, Stephen P.; Evans, Aneurin; Parker, Julia E.

    2015-02-01

    Context. Clathrate hydrates are believed to play a significant role in various solar system environments, e.g. comets, and the surfaces and interiors of icy satellites. However, the structural factors governing their formation and dissociation are poorly understood. Aims: We demonstrate the application of a high pressure gas cell, combined with variable temperature non-contact cooling and fast, time-resolved data collection, to the in situ study of clathrate hydrates under conditions relevant to solar system environments. Methods: Clathrates formed and processed within the sample cell are monitored in situ using time-resolved synchrotron X-ray powder diffraction and laser Raman spectroscopy. Results: X-ray diffraction allows the formation of clathrate hydrates to be observed as CO2 gas is applied to ice formed within the cell. Complete conversion is obtained by annealing at temperatures just below the ice melting point. A subsequent rise in the quantity of clathrate is observed as the cell is thermally cycled. Four regions between 100-5000 cm-1 are present in the in situ Raman spectra that carry features characteristic of both ice and clathrate formation. Conclusions: This novel experimental arrangement is well suited to studying clathrate hydrates over a wide range of temperature (80 -500 K) and pressure (1-100 bar) conditions relevant to solar system bodies and can be used with a variety of different gases and starting aqueous compositions (e.g. saline solutions). We propose the increase in clathrate formation observed during thermal cycling may be due to the formation of a quasi liquid-like phase that forms at temperatures below the ice melting point, but which allows either easier formation of new clathrate cages, or the retention and delocalisation of previously formed clathrate structures, possibly as amorphous clathrate. The structural similarities between hexagonal ice, the quasi liquid-like phase, and crystalline CO2 hydrate mean that differences in the

  16. In-Situ Observations of Sigma Phase Dissolution in 2205 Duplex Stainless Steel Using Synchrotron X-Ray Diffraction

    SciTech Connect

    Elmer, J. W.; Palmer, T. A.; Specht, Eliot D

    2007-01-01

    Synchrotron radiation was used to directly observe the transformation of ferrite, austenite and sigma phases during heating and cooling of 2205 duplex stainless steel. Sigma formed during the initial stages of heating, dissolved as the temperature was increased, and reformed on cooling. The dissolution temperature of sigma was measured to be 985 2.8 C at a heating rate of 0.25 C/s, and the kinetics of sigma formation at 850 Cwas determined to be slower after dissolving at 1000 C than before.

  17. In-Situ Observations of Sigma Phase Dissolution in 2205 Duplex Stainless Steel using Synchrotron X-Ray Diffraction

    SciTech Connect

    Elmer, J; Palmer, T; Specht, E

    2006-08-08

    Synchrotron radiation was used to directly observe the transformation of ferrite, austenite and sigma phases during heating and cooling of 2205 duplex stainless steel. Sigma formed during the initial stages of heating, dissolved as the temperature was increased, and reformed on cooling. The dissolution temperature of sigma was measured to be 985 C {+-} 2.8 C at a heating rate of 0.25 C/s, and the kinetics of sigma formation at 850 C was determined to be slower after dissolving at 1000 C than before.

  18. In situ synchrotron X-ray powder diffraction for studying the role of induced structural defects on the thermoluminescence mechanism of nanocrystalline LiF.

    PubMed

    El Ashmawy, Mostafa; Amer, Hany; Abdellatief, Mahmoud

    2016-03-01

    The correlation between the thermoluminescence (TL) response of nanocrystalline LiF and its microstructure was studied. To investigate the detailed TL mechanism, the glow curves of nanocrystalline LiF samples produced by high-energy ball-milling were analyzed. The microstructure of the prepared samples was analyzed by synchrotron X-ray powder diffraction (XRPD) at room temperature. Then, the microstructure of a representative pulverized sample was investigated in detail by performing in situ XRPD in both isothermal and non-isothermal modes. In the present study, the dislocations produced by ball-milling alter the microstructure of the lattice where the relative concentration of the vacancies, responsible for the TL response, changes with milling time. An enhancement in the TL response was recorded for nanocrystalline LiF at high-temperature traps (after dislocations recovery starts >425 K). It is also found that vacancies are playing a major role in the dislocations recovery mechanism. Moreover, the interactions among vacancies-dislocations and/or dislocations-dislocations weaken the TL response. PMID:26917138

  19. In situ synchrotron X-ray powder diffraction for studying the role of induced structural defects on the thermoluminescence mechanism of nanocrystalline LiF.

    PubMed

    El Ashmawy, Mostafa; Amer, Hany; Abdellatief, Mahmoud

    2016-03-01

    The correlation between the thermoluminescence (TL) response of nanocrystalline LiF and its microstructure was studied. To investigate the detailed TL mechanism, the glow curves of nanocrystalline LiF samples produced by high-energy ball-milling were analyzed. The microstructure of the prepared samples was analyzed by synchrotron X-ray powder diffraction (XRPD) at room temperature. Then, the microstructure of a representative pulverized sample was investigated in detail by performing in situ XRPD in both isothermal and non-isothermal modes. In the present study, the dislocations produced by ball-milling alter the microstructure of the lattice where the relative concentration of the vacancies, responsible for the TL response, changes with milling time. An enhancement in the TL response was recorded for nanocrystalline LiF at high-temperature traps (after dislocations recovery starts >425 K). It is also found that vacancies are playing a major role in the dislocations recovery mechanism. Moreover, the interactions among vacancies-dislocations and/or dislocations-dislocations weaken the TL response.

  20. First stages of siderite crystallisation during CO2 corrosion of steel evaluated using in situ synchrotron small- and wide-angle X-ray scattering.

    PubMed

    Ingham, Bridget; Ko, Monika; Laycock, Nick; Kirby, Nigel M; Williams, David E

    2015-01-01

    We use in situ synchrotron small- and wide-angle X-ray scattering (SAXS/WAXS) to demonstrate that the formation of crystalline siderite (FeCO(3)) during the corrosion of steel in CO(2)-saturated brine - a problem of practical interest relating to the growth of protective scales on the interior surface of oil and gas production pipelines - is preceded by the formation of a colloidal precipitate in the solution and an amorphous surface layer, both assumed to be amorphous ferrous carbonate. Grazing incidence SAXS shows instantaneous film formation upon the application of an anodic potential, followed by development of a separate population of particles at later times, then by the formation of crystalline species, observed by WAXS. These observations can be interpreted in terms of crystal nucleation within the amorphous surface layer. Traces of Cr(3+) in the solution significantly accelerate the precipitation rate of the colloidal precursor and accelerate the appearance of the crystalline scale. We speculate on the significance of these observations for the nucleation, growth and morphology of the corrosion scale and hence its protectiveness.

  1. An in situ synchrotron X-ray diffraction investigation of lepidocrocite and ferrihydrite-seeded Al(OH) 3 crystallisation from supersaturated sodium aluminate liquor

    NASA Astrophysics Data System (ADS)

    Webster, Nathan A. S.; Loan, Melissa J.; Madsen, Ian C.; Knott, Robert B.; Brodie, Greta M.; Kimpton, Justin A.

    2012-02-01

    Lepidocrocite and ferrihydrite-seeded Al(OH) 3 crystallisation from supersaturated sodium aluminate liquor at 70 °C was investigated using in situ synchrotron X-ray diffraction. The presence of iron oxides and oxyhydroxides in the Bayer process has implications for the nucleation and growth of scale on process equipment, and a greater understanding of the effect they have on Al(OH) 3 crystallisation may allow for development of methods for Al(OH) 3 scale prevention. The early stages of both crystallisation reactions were characterised by nucleation of gibbsite on the seed material. This was followed by a rapid increase in gibbsite concentration, which coincided with the appearance of the bayerite and nordstrandite polymorphs of Al(OH) 3. The lepidocrocite-seeded reaction then proceeded via a mechanism similar to that which has been observed previously for goethite, hematite and magnetite-seeded Al(OH) 3 crystallisation. Different behaviour was observed in the ferrihydrite-seeded experiment, with nucleation as well as growth occurring during the period of rapid increase in gibbsite concentration, followed by a period of diffusion controlled growth.

  2. SYNCHROTRON X - RAY OBSERVATIONS OF A MONOLAYER TEMPLATE FOR MINERALIZATION.

    SciTech Connect

    DIMASI,E.; GOWER,L.B.

    2000-11-27

    Mineral nucleation at a Langmuir film interface has been studied by synchrotron x-ray scattering. Diluted calcium bicarbonate solutions were used as subphases for arachidic and stearic acid monolayers, compressed in a Langmuir trough. Self-assembly of the monolayer template is observed directly, and subsequent crystal growth monitored in-situ.

  3. Experimental issues in in-situ synchrotron x-ray diffraction at high pressure and temperature by using a laser-heated diamond-anvil cell

    SciTech Connect

    Yoo, C.S.

    1997-12-01

    An integrated technique of diamond-anvil cell, laser-heating and synchrotron x-ray diffraction technologies is capable of structural investigation of condensed matter in an extended region of high pressures and temperatures above 100 GPa and 3000 K. The feasibility of this technique to obtain reliable data, however, strongly depends on several experimental issues, including optical and x-ray setups, thermal gradients, pressure homogeneity, preferred orientation, and chemical reaction. In this paper, we discuss about these experimental issues together with future perspectives of this technique for obtaining accurate data.

  4. 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

    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

    2014-09-01

    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.

  5. In situ high-pressure synchrotron X-ray powder diffraction study of tunnel manganese oxide minerals: hollandite, romanechite, and todorokite

    NASA Astrophysics Data System (ADS)

    Hwang, Gil Chan; Post, Jeffrey E.; Lee, Yongjae

    2015-05-01

    In situ high-pressure synchrotron X-ray powder diffraction study of three tunnel manganese oxide minerals (hollandite with 2 × 2 MnO6 octahedra tunnels, romanechite with 2 × 3 tunnels, and todorokite with 3 × 3 tunnels) was performed using a diamond anvil cell and nominally penetrating alcohol and water mixture as a pressure-transmitting medium up to ~8 GPa. Bulk moduli ( B 0) calculated using Murnaghan's equation of state are inversely proportional to the size of the tunnel, i.e., 134(4) GPa for hollandite ( I2/m), 108(2) GPa for romanechite ( C2/m), and 67(5) GPa for todorokite ( P2/m). On the other hand, axial compressibilities show different elastic anisotropies depending on the size of the tunnel, i.e., ( a/ a 0) = -0.00066(3) GPa-1, ( b/ b 0) = 0.00179(8) GPa-1, ( c/ c 0) = 0.00637(4) GPa-1 [ c > b > a] for hollandite; ( a/ a 0) = 0.00485(4) GPa-1, ( b/ b 0) = 0.0016(1) GPa-1, ( c/ c 0) = 0.00199(8) GPa-1 [ a > c > b] for romanechite; and ( a/ a 0) = 0.00826(9) GPa-1, ( b/ b 0) = 0.0054(1) GPa-1, ( c/ c 0) = 0.00081(8) GPa-1 [ a > b > c] for todorokite. Overall, the degree of tunnel distortion increases with increasing pressure and correlates with the size of the tunnel, which is evidenced by the gradual increases in the monoclinic β angles up to 3 GPa of 0.62°, 0.8°, and 1.15° in hollandite, romanechite, and todorokite, respectively. The compression of tunnel manganese oxides is related to the tunnel distortion and the size of the tunnel.

  6. X-ray microscopy using synchrotron radiation

    SciTech Connect

    Jones, K.W.; Gordon, B.M.; Hanson, A.L.; Pounds, J.G.; Rivers, M.L.; Schidlovsky, G.; Smith, J.V.; Spanne, P.; Sutton, S.R.

    1989-01-01

    The system for x-ray microscopy now being developed at the X-26 beam line of the Brookhaven National Synchrotron Light Source (NSLS) is described here. Examples of the use of x-ray microscopy for trace element geochemistry, biology and medicine, and materials investigations are given to emphasize the scientific applications of the technique. Future directions for the improvement and further development of the X-26 microscope and of the x-ray microscopy field in general are discussed. 11 refs., 7 figs.

  7. New Insights into Fracture Evolution in Rocks Relevant to the Geological Carbon Sequestration from In Situ Synchrotron X-ray Microtomography

    NASA Astrophysics Data System (ADS)

    Voltolini, M.; Ajo Franklin, J. B.; Yang, L.

    2015-12-01

    Fractured rocks rich in carbonates can be found as candidates for both reservoirs and seals of importance to GCS; however, the mechanisms involved in the evolution of the fractures are still not fully understood despite its importance for both reservoir rocks, where CO2-induced variations in aperture can significantly change injectivity, as well as seals, where feedbacks between dissolution and flow could lead to either leakage or self-sealing behavior. Two samples, a dolomite and a carbonate rich shale, were analyzed in situ using dynamic synchrotron X-ray microtomography (SXR-μCT), flowing CO2-saturated water along a cylindrical sample (~3/8" diameter, ~1" height) with a single fracture along the flow direction. Experiments lasted about one week each, with a constant flow of 5 μl/min under 1400 psi pore pressure and 1700 psi confining pressure. XR tomographic scans were taken at different time steps to monitor the evolution of the fracture characteristics. A comparison of the two systems will be presented. In both samples significant dissolution occurs during the experiment, with the development of wormholes clearly visible from segmented fracture aperture maps. Both samples develop a weathered zone on the fracture surface, but the microstructure and the extent of this weathered layer is markedly different. Effluent chemistry analysis and SEM/EDS also help to reveal some time-dependent processes (e.g. increase in the dolomite dissolution rate with time). In both the experiments the crack surfaces becomes enriched in less soluble minerals and some migration of fines is visible as well. The mobilization of clays in the shale sample is unexpectedly small. With the extent of the dissolution allowed by our experiments, no noticeable closing of the fracture due to the confining pressure is visible, and the contact area evolution is barely noticeable. Peclet and Dahmköhler numbers for this experiments seem to suggest that the self-sealing behavior observed in prior

  8. Nanophase evolution at semiconductor/electrolyte interface in situ probed by time-resolved high-energy synchrotron x-ray diffraction.

    SciTech Connect

    Sun, Y.; Ren, Y.; Haeffner, D. R.; Almer, J. D.; Wang, L.; Yang, W.; Truong, T. T.

    2010-09-01

    Real-time evolution of nanoparticles grown at the semiconductor/electrolyte interface formed between a single crystalline n-type GaAs wafer and an aqueous solution of AgNO{sub 3} has been studied by using high-energy synchrotron X-ray diffraction. The results reveal the distinct nucleation and growth steps involved in the growth of anisotropic Ag nanoplates on the surface of the GaAs wafer. For the first time, a quick transit stage is observed to be responsible for the structural transformation of the nuclei to form structurally stable seeds that are critical for guiding their anisotropic growth into nanoplates. Reaction between a GaAs wafer and AgNO{sub 3} solution at room temperature primarily produces Ag nanoplates on the surface of the GaAs wafer in the dark and at room temperature. In contrast, X-ray irradiation can induce charge separation in the GaAs wafer to drive the growth of nanoparticles made of silver oxy salt (Ag{sub 7}NO{sub 11}) and silver arsenate (Ag{sub 3}AsO{sub 4}) at the semiconductor/electrolyte interface if the GaAs wafer is illuminated by the X-ray and reaction time is long enough.

  9. Nanophase evolution at semiconductor/electrolyte interface in situ probed by time-resolved high-energy synchrotron X-ray diffraction.

    PubMed

    Sun, Yugang; Ren, Yang; Haeffner, Dean R; Almer, Jonathan D; Wang, Lin; Yang, Wenge; Truong, Tu T

    2010-09-01

    Real-time evolution of nanoparticles grown at the semiconductor/electrolyte interface formed between a single crystalline n-type GaAs wafer and an aqueous solution of AgNO(3) has been studied by using high-energy synchrotron X-ray diffraction. The results reveal the distinct nucleation and growth steps involved in the growth of anisotropic Ag nanoplates on the surface of the GaAs wafer. For the first time, a quick transit stage is observed to be responsible for the structural transformation of the nuclei to form structurally stable seeds that are critical for guiding their anisotropic growth into nanoplates. Reaction between a GaAs wafer and AgNO(3) solution at room temperature primarily produces Ag nanoplates on the surface of the GaAs wafer in the dark and at room temperature. In contrast, X-ray irradiation can induce charge separation in the GaAs wafer to drive the growth of nanoparticles made of silver oxy salt (Ag(7)NO(11)) and silver arsenate (Ag(3)AsO(4)) at the semiconductor/electrolyte interface if the GaAs wafer is illuminated by the X-ray and reaction time is long enough.

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

    PubMed

    Huang, Xiaoli; Li, Fangfei; Zhou, Qiang; Meng, Yue; Litasov, Konstantin D; Wang, Xin; Liu, Bingbing; Cui, Tian

    2016-01-01

    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-Grüneisen-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. B 114, 298 (2010)). 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. PMID:26883479

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

    PubMed Central

    Huang, Xiaoli; Li, Fangfei; Zhou, Qiang; Meng, Yue; Litasov, Konstantin D.; Wang, Xin; Liu, Bingbing; Cui, Tian

    2016-01-01

    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–Grüneisen-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. B 114, 298 (2010)). 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. PMID:26883479

  12. In situ synchrotron study of liquid phase separation process in Al-10 wt.% Bi immiscible alloys by radiography and small angle X-ray scattering

    NASA Astrophysics Data System (ADS)

    Lu, W. Q.; Zhang, S. G.; Li, J. G.

    2016-03-01

    Liquid phase separation process of immiscible alloys has been repeatedly tuned to create special structure for developing materials with unique properties. However, the fundamental understanding of the liquid phase separation process is still under debate due to the characteristics of immiscible alloys in opacity and high temperature environment of alloy melt. Here, the liquid phase separation process in solidifying Al-Bi immiscible alloys was investigated by synchrotron radiography and small angle X-ray scattering. We provide the first direct evidence of surface segregation prior to liquid decomposition and present that the time dependence on the number of Bi droplets follows Logistic curve. The liquid decomposition results from a nucleation and growth process rather than spinodal decomposition mechanism because of the positive deviation from Porod's law. We also found that the nanometer-sized Bi-rich droplets in Al matrix melt present mass fractal characteristics.

  13. 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; Meng, Yue; Litasov, Konstantin D.; Wang, Xin; Liu, Bingbing; Cui, Tian

    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

  14. Phase Transformation in Sm{sub 2}O{sub 3} at High Pressure: in Situ Synchrotron X-Ray Diffraction Study And Ab Initio DFT Calculation

    SciTech Connect

    Guo, Q.X.; Zhao, Y.S.; Jiang, C.; Mao, W.L.; Wang, Z.W.; /Cornell U., CHESS

    2009-06-09

    Sm{sub 2}O{sub 3} was compressed at room temperature up to 44.0 GPa and then decompressed back to ambient pressure. In situ X-ray diffraction was used to monitor the structural changes in the sample. A cubic to hexagonal phase transformation was observed in Sm{sub 2}O{sub 3} for the first time. After decompression back to ambient pressure, the hexagonal phase was not quenchable and transformed to a monoclinic phase. Ab initio Density-Functional-Theory (DFT) calculations were performed to obtain theoretical data for comparison with the experimental results and elucidation of the transformation mechanism. A possible phase transformation mechanism that is consistent with the experimental results and theoretical calculations is proposed.

  15. 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.

  16. Pressure-induced amorphization of cubic ZrW{sub 2}O{sub 8} studied in situ and ex situ by synchrotron x-ray diffraction and absorption

    SciTech Connect

    Varga, Tamas; Wilkinson, Angus P.; Jupe, Andrew C.; Lind, Cora; Bassett, William A.; Zha Changsheng

    2005-07-01

    The behavior of cubic ZrW{sub 2}O{sub 8} on compression in a DAC to 7.6 GPa was examined in situ by a combination of synchrotron x-ray diffraction and x-ray absorption spectroscopy (XAS). These data were compared with x-ray absorption measurements on an amorphous sample of ZrW{sub 2}O{sub 8} recovered from 7.5 GPa in a multianvil apparatus. The in situ diffraction data show the complete formation of orthorhombic ZrW{sub 2}O{sub 8} at low pressure (<0.5 GPa), and amorphization onset at >2.4 GPa with completion at <7.6 GPa. The corresponding in situ XAS data suggest a continuous evolution of the local tungsten coordination environment on compression after forming the orthorhombic phase, with the average W-O bond length increasing, indicating an increase in the average coordination number, and the W L{sub I} pre-edge peak decreasing in magnitude, indicating a movement toward tungsten coordination that is closer to centrosymmetric These observations are inconsistent with a model for the amorphization that simply involves a loss of orientational/positional order among existing coordination polyhedra. The XANES data for the amorphous sample recovered from the multianvil apparatus are unlike any of the XANES seen in the in situ measurements, suggesting that the local structure in the glassy material relaxes on decompression. The XANES for the recovered sample are very similar to those for ammonium paratungstate, a material that contains tungsten in a variety of heavily distorted octahedral environments.

  17. 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.

  18. In situ 3D topographic and shape analysis by synchrotron radiation X-ray microtomography for crystal form identification in polymorphic mixtures

    NASA Astrophysics Data System (ADS)

    Yin, Xian-Zhen; Xiao, Ti-Qiao; Nangia, Ashwini; Yang, Shuo; Lu, Xiao-Long; Li, Hai-Yan; Shao, Qun; He, You; York, Peter; Zhang, Ji-Wen

    2016-04-01

    Polymorphism denotes the existence of more than one crystal structure of a substance, and great practical and theoretical interest for the chemical and pharmaceutical industries. In many cases, it is challenging to produce a pure crystal form and establish a sensitive detection method for the identification of crystal form in a mixture of polymorphs. In this study, an accurate and sensitive method based on synchrotron radiation X-ray computed microtomography (SR-μCT) was devised to identify the polymorphs of clopidogrel bisulphate (CLP). After 3D reconstruction, crystal particles were extracted and dozens of structural parameters were calculated. Whilst, the particle shapes of the two crystal forms were all irregular, the surface of CLP II was found to be rougher than CLP I. In order to classify the crystal form based on the quantitative morphological property of particles, Volume Bias Percentage based on Surface Smoothing (VBP) was defined and a new method based on VBP was successfully developed, with a total matching rate of 99.91% for 4544 particles and a lowest detectable limit of 1%. More important for the mixtures in solid pharmaceutical formulations, the interference of excipients can be avoided, a feature cannot achieved by other available analytical methods.

  19. In situ strain profiling of elastoplastic bending in Ti-6Al-4V alloy by synchrotron energy dispersive x-ray diffraction

    SciTech Connect

    Croft, M.; Shukla, V.; Akdogan, E. K.; Sadangi, R.; Ignatov, A.; Balarinni, L.; Tsakalakos, T.; Jisrawi, N.; Zhong, Z.; Horvath, K.

    2009-05-01

    Elastic and plastic strain evolution under four-point bending has been studied by synchrotron energy dispersive x-ray diffraction. Measured strain profiles across the specimen thickness showed an increasing linear elastic strain gradient under increasing four-point bending load up to approx2 kN. The bulk elastic modulus of Ti-6Al-4V was determined as 118 GPa. The onset of plastic deformation was found to set in at a total in-plane strain of approx0.008, both under tension and compression. Plastic deformation under bending is initiated in the vicinity of the surface and at a stress of 1100 MPa, and propagates inward, while a finite core region remains elastically deformed up to 3.67 kN loading. The onset of the plastic regime and the plastic regime itself has been verified by monitoring the line broadening of the (100) peak of alpha-Ti. The effective compression/tension stress-strain curve has been obtained from the scaling collapse of strain profile data taken at seven external load levels. A similar multiple load scaling collapse of the plastic strain variation has also been obtained. The level of precision in strain measurement reported herein was evaluated and found to be 1.5x10{sup -5} or better.

  20. In situ 3D topographic and shape analysis by synchrotron radiation X-ray microtomography for crystal form identification in polymorphic mixtures

    PubMed Central

    Yin, Xian-Zhen; Xiao, Ti-Qiao; Nangia, Ashwini; Yang, Shuo; Lu, Xiao-Long; Li, Hai-Yan; Shao, Qun; He, You; York, Peter; Zhang, Ji-Wen

    2016-01-01

    Polymorphism denotes the existence of more than one crystal structure of a substance, and great practical and theoretical interest for the chemical and pharmaceutical industries. In many cases, it is challenging to produce a pure crystal form and establish a sensitive detection method for the identification of crystal form in a mixture of polymorphs. In this study, an accurate and sensitive method based on synchrotron radiation X-ray computed microtomography (SR-μCT) was devised to identify the polymorphs of clopidogrel bisulphate (CLP). After 3D reconstruction, crystal particles were extracted and dozens of structural parameters were calculated. Whilst, the particle shapes of the two crystal forms were all irregular, the surface of CLP II was found to be rougher than CLP I. In order to classify the crystal form based on the quantitative morphological property of particles, Volume Bias Percentage based on Surface Smoothing (VBP) was defined and a new method based on VBP was successfully developed, with a total matching rate of 99.91% for 4544 particles and a lowest detectable limit of 1%. More important for the mixtures in solid pharmaceutical formulations, the interference of excipients can be avoided, a feature cannot achieved by other available analytical methods. PMID:27097672

  1. Abundance and Charge State of Implanted Solar Wind Transition Metals in Individual Apollo 16 and 17 Lunar Soil Plagioclase Grains Determined In Situ Using Synchrotron X-ray Fluorescence

    SciTech Connect

    Kitts, K.; Sutton, S.; Newville, M.

    2007-03-06

    We report (1) a new method for determining the relative abundances in situ of Cr, Mn, Fe and Ni in implanted solar wind in individual Apollo 16 and 17 lunar plagioclases via synchrotron X-ray fluorescence and (2) the charge states of these metals. By virture of its mass alone, the Sun provides a representative composition of the solar system and can be used as a background against which to gauge excesses or deficiencies of specific components. One way of sampling the Sun is by measuring solar wind implanted ions in lunar soil grains. Such measurements are valuable because of their long exposure ages which compliment shorter time scale collections, such as those obtained by the Genesis spacecraft. Kitts et al. sought to determine the isotopic composition of solar Cr by analyzing the solar wind implanted into plagioclase grains from Apollo 16 lunar soils. The isotopic composition of the solar wind bearing fraction was anomalous and did not match any other known Cr isotopic signature. This could only be explained by either (1) an enrichment in the solar wind of heavy Cr due to spallation in the solar atmosphere or (2) that the Earth and the various parent bodies of the meteorites are distinct from the Sun and must have formed from slightly different mixes of presolar materials. To help resolve this issue, we have developed a wholly independent method for determining the relative abundances of transition metals in the solar wind implanted in individual lunar soil grains. This method is based on in situ abundance measurements by microbeam x-ray fluorescence in both the implantation zone and bulk grains using the synchrotron x-ray microprobe at the Advanced Photon Source (GSECARS sector 13) at Argonne National Laboratory. Here, we report results for Apollo 16 and 17 plagioclase grains. Additionally, a micro-XANES technique was used to determine charge states of the implanted Cr, Mn, Fe and Ni.

  2. Challenges for Synchrotron X-Ray Optics

    NASA Astrophysics Data System (ADS)

    Freund, Andreas K.

    2002-12-01

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

  3. Anhydrate to hydrate solid-state transformations of carbamazepine and nitrofurantoin in biorelevant media studied in situ using time-resolved synchrotron X-ray diffraction.

    PubMed

    Boetker, Johan P; Rantanen, Jukka; Arnfast, Lærke; Doreth, Maria; Raijada, Dhara; Loebmann, Korbinian; Madsen, Cecilie; Khan, Jamal; Rades, Thomas; Müllertz, Anette; Hawley, Adrian; Thomas, Diana; Boyd, Ben J

    2016-03-01

    Transformation of the solid-state form of a drug compound in the lumen of the gastrointestinal tract may alter the drug bioavailability and in extreme cases result in patient fatalities. The solution-mediated anhydrate-to-hydrate phase transformation was examined using an in vitro model with different biorelevant media, simulated fasted and fed state intestinal fluids containing bile salt and dioleoylphosphatidylcholine (DOPC) micelles, DOPC/sodium dodecyl sulfate (SDS) mixture, bile salt solution and water. Two anhydrate compounds (carbamazepine, CBZ and nitrofurantoin, NF) with different overall transformation time into hydrate form were used as model compounds. The transformations were monitored using direct structural information from time-resolved synchrotron X-ray diffraction. The kinetics of these transformations were estimated using multivariate data analysis (principal component analysis, PCA) and compared to those for nitrofurantoin (NF). The study showed that the solution-mediated phase transformation of CBZ anhydrate was remarkably faster in the DOPC/SDS medium compared to transformation in all the other aqueous dispersion media. The conversion time for CBZ anhydrate in water was shorter than for DOPC/SDS but still faster than the conversion seen in fed and fasted state micellar media. The conversion of CBZ anhydrate to hydrate was the slowest in the solution containing bile salt alone. In contrast, the solution-mediated phase transformations of NF did only show limited kinetic dependence on the dispersion media used, indicating the complexity of the nucleation process. Furthermore, when the CBZ and NF material was compacted into tablets the transformation times were remarkably slower. Results suggest that variations in the composition of the contents of the stomach/gut may affect the recrystallization kinetics, especially when investigating compounds with relatively fast overall transformation time, such as CBZ.

  4. Rupture Orientation and Strain-induced Crystallization of Polymer Chain and Network in Vulcanized Polyisoprene During Uniaxial Deformation by in-situ Electron Spin Resonance(ESR) and Synchrotron X-ray Analysis

    SciTech Connect

    S Toki; R Takagi; M Ito; B Hsiao

    2011-12-31

    Different network structures of vulcanized polyisoprene rubbers were studied by in-situ ESR and synchrotron X-ray during deformation to analyze the rupture, orientation, and strain-induced crystallization of polymer chains and network points. Rupture of network points occur, depending on network structure, and create an un-reversible change in vulcanized rubber. The flexibility of network points affects the possibility of rupture, polymer orientation and strain-induced crystallization. Peroxide vulcanized network is rigid and un-rupturable. Poly-sulfide rich vulcanized network is more flexible and less rupturable than mono-sulfide rich vulcanized network. Chain flexibility and rupturability of network points affect the strain-induced crystallization and stress-strain relation.

  5. Dynamics of mineral crystallization at inclusion-garnet interface from precipitated slab-derived fluid phase: first in-situ synchrotron x-ray measurements

    NASA Astrophysics Data System (ADS)

    Malaspina, Nadia; Alvaro, Matteo; Campione, Marcello; Nestola, Fabrizio

    2015-04-01

    Remnants of the fluid phase at ultrahigh pressure (UHP) in subduction environments may be preserved as primary multiphase inclusions in UHP minerals. These inclusions are frequently hosted by minerals stable at mantle depths, such as garnet, and show the same textural features as fluid inclusions. The mineral infillings of the solid multiphase inclusions are generally assumed to have crystallized by precipitation from the solute load of dense supercritical fluids equilibrating with the host rock. Notwithstanding the validity of this assumption, the mode of crystallization of daughter minerals during precipitation within the inclusion and/or the mechanism of interaction between the fluid at supercritical conditions and the host mineral are still poorly understood from a crystallographic point of view. A case study is represented by garnet orthopyroxenites from the Maowu Ultramafic Complex (China) deriving from harzburgite precursors metasomatised at ~ 4 GPa, 750 °C by a silica- and incompatible trace element-rich fluid phase. This metasomatism produced poikilitic orthopyroxene and inclusion-rich garnet porphyroblasts. Solid multiphase primary inclusions in garnet display a size within a few tens of micrometers and negative crystal shapes. Infilling minerals (spinel: 10-20 vol.%; amphibole, chlorite, talc, mica: 80- 90 vol.%) occur with constant volume ratios and derive from trapped solute-rich aqueous fluids. To constrain the possible mode of precipitation of daughter minerals, we performed for the first time a single-crystal X-ray diffraction experiment by means of Synchrotron Radiation at DLS-Diamond Light Source. In combination with electron probe microanalyses, this measurement allowed the unique identification of each mineral phase and their reciprocal orientations. We demonstrated the epitaxial relationship between spinel and garnet and between some hydrous minerals. Epitaxy drives a first-stage nucleation of spinel under near-to-equilibrium conditions

  6. On the P-induced behavior of the zeolite phillipsite: an in situ single-crystal synchrotron X-ray diffraction study

    NASA Astrophysics Data System (ADS)

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

    2016-08-01

    The elastic behavior and the structural evolution at high pressure of a natural phillipsite have been investigated by in situ single-crystal X-ray diffraction up to 9.44 GPa, using a diamond anvil cell and the nominally penetrating P-transmitting fluid methanol:ethanol:water (16:3:1) mix. Although no phase transition was observed within the P-range investigated, two different compressional regimes occur. Between 0.0001 and 2.0 GPa, the refined elastic parameters, calculated by a second-order Birch-Murnaghan equation of state (BM-EoS) fit, are V 0 = 1005(1) Å3, K 0 = 89(8) GPa for the unit-cell volume; a 0 = 9.914(7) Å, K a = 81(12) GPa for the a-axis; b 0 = 14.201(9) Å, K b = 50(5) GPa for the b-axis; and c 0 = 8.707(2) Å, K c = 107(8) GPa for the c-axis (K a :K b :K c ~1.62:1:2.14). Between 2.0 and 9.4 GPa, a P-induced change in the configuration of H2O molecules, coupled with a change in the tilting mechanisms of the framework tetrahedra, gives rise to a second compressional regime, in which the phillipsite structure is softer if compared to the first compressional range. In the second compressional regime, the refined elastic parameters, calculated by a second-order BM-EoS fit, are V 0 = 1098 (7) Å3, K 0 = 18.8(7) GPa for the unit-cell volume; a 0 = 10.07(3) Å, K a = 30(2) GPa for the a-axis; b 0 = 14.8(1) Å, K b = 11(1) GPa for the b-axis; and c 0 = 8.94(2) Å, K c = 21(1) GPa for the c-axis (K a :K b :K c ~2.72:1:1.90). The evolution of the monoclinic β angle with pressure shows two distinct trends in the two compressional regimes: with a negative slope between 0.0001 and 2.0 GPa, and a positive slope between 2.0 and 9.4 GPa. The mechanisms, at the atomic scale, that govern the two compressional regimes of the phillipsite structure are described.

  7. Oxygen storage properties of La1-xSrxFeO3-δ for chemical-looping reactions–An in-situ neutron and synchrotron X-ray study

    DOE PAGES

    Taylor, Daniel D.; Schreiber, Nathaniel J.; Levitas, Benjamin D.; Xu, Wenqian; Rodriguez, Efrain E.; Whitfield, Pamela S.

    2016-05-16

    Oxygen storage materials (OSMs) provide lattice oxygen for a number of chemical-looping reactions including natural gas combustion and methane reforming. La1–xSrxFeO3-δ has shown promise for use as an OSM in methane reforming reactions due to its high product selectivity, fast oxide diffusion, and cycle stability. Here, we investigate the structural evolution of the series La1–xSrxFeO3-δ for x = 0, 1/3, 1/2, 2/3, and 1, using in situ synchrotron X-ray and neutron diffraction, as it is cycled under the conditions of a chemical-looping reactor (methane and oxygen atmospheres). In the compositions x = 1/3, 1/2, 2/3, and 1, we discover anmore » envelope , or temperature range, of oxygen storage capacity (OSC), where oxygen can easily and reversibly be inserted and removed from the OSM. Our in situ X-ray and neutron diffraction results reveal that while samples with higher Sr contents had a higher OSC, those same samples suffered from slower reaction kinetics and some, such as the x = 1/2 and x = 2/3 compositions, had local variations in Sr content, which led to inhomogeneous regions with varying reaction rates. Therefore, we highlight the importance of in situ diffraction studies, and we propose that these measurements are required for the thorough evaluation of future candidate OSMs. Furthermore, we recommend La2/3Sr1/3FeO3-δ as the optimal OSM in the series because its structure remains homogeneous throughout the reaction, and its OSC envelope is similar to that of the higher doped materials.« less

  8. Synchrotron x-ray fluorescence and extended x-ray absorption fine structure analysis

    SciTech Connect

    Chen, J.R.; Gordon, B.M.; Hanson, A.L.; Jones, K.W.; Kraner, H.W.; Chao, E.C.T.; Minkin, J.A.

    1984-01-01

    The advent of dedicated synchrotron radiation sources has led to a significant increase in activity in many areas of science dealing with the interaction of x-rays with matter. Synchrotron radiation provides intense, linearly polarized, naturally collimated, continuously tunable photon beams, which are used to determine not only the elemental composition of a complex, polyatomic, dilute material but also the chemical form of the elements with improved accuracy. Examples of the application of synchrotron radiation include experiments in synchrotron x-ray fluorescence (SXRF) analysis and extended x-ray absorption fine structure (EXAFS) analysis. New synchrotron radiation x-ray microprobes for elemental analysis in the parts per billion range are under construction at several laboratories. 76 references, 24 figures.

  9. In-situ Measurements of Colloid Transport and Retention Using Synchroton X-ray Fluorescence

    Technology Transfer Automated Retrieval System (TEKTRAN)

    The physics regarding the retention and mobilization of colloids in saturated and unsaturated conditions remains poorly understood, partially due to the inability to measure colloid concentrations in-situ. In this study, we attached Cd+2 ions to clay colloids, and used synchrotron x-rays to cause th...

  10. An atomic layer deposition chamber for in situ x-ray diffraction and scattering analysis

    SciTech Connect

    Geyer, Scott M.; Methaapanon, Rungthiwa; Kim, Woo-Hee; Bent, Stacey F.; Johnson, Richard W.; Van Campen, Douglas G.; Metha, Apurva

    2014-05-15

    The crystal structure of thin films grown by atomic layer deposition (ALD) will determine important performance properties such as conductivity, breakdown voltage, and catalytic activity. We report the design of an atomic layer deposition chamber for in situ x-ray analysis that can be used to monitor changes to the crystal structural during ALD. The application of the chamber is demonstrated for Pt ALD on amorphous SiO{sub 2} and SrTiO{sub 3} (001) using synchrotron-based high resolution x-ray diffraction, grazing incidence x-ray diffraction, and grazing incidence small angle scattering.

  11. Development and applications of an epifluorescence module for synchrotron x-ray fluorescence microprobe imaging

    SciTech Connect

    Miller, Lisa M.; Smith, Randy J.; Ruppel, Meghan E.; Ott, Cassandra H.; Lanzirotti, Antonio

    2005-06-15

    Synchrotron x-ray fluorescence (XRF) microprobe is a valuable analysis tool for imaging trace element composition in situ at a resolution of a few microns. Frequently, epifluorescence microscopy is beneficial for identifying the region of interest. To date, combining epifluorescence microscopy with x-ray microprobe has involved analyses with two different microscopes. We report the development of an epifluorescence module that is integrated into a synchrotron XRF microprobe beamline, such that visible fluorescence from a sample can be viewed while collecting x-ray microprobe images simultaneously. This unique combination has been used to identify metal accumulation in Alzheimer's disease plaques and the mineral distribution in geological samples. The flexibility of this accessory permits its use on almost any synchrotron x-ray fluorescence microprobe beamline and applications in many fields of science can benefit from this technology.

  12. The metrology of spherical shells using synchrotron x ray microtomography

    NASA Technical Reports Server (NTRS)

    Hmelo, Anthony B.; Allen, James L.; Damico, Kevin L.

    1990-01-01

    With recent advances in solid state imaging technology and the increasing availability of synchrotron x-ray radiation sources, synchrotron x-ray microtomography is emerging as a nondestructive technique for the evaluation of the structure and composition of small specimens with spatial resolution in the micron range. Synchrotron radiation offers the following advantages over conventional x-ray sources: high brightness, continuous emission which is tunable over a large energy range, faster data collection rates, and a highly collimated beam of large cross section permitting the illumination of large specimens. Synchrotron x-ray microtomography enables the structure of individual spheres to be evaluated in order to reveal the concentricity and sphericity of the internal void and the uniformity of the shell wall in the case of high quality spherical shells for Sandia National Laboratories' Inertial Confinement Fusion project.

  13. In situ synchrotron X-ray diffraction investigation of the evolution of a PbO₂/PbSO₄ surface layer on a copper electrowinning Pb anode in a novel electrochemical flow cell.

    PubMed

    Clancy, Marie; Styles, Mark J; Bettles, Colleen J; Birbilis, Nick; Chen, Miao; Zhang, Yansheng; Gu, Qinfen; Kimpton, Justin A; Webster, Nathan A S

    2015-03-01

    This paper describes the quantitative measurement, by in situ synchrotron X-ray diffraction (S-XRD) and subsequent Rietveld-based quantitative phase analysis and thickness calculations, of the evolution of the PbO2 and PbSO4 surface layers formed on a pure lead anode under simulated copper electrowinning conditions in a 1.6 M H2SO4 electrolyte at 318 K. This is the first report of a truly in situ S-XRD study of the surface layer evolution on a Pb substrate under cycles of galvanostatic and power interruption conditions, of key interest to the mining, solvent extraction and lead acid battery communities. The design of a novel reflection geometry electrochemical flow cell is also described. The in situ S-XRD results show that β-PbO2 forms immediately on the anode under galvanostatic conditions, and undergoes continued growth until power interruption where it transforms to PbSO4. The kinetics of the β-PbO2 to PbSO4 conversion decrease as the number of cycles increases, whilst the amount of residual PbO2 increases with the number of cycles due to incomplete conversion to PbSO4. Conversely, complete transformation of PbSO4 to β-PbO2 was observed in each cycle. The results of layer thickness calculations demonstrate a significant volume change upon PbSO4 to β-PbO2 transformation. PMID:25723938

  14. New pressure flow cell to monitor BaSO4 precipitation using synchrotron in situ angle-dispersive X-ray diffraction.

    PubMed

    Hennessy, Alison; Graham, Gordon; Hastings, Jerry; Siddons, D Peter; Zhong, Zhong

    2002-09-01

    A flow cell has been commissioned to monitor in situ precipitation reactions under non-ambient conditions. The majority of high-pressure systems use anvils and presses to obtain high pressures around a small reaction area; however, this prototype is unique in that solutions may be examined as they flow through the cell under pressure. The cell is made of single-crystal silicon, which is capable of withstanding the high pressures created by liquid flow within the cell. With the capability of reaching pressures of up to 4 x 10(7) Pa, the cell is ideal for work on geological and oilfield systems. Here it is used to examine the formation of barium sulfate scale in situ under non-ambient conditions using angle-dispersive XRD on beamline X17b1 at the NSLS.

  15. Investigation of Phase Transformations in High-Alloy Austenitic TRIP Steel Under High Pressure (up to 18 GPa) by In Situ Synchrotron X-ray Diffraction and Scanning Electron Microscopy

    NASA Astrophysics Data System (ADS)

    Ackermann, Stephanie; Martin, Stefan; Schwarz, Marcus R.; Schimpf, Christian; Kulawinski, Dirk; Lathe, Christian; Henkel, Sebastian; Rafaja, David; Biermann, Horst; Weidner, Anja

    2016-01-01

    In order to clarify the difference between the deformation-induced ɛ-martensite ( ɛ 1) and the pressure-induced ɛ-iron ( ɛ 2), high-pressure quasi-hydrostatic experiments were performed on a low-carbon, high-alloy metastable austenitic steel. In situ synchrotron X-ray diffraction measurements as well as post-mortem investigations of the microstructure by electron backscatter diffraction were carried out to study the microstructural transformations. Three processes were observed during compression experiments: first, the formation of deformation-induced hexagonal ɛ 1-martensite, as well as small nuclei of deformation-induced bcc α'-martensite ( α 1') within the fcc γ-matrix due to non-hydrostaticity in the experiments; second, the onset of the phase transformation from the metastable fcc γ-austenite into the hexagonal pressure-induced ɛ 2-iron phase occurred at around 6 GPa; third, during decompression, the hexagonal pressure-induced ɛ 2-iron transformed partially into bcc α'-martensite ( α 2'). Completely different characteristics with regard to habitus as well as to orientation relationships were observed between the pressure-induced phases ( ɛ 2-iron phase and α 2'-martensite) and the deformation-induced martensites ( ɛ 1- and α 1'-martensite).

  16. Synchrotron-Radiation Induced X-Ray Emission (SRIXE)

    SciTech Connect

    Jones, Keith W.

    1999-09-01

    Elemental analysis using emission of characteristic x rays is a well-established scientific method. The success of this analytical method is highly dependent on the properties of the source used to produce the x rays. X-ray tubes have long existed as a principal excitation source, but electron and proton beams have also been employed extensively. The development of the synchrotron radiation x-ray source that has taken place during the past 40 years has had a major impact on the general field of x-ray analysis. Even tier 40 years, science of x-ray analysis with synchrotron x-ray beams is by no means mature. Improvements being made to existing synchrotron facilities and the design and construction of new facilities promise to accelerate the development of the general scientific use of synchrotron x-ray sources for at least the next ten years. The effective use of the synchrotron source technology depends heavily on the use of high-performance computers for analysis and theoretical interpretation of the experimental data. Fortunately, computer technology has advanced at least as rapidly as the x-ray technology during the past 40 years and should continue to do so during the next decade. The combination of these technologies should bring about dramatic advances in many fields where synchrotron x-ray science is applied. It is interesting also to compare the growth and rate of acceptance of this particular research endeavor to the rates for other technological endeavors. Griibler [1997] cataloged the time required for introduction, diffusion,and acceptance of technological, economic, and social change and found mean values of 40 to 50 years. The introduction of the synchrotron source depends on both technical and non-technical factors, and the time scale at which this seems to be occurring is quite compatible with what is seen for other major innovations such as the railroad or the telegraph. It will be interesting to see how long the present rate of technological change

  17. Gas cell for in situ soft X-ray transmission-absorption spectroscopy of materials

    SciTech Connect

    Drisdell, W. S.; Kortright, J. B.

    2014-07-15

    A simple gas cell design, constructed primarily from commercially available components, enables in situ soft X-ray transmission-absorption spectroscopy of materials in contact with gas at ambient temperature. The cell has a minimum X-ray path length of 1 mm and can hold gas pressures up to ∼300 Torr, and could support higher pressures with simple modifications. The design enables cycling between vacuum and gas environments without interrupting the X-ray beam, and can be fully sealed to allow for measurements of air-sensitive samples. The cell can attach to the downstream port of any appropriate synchrotron beamline, and offers a robust and versatile method for in situ measurements of certain materials. The construction and operation of the cell are discussed, as well as sample preparation and proper spectral analysis, illustrated by examples of spectral measurements. Potential areas for improvement and modification for specialized applications are also mentioned.

  18. In-situ observations of catalytic surface reactions with soft x-rays under working conditions

    NASA Astrophysics Data System (ADS)

    Toyoshima, Ryo; Kondoh, Hiroshi

    2015-03-01

    Catalytic chemical reactions proceeding on solid surfaces are an important topic in fundamental science and industrial technologies such as energy conversion, pollution control and chemical synthesis. Complete understanding of the heterogeneous catalysis and improving its efficiency to an ultimate level are the eventual goals for many surface scientists. Soft x-ray is one of the prime probes to observe electronic and structural information of the target materials. Most studies in surface science using soft x-rays have been performed under ultra-high vacuum conditions due to the technical limitation, though the practical catalytic reactions proceed under ambient pressure conditions. However, recent developments of soft x-ray based techniques operating under ambient pressure conditions have opened a door to the in-situ observation of materials under realistic environments. The near-ambient-pressure x-ray photoelectron spectroscopy (NAP-XPS) using synchrotron radiation enables us to observe the chemical states of surfaces of condensed matters under the presence of gas(es) at elevated pressures, which has been hardly conducted with the conventional XPS technique. Furthermore, not only the NAP-XPS but also ambient-pressure compatible soft x-ray core-level spectroscopies, such as near-edge absorption fine structure (NEXAFS) and x-ray emission spectroscopy (XES), have been significantly contributing to the in-situ observations. In this review, first we introduce recent developments of in-situ observations using soft x-ray techniques and current status. Then we present recent new findings on catalytically active surfaces using soft x-ray techniques, particularly focusing on the NAP-XPS technique. Finally we give a perspective on the future direction of this emerging technique.

  19. Synchrotron X-ray phase nano-tomography-based analysis of the lacunar-canalicular network morphology and its relation to the strains experienced by osteocytes in situ as predicted by case-specific finite element analysis.

    PubMed

    Varga, Peter; Hesse, Bernhard; Langer, Max; Schrof, Susanne; Männicke, Nils; Suhonen, Heikki; Pacureanu, Alexandra; Pahr, Dieter; Peyrin, Françoise; Raum, Kay

    2015-04-01

    Osteocytes are hypothesized to regulate bone remodeling guided by both biological and mechanical stimuli. Morphology of the lacunar-canalicular network of osteocytes has been hypothesized to be strongly related to the level of mechanical loading and to various bone diseases. Finite element modeling could help to better understand the mechanosensation process by predicting the physiological strain environment. The aims of this study were to (i) quantify the lacunar-canalicular morphology in the cortex of the human femur; (ii) predict the in situ local deformations around and in osteocytes by means of case-specific finite element models; and (iii) investigate the potential relationship between morphology and deformations. Human femoral cortical bone samples were imaged using synchrotron X-ray phase nano-tomography with 50 nm voxel size. Rectangular volumes of interest were selected to contain single osteocyte lacunae and the surrounding matrix. Lacunar-canalicular morphology was quantified and the cell geometry was artificially reconstructed based on a priori assumptions. Finite element models of the volumes of interest were generated, containing the extracellular matrix, osteocyte and peri-cellular matrix, and subjected to uniaxial compression. The morphological analysis revealed that canalicular number was dictated by lacunar size, that the spacing of canaliculi fell within a narrow range, suggesting that these pores are well distributed throughout the bone matrix and indicated the trend that lacunae at the outer osteon boundary were less elongated than others. No apparent relationship was found between the morphological parameters and the predicted strains. The globally applied strain was amplified locally by factors up to 10 and up to 70 in the extracellular matrix and the in cells, respectively. Cell deformations were localized mainly at the body-dendrite junctions, with magnitudes reaching the in vitro stimulatory threshold reported for osteocytes.

  20. Synchrotron X-ray footprinting on tour

    PubMed Central

    Bohon, Jen; D’Mello, Rhijuta; Ralston, Corie; Gupta, Sayan; Chance, Mark R.

    2014-01-01

    Synchrotron footprinting is a valuable technique in structural biology for understanding macromolecular solution-state structure and dynamics of proteins and nucleic acids. Although an extremely powerful tool, there is currently only a single facility in the USA, the X28C beamline at the National Synchrotron Light Source (NSLS), dedicated to providing infrastructure, technology development and support for these studies. The high flux density of the focused white beam and variety of specialized exposure environments available at X28C enables footprinting of highly complex biological systems; however, it is likely that a significant fraction of interesting experiments could be performed at unspecialized facilities. In an effort to investigate the viability of a beamline-flexible footprinting program, a standard sample was taken on tour around the nation to be exposed at several US synchrotrons. This work describes how a relatively simple and transportable apparatus can allow beamlines at the NSLS, CHESS, APS and ALS to be used for synchrotron footprinting in a general user mode that can provide useful results. PMID:24365913

  1. X-ray polarization splitting by a single crystal evaluated with synchrotron x-rays.

    PubMed

    Pereira, N R; Presura, R; Wallace, M; Kastengren, A

    2014-07-01

    In hexagonal crystals such as quartz, an asymmetric Bragg reflection from two equivalent internal crystal planes can separate unpolarized x-rays into two linearly polarized components. The perfectly polarized and tunable x-rays from a synchrotron are ideal to evaluate polarization spitting in detail. One unanticipated feature is that additional reflections from the crystal affect the diffraction intensity of the two polarized components, an effect that is unlikely to matter in polarization spectroscopy of radiating plasmas for which the crystal is intended.

  2. X-ray polarization splitting by a single crystal evaluated with synchrotron x-rays

    SciTech Connect

    Pereira, N. R.; Presura, R.; Wallace, M.; Kastengren, A.

    2014-07-15

    In hexagonal crystals such as quartz, an asymmetric Bragg reflection from two equivalent internal crystal planes can separate unpolarized x-rays into two linearly polarized components. The perfectly polarized and tunable x-rays from a synchrotron are ideal to evaluate polarization spitting in detail. One unanticipated feature is that additional reflections from the crystal affect the diffraction intensity of the two polarized components, an effect that is unlikely to matter in polarization spectroscopy of radiating plasmas for which the crystal is intended.

  3. X-ray imaging detectors for synchrotron and XFEL sources

    PubMed Central

    Hatsui, Takaki; Graafsma, Heinz

    2015-01-01

    Current trends for X-ray imaging detectors based on hybrid and monolithic detector technologies are reviewed. Hybrid detectors with photon-counting pixels have proven to be very powerful tools at synchrotrons. Recent developments continue to improve their performance, especially for higher spatial resolution at higher count rates with higher frame rates. Recent developments for X-ray free-electron laser (XFEL) experiments provide high-frame-rate integrating detectors with both high sensitivity and high peak signal. Similar performance improvements are sought in monolithic detectors. The monolithic approach also offers a lower noise floor, which is required for the detection of soft X-ray photons. The link between technology development and detector performance is described briefly in the context of potential future capabilities for X-ray imaging detectors. PMID:25995846

  4. Synchrotron X-ray emission from old pulsars

    NASA Astrophysics Data System (ADS)

    Kisaka, Shota; Tanaka, Shuta J.

    2014-09-01

    We study the synchrotron radiation as the observed non-thermal emission by the X-ray satellites from old pulsars (≳1-10 Myr) to investigate the particle acceleration in their magnetospheres. We assume that the power-law component of the observed X-ray spectra is caused by the synchrotron radiation from electrons and positrons in the magnetosphere. We consider two pair-production mechanisms of X-ray emitting particles, the magnetic and the photon-photon pair productions. High-energy photons, which ignite the pair production, are emitted via the curvature radiation of the accelerated particles. We use the analytical description for the radiative transfer and estimate the luminosity of the synchrotron radiation. We find that for pulsars with the spin-down luminosity Lsd ≲ 1033 erg s-1, the locations of the particle acceleration and the non-thermal X-ray emission are within ≲107 cm from the centre of the neutron star, where the magnetic pair production occurs. For pulsars with the spin-down luminosity Lsd ≲ 1031 erg s-1 such as J0108-1431, the synchrotron radiation is difficult to explain the observed non-thermal component even if we consider the existence of the strong and small-scale surface magnetic field structures.

  5. High-energy synchrotron X-ray radiography of shock-compressed materials

    NASA Astrophysics Data System (ADS)

    Rutherford, Michael E.; Chapman, David J.; Collinson, Mark A.; Jones, David R.; Music, Jasmina; Stafford, Samuel J. P.; Tear, Gareth R.; White, Thomas G.; Winters, John B. R.; Drakopoulos, Michael; Eakins, Daniel E.

    2015-06-01

    This presentation will discuss the development and application of a high-energy (50 to 250 keV) synchrotron X-ray imaging method to study shock-compressed, high-Z samples at Beamline I12 at the Diamond Light Source synchrotron (Rutherford-Appleton Laboratory, UK). Shock waves are driven into materials using a portable, single-stage gas gun designed by the Institute of Shock Physics. Following plate impact, material deformation is probed in-situ by white-beam X-ray radiography and complimentary velocimetry diagnostics. The high energies, large beam size (13 x 13 mm), and appreciable sample volumes (~ 1 cm3) viable for study at Beamline I12 compliment existing in-house pulsed X-ray capabilities and studies at the Dynamic Compression Sector. The authors gratefully acknowledge the ongoing support of Imperial College London, EPSRC, STFC and the Diamond Light Source, and AWE Plc.

  6. Two-dimensional in situ metrology of X-ray mirrors using the speckle scanning technique.

    PubMed

    Wang, Hongchang; Kashyap, Yogesh; Laundy, David; Sawhney, Kawal

    2015-07-01

    In situ metrology overcomes many of the limitations of existing metrology techniques and is capable of exceeding the performance of present-day optics. A novel technique for precisely characterizing an X-ray bimorph mirror and deducing its two-dimensional (2D) slope error map is presented. This technique has also been used to perform fast optimization of a bimorph mirror using the derived 2D piezo response functions. The measured focused beam size was significantly reduced after the optimization, and the slope error map was then verified by using geometrical optics to simulate the focused beam profile. This proposed technique is expected to be valuable for in situ metrology of X-ray mirrors at synchrotron radiation facilities and in astronomical telescopes. PMID:26134795

  7. Two-dimensional in situ metrology of X-ray mirrors using the speckle scanning technique.

    PubMed

    Wang, Hongchang; Kashyap, Yogesh; Laundy, David; Sawhney, Kawal

    2015-07-01

    In situ metrology overcomes many of the limitations of existing metrology techniques and is capable of exceeding the performance of present-day optics. A novel technique for precisely characterizing an X-ray bimorph mirror and deducing its two-dimensional (2D) slope error map is presented. This technique has also been used to perform fast optimization of a bimorph mirror using the derived 2D piezo response functions. The measured focused beam size was significantly reduced after the optimization, and the slope error map was then verified by using geometrical optics to simulate the focused beam profile. This proposed technique is expected to be valuable for in situ metrology of X-ray mirrors at synchrotron radiation facilities and in astronomical telescopes.

  8. Synchrotron-based X-ray computed tomography during compression loading of cellular materials

    DOE PAGES

    Cordes, Nikolaus L.; Henderson, Kevin; Stannard, Tyler; Williams, Jason J.; Xiao, Xianghui; Robinson, Mathew W. C.; Schaedler, Tobias A.; Chawla, Nikhilesh; Patterson, Brian M.

    2015-04-29

    Three-dimensional X-ray computed tomography (CT) of in situ dynamic processes provides internal snapshot images as a function of time. Tomograms are mathematically reconstructed from a series of radiographs taken in rapid succession as the specimen is rotated in small angular increments. In addition to spatial resolution, temporal resolution is important. Thus temporal resolution indicates how close together in time two distinct tomograms can be acquired. Tomograms taken in rapid succession allow detailed analyses of internal processes that cannot be obtained by other means. This article describes the state-of-the-art for such measurements acquired using synchrotron radiation as the X-ray source.

  9. Synchrotron-based X-ray computed tomography during compression loading of cellular materials

    SciTech Connect

    Cordes, Nikolaus L.; Henderson, Kevin; Stannard, Tyler; Williams, Jason J.; Xiao, Xianghui; Robinson, Mathew W. C.; Schaedler, Tobias A.; Chawla, Nikhilesh; Patterson, Brian M.

    2015-04-29

    Three-dimensional X-ray computed tomography (CT) of in situ dynamic processes provides internal snapshot images as a function of time. Tomograms are mathematically reconstructed from a series of radiographs taken in rapid succession as the specimen is rotated in small angular increments. In addition to spatial resolution, temporal resolution is important. Thus temporal resolution indicates how close together in time two distinct tomograms can be acquired. Tomograms taken in rapid succession allow detailed analyses of internal processes that cannot be obtained by other means. This article describes the state-of-the-art for such measurements acquired using synchrotron radiation as the X-ray source.

  10. The recent development of an X-ray grating interferometer at Shanghai Synchrotron Radiation Facility

    SciTech Connect

    Sun Haohua; Kou Bingquan; Xi Yan; Qi Juncheng; Sun Jianqi; Mohr, Juergen; Boerner, Martin; Zhao Jun; Xu, Lisa X.; Xiao Tiqiao; Wang Yujie

    2012-07-31

    An X-ray grating interferometer has been installed at Shanghai Synchrotron Radiation Facility (SSRF). Three sets of phase gratings were designed to cover the wide X-ray energy range needed for biological and soft material imaging capabilities. The performance of the grating interferometer has been evaluated by a tomography study of a PMMA particle packing and a new born mouse chest. In the mouse chest study, the carotid artery and carotid vein inside the mouse can be identified in situ without contrast agents.

  11. Anomalous lattice expansion in yttria stabilized zirconia under simultaneous applied electric and thermal fields: A time-resolved in situ energy dispersive x-ray diffractometry study with an ultrahigh energy synchrotron probe

    SciTech Connect

    Akdogan, E. K.; Savkl Latin-Small-Letter-Dotless-I y Latin-Small-Letter-Dotless-I ld Latin-Small-Letter-Dotless-I z, I.; Bicer, H.; Paxton, W.; Toksoy, F.; Tsakalakos, T.; Zhong, Z.

    2013-06-21

    Nonisothermal densification in 8% yttria doped zirconia (8YSZ) particulate matter of 250 nm median particle size was studied under 215 V/cm dc electric field and 9 Degree-Sign C/min heating rate, using time-resolved in-situ high temperature energy dispersive x-ray diffractometry with a polychromatic 200 keV synchrotron probe. Densification occurred in the 876-905 Degree-Sign C range, which resulted in 97% of the theoretical density. No local melting at particle-particle contacts was observed in scanning electron micrographs, implying densification was due to solid state mass transport processes. The maximum current draw at 905 Degree-Sign C was 3 A, corresponding to instantaneous absorbed power density of 570 W/cm{sup 3}. Densification of 8YSZ was accompanied by anomalous elastic volume expansions of the unit cell by 0.45% and 2.80% at 847 Degree-Sign C and 905 Degree-Sign C, respectively. The anomalous expansion at 905 Degree-Sign C at which maximum densification was observed is characterized by three stages: (I) linear stage, (II) anomalous stage, and (III) anelastic recovery stage. The densification in stage I (184 s) and II (15 s) was completed in 199 s, while anelastic relaxation in stage III lasted 130 s. The residual strains ({epsilon}) at room temperature, as computed from tetragonal (112) and (211) reflections, are {epsilon}{sub (112)} = 0.05% and {epsilon}{sub (211)} = 0.13%, respectively. Time dependence of (211) and (112) peak widths ({beta}) show a decrease with both exhibiting a singularity at 905 Degree-Sign C. An anisotropy in (112) and (211) peak widths of {l_brace} {beta}{sub (112)}/{beta}{sub (211)}{r_brace} = (3:1) magnitude was observed. No phase transformation occurred at 905 Degree-Sign C as verified from diffraction spectra on both sides of the singularity, i.e., the unit cell symmetry remains tetragonal. We attribute the reduction in densification temperature and time to ultrafast ambipolar diffusion of species arising from the

  12. X-ray microscopy using collimated and focussed synchrotron radiation

    SciTech Connect

    Jones, K.W.; Kwiatek, W.M.; Gordon, B.M.; Hanson, A.L.; Pounds, J.G.; Rivers, M.L.; Sutton, S.R.; Thompson, A.C.; Underwood, J.H.; Giauque, R.D.

    1987-01-01

    X-ray microscopy is a field that has developed rapidly in recent years. Two different approaches have been used. Zone plates have been employed to produce focused beams with sizes as low as 0.07 ..mu..m for x-ray energies below 1 keV. Images of biological materials and elemental maps for major and minor low Z have been produced using above and below absorption edge differences. At higher energies collimators and focusing mirrors have been used to make small diameter beams for excitation of characteristic K- or L-x rays of all elements in the periodic table. The practicality of a single instrument combining all the features of these two approaches is unclear. The use of high-energy x rays for x-ray microscopy has intrinsic value for characterization of thick samples and determination of trace amounts of most elements. A summary of work done on the X-26 beam line at the National Synchrotron Light Source (NSLS) with collimated and focused x rays with energies above 4 keV is given here. 6 refs., 5 figs., 1 tab.

  13. Rapid combinatorial screening by synchrotron X-ray imaging

    NASA Astrophysics Data System (ADS)

    Eba, Hiromi; Sakurai, Kenji

    2006-01-01

    An X-ray imaging system, which does not require any scans of the sample or an X-ray beam and which, therefore, dramatically reduces the amount of time required, was employed to evaluate combinatorial libraries efficiently. Two-dimensional X-ray fluorescence (XRF) images of an 8 mm × 8 mm area were observed for combinatorial substrates of manganese-cobalt spinel MnCo 2O 4 and lithium ferrite LiFeO 2 via an exposure time of 1-3 s using synchrotron X-rays. Thus, XRF signals from a whole substrate could be observed at once in a short space of time. In order to observe the chemical environment simultaneously for all materials arranged on the substrate, the fluorescent X-ray absorption fine structure (XAFS) was measured by repeating the imaging during the monochromator scans across the absorption edge for metals. This is extremely efficient because XAFS spectra for all materials placed on the common substrate are obtained from only a single energy scan. One can determine the valence numbers, as well as other aspects of the chemical environment of the metal included in each material, from the differences in spectral features and the energy shifts. Hence, combinatorial libraries can be screened very rapidly, and therefore efficiently, using the X-ray imaging system.

  14. 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.

  15. Synchrotron radiation X-ray imaging of cavitation bubbles in Al-Cu alloy melt.

    PubMed

    Huang, Haijun; Shu, Da; Fu, Yanan; Wang, Jun; Sun, Baode

    2014-07-01

    Cavitation bubbles in Al-10 wt.%Cu melt has been investigated by adopting synchrotron radiation X-ray imaging technology. In-situ observation reveals that most of bubbles concentrate within an intense cavitation zone nearby the radiation face. The measured near-maximum bubble radii obey a similar truncated Gaussian distribution as in water but increase by nearly the magnitude of one order due to higher ultrasonic intensity applied in aluminum melt.

  16. In situ surface/interface x-ray diffractometer for oxide molecular beam epitaxy

    SciTech Connect

    Lee, J. H.; Tung, I. C.; Chang, S. -H.; Bhattacharya, A.; Fong, D. D.; Freeland, J. W.; Hong, Hawoong

    2016-01-01

    In situ studies of oxide molecular beam epitaxy by synchrotron x-ray scattering has been made possible by upgrading an existing UHV/molecular beam epitaxy (MBE) six-circle diffractometer system. For oxide MBE growth, pure ozone delivery to the chamber has been made available, and several new deposition sources have been made available on a new 12 in. CF (ConFlat, a registered trademark of Varian, Inc.) flange. X-ray diffraction has been used as a major probe for film growth and structures for the system. In the original design, electron diffraction was intended for the secondary diagnostics available without the necessity of the x-ray and located at separate positions. Deposition of films was made possible at the two diagnostic positions. And, the aiming of the evaporation sources is fixed to the point between two locations. Ozone can be supplied through two separate nozzles for each location. Also two separate thickness monitors are installed. Additional features of the equipment are also presented together with the data taken during typical oxide film growth to illustrate the depth of information available via in situ x-ray techniques.

  17. In situ surface/interface x-ray diffractometer for oxide molecular beam epitaxy.

    PubMed

    Lee, J H; Tung, I C; Chang, S-H; Bhattacharya, A; Fong, D D; Freeland, J W; Hong, Hawoong

    2016-01-01

    In situ studies of oxide molecular beam epitaxy by synchrotron x-ray scattering has been made possible by upgrading an existing UHV/molecular beam epitaxy (MBE) six-circle diffractometer system. For oxide MBE growth, pure ozone delivery to the chamber has been made available, and several new deposition sources have been made available on a new 12 in. CF (ConFlat, a registered trademark of Varian, Inc.) flange. X-ray diffraction has been used as a major probe for film growth and structures for the system. In the original design, electron diffraction was intended for the secondary diagnostics available without the necessity of the x-ray and located at separate positions. Deposition of films was made possible at the two diagnostic positions. And, the aiming of the evaporation sources is fixed to the point between two locations. Ozone can be supplied through two separate nozzles for each location. Also two separate thickness monitors are installed. Additional features of the equipment are also presented together with the data taken during typical oxide film growth to illustrate the depth of information available via in situ x-ray techniques.

  18. Synchrotron x-ray reflectivity study of oxidation/passivation of copper and silicon.

    SciTech Connect

    Chu, Y.; Nagy, Z.; Parkhutik, V.; You, H.

    1999-07-21

    Synchrotron x-ray-scattering technique studies of copper and silicon electrochemical interfaces are reported. These two examples illustrate the application of synchrotron x-ray techniques for oxidation, passivation, and dissolution of metals and semiconductors.

  19. Application of X-ray synchrotron microscopy instrumentation in biology

    SciTech Connect

    Gasperini, F. M.; Pereira, G. R.; Granjeiro, J. M.; Calasans-Maia, M. D.; Rossi, A. M.; Perez, C. A.; Lopes, R. T.; Lima, I.

    2011-07-01

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

  20. Calcified-tissue investigations using synchrotron x-ray microscopy

    SciTech Connect

    Jones, K.W.; Spanne, P.; Schidlovsky, G.; Dejun, X. ); Bockman, R.S. . Medical Coll.); Rabinowitz, M.B. ); Hammond, P.B.; Bornschein, R.L. ); Hoeltzel, D.A. )

    1990-10-01

    Synchrotron x-ray microscopy (SXRM) in both emission and absorption modes has been used to examine elemental distributions in specimens of rat tibia, human deciduous teeth, and an orthopedic implant phantom. The work was performed with a spatial resolution of 8 {mu}m for the emission work and 25 {mu}m for the absorption work. The results illustrate the usefulness of SXRM for measurements of different types of calcified tissue. 3 figs.

  1. In situ x-ray photoelectron spectroscopy for electrochemical reactions in ordinary solvents

    SciTech Connect

    Masuda, Takuya; Yoshikawa, Hideki; Kobata, Masaaki; Kobayashi, Keisuke; Noguchi, Hidenori; Kawasaki, Tadahiro; Uosaki, Kohei

    2013-09-09

    In situ electrochemical X-ray photoelectron spectroscopy (XPS) apparatus, which allows XPS at solid/liquid interfaces under potential control, was constructed utilizing a microcell with an ultra-thin Si membrane, which separates vacuum and a solution. Hard X-rays from a synchrotron source penetrate into the Si membrane surface exposed to the solution. Electrons emitted at the Si/solution interface can pass through the membrane and be analyzed by an analyzer placed in vacuum. Its operation was demonstrated for potential-induced Si oxide growth in water. Effect of potential and time on the thickness of Si and Si oxide layers was quantitatively determined at sub-nanometer resolution.

  2. Synchrotron X-ray Enhanced Scanning Tunneling Microscopy

    NASA Astrophysics Data System (ADS)

    Rose, Volker; Freeland, John

    2011-03-01

    Proper understanding of complex phenomena occurring in nanostructures requires tools with both the ability to resolve the nanometer scale as well as provide detailed information about chemical, electronic, and magnetic structure. Scanning tunneling microscopy (STM) achieves the requisite high spatial resolution; however, direct elemental determination is not easily accomplished. X-ray microscopies, on the other hand, provide elemental selectivity, but currently have spatial resolution only of tens of nanometers. We present a novel and radically different concept that employs detection of local synchrotron x-ray interactions utilizing a STM that provides spatial resolution, and x-ray absorption directly yields chemical, electronic, and magnetic sensitivity. If during tunneling the sample is simultaneously illuminated with monochromatic x-rays, characteristic absorption will arise. Electrons that are excited into unoccupied levels close to the Fermi level modulate the tunneling current giving rise to elemental contrast. This work was supported by the U. S. Department of Energy, Office of Science, Office of Basic Energy Sciences, under contract DE-AC02-06CH11357.

  3. X-ray diffraction microtomography using synchrotron radiation

    NASA Astrophysics Data System (ADS)

    Barroso, R. C.; Lopes, R. T.; de Jesus, E. F. O.; Oliveira, L. F.

    2001-09-01

    The X-ray diffraction computed tomography technique is based on the interference phenomena of the coherent scatter. For low-momentum transfer, it is most probable that the scattering interaction will be coherent. A selective discrimination of a given element in a scanned specimen can be realized by fixing the Bragg angle which produces an interference peak and then, to carry out the computed tomography in the standard mode. The image reconstructed exalts the presence of this element with respect to other ones in a sample. This work reports the feasibility of a non-destructive synchrotron radiation X-ray diffraction imaging technique. This research was performed at the X-ray Diffraction beam line of the National Synchrotron Light Laboratory (LNLS) in Brazil. The coherent scattering properties of different tissue and bone substitute materials were evaluated. Furthermore, diffraction patterns of some polycrystalline solids were studied due to industrial and environmental human exposure to these metals. The obtained diffraction patterns form the basis of a selective tomography technique. Preliminary images are presented.

  4. In-situ synchrotron energy-dispersive x-ray diffraction study of thin Pd foils with Pd:D and Pd:H concentrations up to 1:1

    SciTech Connect

    Knies, D. L.; Grabowski, K. S.; Dominguez, D. D.; Qadri, S. B.; Hubler, G. K.; Violante, V.; Hu, J. Z.; He, J. H.

    2012-10-15

    Time resolved, in-situ, energy dispersive x-ray diffraction was performed in an electrolysis cell during electrochemical loading of palladium foil cathodes with hydrogen and deuterium. Concentrations of H:Pd (D:Pd) up to 1:1 in 0.1 M LiOH (LiOD) in H{sub 2}O (D{sub 2}O) electrolyte were obtained, as determined by both the Pd lattice parameter and cathode resistivity. In addition, some indications on the kinetics of loading and deloading of hydrogen from the Pd surface were obtained. The alpha-beta phase transformations were clearly delineated but no new phases at high concentration were determined.

  5. Synchrotron X-ray Microbeam Diffraction from Abalone Shell

    NASA Astrophysics Data System (ADS)

    Dimasi, Elaine; Sarikaya, Mehmet

    2004-03-01

    Microstructured biomaterials such as mollusk shells receive much attention, due to the promise that advanced materials can be designed and synthesized with biomimetic techniques that take advantage of self-assembly and aqueous, ambient processing conditions. A satisfactory understanding of this process requires characterization of the microstructure at the growth fronts where control over crystal orientation and morphology is enacted. We present synchrotron x-ray microbeam observations near the nacre-prismatic interface of red abalone shell (Haliotis rufescens). The relative orientations of calcite and aragonite grains exhibit differences from the idealizations reported previously. Long calcite grains impinge the boundary at 45^rc angles, suggestive of nucleation on (104) planes followed by c-axis growth. Within 100 μm of the boundary, crystals lose their bulk orientational order. The calcite crystal mosaic measured by x-ray diffraction rocking curves is resolution limited, comparable to geological calcite.

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

    PubMed

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

    2013-03-01

    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

  7. 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

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

    SciTech Connect

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

    2013-03-15

    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 Degree-Sign 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.

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

    PubMed

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

    2013-03-01

    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.

  10. Fabrication of X-ray mirrors for synchrotron applications

    NASA Astrophysics Data System (ADS)

    Thiess, H.; Lasser, H.; Siewert, F.

    2010-05-01

    Application of conic section geometries play an important role for soft X-ray synchrotron beams. Mirror design for collimation or focusing under stringent boundary conditions may end up with very aspheric geometries. In particular, the aspheric departure of these surfaces from "base geometries" in combination with high-quality requirements for slope and roughness is challenging. Mirror manufacturing of very aspheric mirrors at Carl Zeiss Laser Optics will be illustrated by recent examples. Fabrication issues of ellipsoids and 2D-parabolas are discussed. In addition, the close interaction of metrology and polishing will be highlighted.

  11. X-ray microscopy for in situ characterization of 3D nanostructural evolution in the laboratory

    NASA Astrophysics Data System (ADS)

    Hornberger, Benjamin; Bale, Hrishikesh; Merkle, Arno; Feser, Michael; Harris, William; Etchin, Sergey; Leibowitz, Marty; Qiu, Wei; Tkachuk, Andrei; Gu, Allen; Bradley, Robert S.; Lu, Xuekun; Withers, Philip J.; Clarke, Amy; Henderson, Kevin; Cordes, Nikolaus; Patterson, Brian M.

    2015-09-01

    X-ray microscopy (XRM) has emerged as a powerful technique that reveals 3D images and quantitative information of interior structures. XRM executed both in the laboratory and at the synchrotron have demonstrated critical analysis and materials characterization on meso-, micro-, and nanoscales, with spatial resolution down to 50 nm in laboratory systems. The non-destructive nature of X-rays has made the technique widely appealing, with potential for "4D" characterization, delivering 3D micro- and nanostructural information on the same sample as a function of sequential processing or experimental conditions. Understanding volumetric and nanostructural changes, such as solid deformation, pore evolution, and crack propagation are fundamental to understanding how materials form, deform, and perform. We will present recent instrumentation developments in laboratory based XRM including a novel in situ nanomechanical testing stage. These developments bridge the gap between existing in situ stages for micro scale XRM, and SEM/TEM techniques that offer nanometer resolution but are limited to analysis of surfaces or extremely thin samples whose behavior is strongly influenced by surface effects. Several applications will be presented including 3D-characterization and in situ mechanical testing of polymers, metal alloys, composites and biomaterials. They span multiple length scales from the micro- to the nanoscale and different mechanical testing modes such as compression, indentation and tension.

  12. Synchrotron Area X-ray Detectors, Present and Future

    SciTech Connect

    Gruner, Sol M.

    2010-06-23

    X-ray experiments are very frequently detector limited at today's storage ring synchrotron radiation (SR) sources, and will be even more so at future Energy Recovery Linac and X-ray Free Electron Laser sources. Image plate and phosphor-coupled CCD detectors that predominate at present-day sources were outgrowths of technologies initially developed for the medical and astronomical communities, respectively, with resultant limitations for SR. These limitations are enumerated. The growth of commercial silicon foundries and design tools enabling the production of large, customized integrated circuits is beginning to have a profound impact on SR detectors and is ushering in the age of 'designer detectors'. Novel area Pixel Array Detectors (PADs) are starting to appear in which each pixel has dedicated, complex circuitry capable of high speed and, in some cases, significant data processing power for specific applications. PADs now at, or near the horizon will be described. Integrated circuit methods continue to develop at a rapid pace. Implications for future x-ray detectors will be discussed.

  13. Synchrotron X-ray measurement techniques for thermal barrier coated cylindrical samples under thermal gradients

    SciTech Connect

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

    2013-08-15

    Measurement techniques to obtain accurate in situ synchrotron strain measurements of thermal barrier coating systems (TBCs) applied to hollow cylindrical specimens are presented in this work. The Electron Beam Physical Vapor Deposition coated specimens with internal cooling were designed to achieve realistic temperature gradients over the TBC coated material such as that occurring in the turbine blades of aeroengines. Effects of the circular cross section on the x-ray diffraction (XRD) measurements in the various layers, including the thermally grown oxide, are investigated using high-energy synchrotron x-rays. Multiple approaches for beam penetration including collection, tangential, and normal to the layers, along with variations in collection parameters are compared for their ability to attain high-resolution XRD data from the internal layers. This study displays the ability to monitor in situ, the response of the internal layers within the TBC, while implementing a thermal gradient across the thickness of the coated sample. The thermal setup maintained coating surface temperatures in the range of operating conditions, while monitoring the substrate cooling, for a controlled thermal gradient. Through variation in measurement location and beam parameters, sufficient intensities are obtained from the internal layers which can be used for depth resolved strain measurements. Results are used to establish the various techniques for obtaining XRD measurements through multi-layered coating systems and their outcomes will pave the way towards goals in achieving realistic in situ testing of these coatings.

  14. Synchrotron X-ray measurement techniques for thermal barrier coated cylindrical samples under thermal gradients

    NASA Astrophysics Data System (ADS)

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

    2013-08-01

    Measurement techniques to obtain accurate in situ synchrotron strain measurements of thermal barrier coating systems (TBCs) applied to hollow cylindrical specimens are presented in this work. The Electron Beam Physical Vapor Deposition coated specimens with internal cooling were designed to achieve realistic temperature gradients over the TBC coated material such as that occurring in the turbine blades of aeroengines. Effects of the circular cross section on the x-ray diffraction (XRD) measurements in the various layers, including the thermally grown oxide, are investigated using high-energy synchrotron x-rays. Multiple approaches for beam penetration including collection, tangential, and normal to the layers, along with variations in collection parameters are compared for their ability to attain high-resolution XRD data from the internal layers. This study displays the ability to monitor in situ, the response of the internal layers within the TBC, while implementing a thermal gradient across the thickness of the coated sample. The thermal setup maintained coating surface temperatures in the range of operating conditions, while monitoring the substrate cooling, for a controlled thermal gradient. Through variation in measurement location and beam parameters, sufficient intensities are obtained from the internal layers which can be used for depth resolved strain measurements. Results are used to establish the various techniques for obtaining XRD measurements through multi-layered coating systems and their outcomes will pave the way towards goals in achieving realistic in situ testing of these coatings.

  15. Synchrotron X-ray measurement techniques for thermal barrier coated cylindrical samples under thermal gradients.

    PubMed

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

    2013-08-01

    Measurement techniques to obtain accurate in situ synchrotron strain measurements of thermal barrier coating systems (TBCs) applied to hollow cylindrical specimens are presented in this work. The Electron Beam Physical Vapor Deposition coated specimens with internal cooling were designed to achieve realistic temperature gradients over the TBC coated material such as that occurring in the turbine blades of aeroengines. Effects of the circular cross section on the x-ray diffraction (XRD) measurements in the various layers, including the thermally grown oxide, are investigated using high-energy synchrotron x-rays. Multiple approaches for beam penetration including collection, tangential, and normal to the layers, along with variations in collection parameters are compared for their ability to attain high-resolution XRD data from the internal layers. This study displays the ability to monitor in situ, the response of the internal layers within the TBC, while implementing a thermal gradient across the thickness of the coated sample. The thermal setup maintained coating surface temperatures in the range of operating conditions, while monitoring the substrate cooling, for a controlled thermal gradient. Through variation in measurement location and beam parameters, sufficient intensities are obtained from the internal layers which can be used for depth resolved strain measurements. Results are used to establish the various techniques for obtaining XRD measurements through multi-layered coating systems and their outcomes will pave the way towards goals in achieving realistic in situ testing of these coatings. PMID:24007076

  16. Unraveling the Hydrogenation of TiO 2 and Graphene Oxide/TiO 2 Composites in Real Time by in Situ Synchrotron X-ray Powder Diffraction and Pair Distribution Function Analysis

    DOE PAGES

    Nguyen-Phan, Thuy-Duong; Liu, Zongyuan; Luo, Si; Gamalski, Andrew D.; Vovchok, Dimitry; Xu, Wenqian; Stach, Eric A.; Polyansky, Dmitry E.; Fujita, Etsuko; Rodriguez, José A.; et al

    2016-02-18

    The functionalization of graphene oxide (GO) and graphene by TiO2 and other metal oxides has attracted considerable attention due to numerous promising applications in catalysis, energy conversion, and storage. We propose hydrogenation of this class of materials as a promising way to tune catalytic properties by altering the structural and chemical transformations that occur upon H incorporation. We also investigate the structural changes that occur during the hydrogenation process using in situ powder X-ray diffraction and pair distribution function analysis of GO–TiO2 and TiO2 under H2 reduction. Sequential Rietveld refinement was employed to gain insight into the evolution of crystalmore » growth of TiO2 nanoparticles in the presence of two-dimensional (2D) GO nanosheets. GO sheets not only significantly retarded the nucleation and growth of rutile impurities, stabilizing the anatase structure, but was also partially reduced to hydrogenated graphene by the introduction of atomic hydrogen into the honeycomb lattice. We discuss the hydrogenation processes and the resulting composite structure that occurs during the incorporation of atomic H and the dynamic structural transformations that leads to a highly active photocatalyst.« less

  17. Elemental characterisation of melanin in feathers via synchrotron X-ray imaging and absorption spectroscopy

    NASA Astrophysics Data System (ADS)

    Edwards, Nicholas P.; van Veelen, Arjen; Anné, Jennifer; Manning, Phillip L.; Bergmann, Uwe; Sellers, William I.; Egerton, Victoria M.; Sokaras, Dimosthenis; Alonso-Mori, Roberto; Wakamatsu, Kazumasa; Ito, Shosuke; Wogelius, Roy A.

    2016-09-01

    Melanin is a critical component of biological systems, but the exact chemistry of melanin is still imprecisely known. This is partly due to melanin’s complex heterogeneous nature and partly because many studies use synthetic analogues and/or pigments extracted from their natural biological setting, which may display important differences from endogenous pigments. Here we demonstrate how synchrotron X-ray analyses can non-destructively characterise the elements associated with melanin pigment in situ within extant feathers. Elemental imaging shows that the distributions of Ca, Cu and Zn are almost exclusively controlled by melanin pigment distribution. X-ray absorption spectroscopy demonstrates that the atomic coordination of zinc and sulfur is different within eumelanised regions compared to pheomelanised regions. This not only impacts our fundamental understanding of pigmentation in extant organisms but also provides a significant contribution to the evidence-based colour palette available for reconstructing the appearance of fossil organisms.

  18. Elemental characterisation of melanin in feathers via synchrotron X-ray imaging and absorption spectroscopy

    PubMed Central

    Edwards, Nicholas P.; van Veelen, Arjen; Anné, Jennifer; Manning, Phillip L.; Bergmann, Uwe; Sellers, William I.; Egerton, Victoria M.; Sokaras, Dimosthenis; Alonso-Mori, Roberto; Wakamatsu, Kazumasa; Ito, Shosuke; Wogelius, Roy A.

    2016-01-01

    Melanin is a critical component of biological systems, but the exact chemistry of melanin is still imprecisely known. This is partly due to melanin’s complex heterogeneous nature and partly because many studies use synthetic analogues and/or pigments extracted from their natural biological setting, which may display important differences from endogenous pigments. Here we demonstrate how synchrotron X-ray analyses can non-destructively characterise the elements associated with melanin pigment in situ within extant feathers. Elemental imaging shows that the distributions of Ca, Cu and Zn are almost exclusively controlled by melanin pigment distribution. X-ray absorption spectroscopy demonstrates that the atomic coordination of zinc and sulfur is different within eumelanised regions compared to pheomelanised regions. This not only impacts our fundamental understanding of pigmentation in extant organisms but also provides a significant contribution to the evidence-based colour palette available for reconstructing the appearance of fossil organisms. PMID:27658854

  19. In situ determination of the spinel-post-spinel transition in Fe3O4 at high pressure and temperature by synchrotron X-ray diffraction

    SciTech Connect

    Schollenbruch, K; Woodland, A B; Frost, D J; Wang, Y; Sanehira, T; Langenhorst, F

    2011-08-10

    The position of the spinel-post-spinel phase transition in Fe3O4 has been determined in pressure-temperature space by in situ measurements using a multi-anvil press combined with white synchrotron radiation. Pressure measurement using the equation of state for MgO permitted pressure changes to be monitored at high temperature. The phase boundary was determined by the first appearance of diffraction peaks of the high-pressure polymorph (h-Fe3O4) during pressure increase and the disappearance of these peaks on pressure decrease along several isotherms. We intersected the phase boundary over the temperature interval of 700-1400 ºC. The boundary is linear and nearly isobaric, with a slightly positive slope. Post-experiment investigation by TEM confirms that the reverse reaction from h-Fe 3O4 to magnetite during decompression leads to the formation of microtwins on the (311) plane in the newly formed magnetite. Observations made during the phase transition suggest that the transition has a pseudomartensitic character, explaining in part why magnetite persists at conditions well within the stability field of h-Fe3O4, even at high temperatures. This study emphasizes the utility of studying phase transitions in situ at simultaneously high temperatures and pressures since the reaction kinetics may not be favorable at room temperature.

  20. Electro-deposition of Cu studied with in situ electrochemical scanning transmission x-ray microscopy

    NASA Astrophysics Data System (ADS)

    Hitchcock, A. P.; Qin, Z.; Rosendahl, S. M.; Lee, V.; Reynolds, M.; Hosseinkhannazer, H.

    2016-01-01

    Soft X-ray scanning transmission X-ray microscopy (STXM) was used to investigate Cu deposition onto, and stripping from a Au surface. Cu 2p spectromicroscopy was used to analyze initial and final states (ex situ processing) and follow the processes in situ. The in situ experiments were carried out using a static electrochemical cell with an electrolyte layer thickness of ˜1 μm. A new apparatus for in situ electrochemical STXM is described.

  1. X-ray and synchrotron studies of porous silicon

    SciTech Connect

    Sivkov, V. N.; Lomov, A. A.; Vasil'ev, A. L.; Nekipelov, S. V.; Petrova, O. V.

    2013-08-15

    The results of comprehensive studies of layers of porous silicon of different conductivity types, grown by anodizing standard Si(111) substrates in an electrolyte based on fluoric acid and ethanol with the addition of 5% of iodine and kept in air for a long time, are discussed. Measurements are performed by scanning electron microscopy, high-resolution X-ray diffraction, and ultrasoft X-ray spectroscopy using synchrotron radiation. The structural parameters of the layers (thickness, strain, and porosity) and atomic and chemical composition of the porous-silicon surface are determined. It is found that an oxide layer 1.5-2.3-nm thick is formed on the surface of the silicon skeleton. The near-edge fine structure of the Si 2p absorption spectrum of this layer corresponds to the fine structure of the 2p spectrum of well coordinated SiO{sub 2}. In this case, the fine structure in the Si 2p-edge absorption region of the silicon skeleton is identical to that of the 2p absorption spectrum of crystalline silicon.

  2. Synchrotron energy-dispersive X-ray diffraction tomography

    NASA Astrophysics Data System (ADS)

    Hall, C.; Barnes, P.; Cockcroft, J. K.; Colston, S. L.; Häusermann, D.; Jacques, S. D. M.; Jupe, A. C.; Kunz, M.

    1998-04-01

    Energy-dispersive diffraction tomography using white-beam synchrotron X-rays with energies up to 140 keV yields images of the interior features of solid objects up to 50 mm thick. The volume sampled is determined by the geometry of the diffracting lozenge defined by the incident beam, the detector system collimation and the Bragg angle. Using conventional beam slits to form a highly collimated 50 μm × 50 μm incident beam and a 40 μm collimator aperture, we demonstrate on a PEEK phantom that a lateral resolution (transverse to the beam direction) of a few microns can be achieved. The resolution in the direction of the incident beam is necessarily poorer than this since the diffracting lozenge is elongated in this direction, with length increasing rapidly at small angles. There is no evidence of significant contamination of the diffracted intensity by the effects of multiple scattering from outside the primary lozenge.

  3. In meso in situ serial X-ray crystallography of soluble and membrane proteins

    PubMed Central

    Huang, Chia-Ying; Olieric, Vincent; Ma, Pikyee; Panepucci, Ezequiel; Diederichs, Kay; Wang, Meitian; Caffrey, Martin

    2015-01-01

    The lipid cubic phase (LCP) continues to grow in popularity as a medium in which to generate crystals of membrane (and soluble) proteins for high-resolution X-ray crystallographic structure determination. To date, the PDB includes 227 records attributed to the LCP or in meso method. Among the listings are some of the highest profile membrane proteins, including the β2-adrenoreceptor–Gs protein complex that figured in the award of the 2012 Nobel Prize in Chemistry to Lefkowitz and Kobilka. The most successful in meso protocol to date uses glass sandwich crystallization plates. Despite their many advantages, glass plates are challenging to harvest crystals from. However, performing in situ X-ray diffraction measurements with these plates is not practical. Here, an alternative approach is described that provides many of the advantages of glass plates and is compatible with high-throughput in situ measurements. The novel in meso in situ serial crystallography (IMISX) method introduced here has been demonstrated with AlgE and PepT (alginate and peptide transporters, respectively) as model integral membrane proteins and with lysozyme as a test soluble protein. Structures were solved by molecular replacement and by experimental phasing using bromine SAD and native sulfur SAD methods to resolutions ranging from 1.8 to 2.8 Å using single-digit microgram quantities of protein. That sulfur SAD phasing worked is testament to the exceptional quality of the IMISX diffraction data. The IMISX method is compatible with readily available, inexpensive materials and equipment, is simple to implement and is compatible with high-throughput in situ serial data collection at macromolecular crystallography synchrotron beamlines worldwide. Because of its simplicity and effectiveness, the IMISX approach is likely to supplant existing in meso crystallization protocols. It should prove particularly attractive in the area of ligand screening for drug discovery and development. PMID

  4. In meso in situ serial X-ray crystallography of soluble and membrane proteins.

    PubMed

    Huang, Chia Ying; Olieric, Vincent; Ma, Pikyee; Panepucci, Ezequiel; Diederichs, Kay; Wang, Meitian; Caffrey, Martin

    2015-06-01

    The lipid cubic phase (LCP) continues to grow in popularity as a medium in which to generate crystals of membrane (and soluble) proteins for high-resolution X-ray crystallographic structure determination. To date, the PDB includes 227 records attributed to the LCP or in meso method. Among the listings are some of the highest profile membrane proteins, including the β2-adrenoreceptor-Gs protein complex that figured in the award of the 2012 Nobel Prize in Chemistry to Lefkowitz and Kobilka. The most successful in meso protocol to date uses glass sandwich crystallization plates. Despite their many advantages, glass plates are challenging to harvest crystals from. However, performing in situ X-ray diffraction measurements with these plates is not practical. Here, an alternative approach is described that provides many of the advantages of glass plates and is compatible with high-throughput in situ measurements. The novel in meso in situ serial crystallography (IMISX) method introduced here has been demonstrated with AlgE and PepT (alginate and peptide transporters, respectively) as model integral membrane proteins and with lysozyme as a test soluble protein. Structures were solved by molecular replacement and by experimental phasing using bromine SAD and native sulfur SAD methods to resolutions ranging from 1.8 to 2.8 Å using single-digit microgram quantities of protein. That sulfur SAD phasing worked is testament to the exceptional quality of the IMISX diffraction data. The IMISX method is compatible with readily available, inexpensive materials and equipment, is simple to implement and is compatible with high-throughput in situ serial data collection at macromolecular crystallography synchrotron beamlines worldwide. Because of its simplicity and effectiveness, the IMISX approach is likely to supplant existing in meso crystallization protocols. It should prove particularly attractive in the area of ligand screening for drug discovery and development.

  5. Note: High-pressure in situ x-ray laminography using diamond anvil cell.

    PubMed

    Nomura, Ryuichi; Uesugi, Kentaro

    2016-04-01

    A high-pressure in situ X-ray laminography technique was developed using a newly designed, laterally open diamond anvil cell. A low X-ray beam of 8 keV energy was used, aiming at future application to dual energy X-ray chemical imaging techniques. The effects of the inclination angle and the imaging angle range were evaluated at ambient pressure using the apparatus. Sectional images of ruby ball samples were successfully reconstructed at high pressures, up to approximately 50 GPa. The high-pressure in situ X-ray laminography technique is expected to provide new insights into the deep Earth sciences. PMID:27131721

  6. Note: High-pressure in situ x-ray laminography using diamond anvil cell

    NASA Astrophysics Data System (ADS)

    Nomura, Ryuichi; Uesugi, Kentaro

    2016-04-01

    A high-pressure in situ X-ray laminography technique was developed using a newly designed, laterally open diamond anvil cell. A low X-ray beam of 8 keV energy was used, aiming at future application to dual energy X-ray chemical imaging techniques. The effects of the inclination angle and the imaging angle range were evaluated at ambient pressure using the apparatus. Sectional images of ruby ball samples were successfully reconstructed at high pressures, up to approximately 50 GPa. The high-pressure in situ X-ray laminography technique is expected to provide new insights into the deep Earth sciences.

  7. In situ analysis of foliar zinc absorption and short-distance movement in fresh and hydrated leaves of tomato and citrus using synchrotron-based X-ray fluorescence microscopy

    PubMed Central

    Du, Yumei; Kopittke, Peter M.; Noller, Barry N.; James, Simon A.; Harris, Hugh H.; Xu, Zhi Ping; Li, Peng; Mulligan, David R.; Huang, Longbin

    2015-01-01

    Background and Aims Globally, zinc deficiency is one of the most important nutritional factors limiting crop yield and quality. Despite widespread use of foliar-applied zinc fertilizers, much remains unknown regarding the movement of zinc from the foliar surface into the vascular structure for translocation into other tissues and the key factors affecting this diffusion. Methods Using synchrotron-based X-ray fluorescence microscopy (µ-XRF), absorption of foliar-applied zinc nitrate or zinc hydroxide nitrate was examined in fresh leaves of tomato (Solanum lycopersicum) and citrus (Citrus reticulatus). Key Results The foliar absorption of zinc increased concentrations in the underlying tissues by up to 600-fold in tomato but only up to 5-fold in citrus. The magnitude of this absorption was influenced by the form of zinc applied, the zinc status of the treated leaf and the leaf surface to which it was applied (abaxial or adaxial). Once the zinc had moved through the leaf surface it appeared to bind strongly, with limited further redistribution. Regardless of this, in these underlying tissues zinc moved into the lower-order veins, with concentrations 2- to 10-fold higher than in the adjacent tissues. However, even once in higher-order veins, the movement of zinc was still comparatively limited, with concentrations decreasing to levels similar to the background within 1–10 mm. Conclusions The results advance our understanding of the factors that influence the efficacy of foliar zinc fertilizers and demonstrate the merits of an innovative methodology for studying foliar zinc translocation mechanisms. PMID:25399024

  8. In meso in situ serial X-ray crystallography of soluble and membrane proteins

    SciTech Connect

    Huang, Chia-Ying; Olieric, Vincent; Ma, Pikyee; Panepucci, Ezequiel; Diederichs, Kay; Wang, Meitian; Caffrey, Martin

    2015-05-14

    A method for performing high-throughput in situ serial X-ray crystallography with soluble and membrane proteins in the lipid cubic phase is described. It works with microgram quantities of protein and lipid (and ligand when present) and is compatible with the most demanding sulfur SAD phasing. The lipid cubic phase (LCP) continues to grow in popularity as a medium in which to generate crystals of membrane (and soluble) proteins for high-resolution X-ray crystallographic structure determination. To date, the PDB includes 227 records attributed to the LCP or in meso method. Among the listings are some of the highest profile membrane proteins, including the β{sub 2}-adrenoreceptor–G{sub s} protein complex that figured in the award of the 2012 Nobel Prize in Chemistry to Lefkowitz and Kobilka. The most successful in meso protocol to date uses glass sandwich crystallization plates. Despite their many advantages, glass plates are challenging to harvest crystals from. However, performing in situ X-ray diffraction measurements with these plates is not practical. Here, an alternative approach is described that provides many of the advantages of glass plates and is compatible with high-throughput in situ measurements. The novel in meso in situ serial crystallography (IMISX) method introduced here has been demonstrated with AlgE and PepT (alginate and peptide transporters, respectively) as model integral membrane proteins and with lysozyme as a test soluble protein. Structures were solved by molecular replacement and by experimental phasing using bromine SAD and native sulfur SAD methods to resolutions ranging from 1.8 to 2.8 Å using single-digit microgram quantities of protein. That sulfur SAD phasing worked is testament to the exceptional quality of the IMISX diffraction data. The IMISX method is compatible with readily available, inexpensive materials and equipment, is simple to implement and is compatible with high-throughput in situ serial data collection at

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

    NASA Astrophysics Data System (ADS)

    Koval'chuk, M. V.; Yatsishina, E. B.; Blagov, A. E.; Tereshchenko, E. Yu.; Prosekov, P. A.; Dyakova, Yu. A.

    2016-09-01

    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.

  10. Synchrotron x-ray sources and new opportunities in the soil and environmental sciences

    SciTech Connect

    Schulze, D. ); Anderson, S. ); Mattigod, S. )

    1990-07-01

    This report contains the following papers: characteristics of the advanced photon source and comparison with existing synchrotron facilities; x-ray absorption spectroscopy: EXAFS and XANES -- A versatile tool to study the atomic and electronic structure of materials; applications of x-ray spectroscopy and anomalous scattering experiments in the soil and environmental sciences; X-ray fluorescence microprobe and microtomography.

  11. High pressure x-ray diffraction techniques with synchrotron radiation

    NASA Astrophysics Data System (ADS)

    Jing, Liu

    2016-07-01

    This article summarizes the developments of experimental techniques for high pressure x-ray diffraction (XRD) in diamond anvil cells (DACs) using synchrotron radiation. Basic principles and experimental methods for various diffraction geometry are described, including powder diffraction, single crystal diffraction, radial diffraction, as well as coupling with laser heating system. Resolution in d-spacing of different diffraction modes is discussed. More recent progress, such as extended application of single crystal diffraction for measurements of multigrain and electron density distribution, time-resolved diffraction with dynamic DAC and development of modulated heating techniques are briefly introduced. The current status of the high pressure beamline at BSRF (Beijing Synchrotron Radiation Facility) and some results are also presented. Project supported by the National Natural Science Foundation of China (Grant Nos. 10875142, 11079040, and 11075175). The 4W2 beamline of BSRF was supported by the Chinese Academy of Sciences (Grant Nos. KJCX2-SW-N20, KJCX2-SW-N03, and SYGNS04).

  12. Extensional rheometer for in situ x-ray scattering study on flow-induced crystallization of polymer

    NASA Astrophysics Data System (ADS)

    Liu, Yanping; Zhou, Weiqing; Cui, Kunpeng; Tian, Nan; Wang, Xiao; Liu, Liangbao; Li, Liangbin; Zhou, Yingui

    2011-04-01

    We designed and constructed an extensional rheometer for in situ small and wide angle x-ray study on flow-induced crystallization of polymer. Two rotating drums with an axis distance of 20 mm are employed to impose extensional deformation on the samples. With a constant angular velocity, the two drums generate a constant Henkcy strain rate as sample length for testing keeps constant during deformation. An ionic liquid is used as heating medium to prevent polymer melt from bending downward due to gravity, which is excellent in terms of high thermal stability, low viscosity, and relative low adsorption on x-ray. Flow-induced crystallization experiments are conducted with this apparatus on x-ray scattering station in Shanghai Synchrotron Radiation Facility (SSRF), which allows us to collect rheological and structural data simultaneously and may lead to a better understanding on flow-induced crystallization of polymer.

  13. Synchrotron X-ray bio-imaging of natural and synthetic bone-graft materials in an aqueous environment

    NASA Astrophysics Data System (ADS)

    Kim, Yong-Gun; Bark, Chung Wung

    2014-11-01

    Bone-graft materials in dentistry have osteoinductive and osteoconductive abilities, which depend on their microstructural characteristics, such as their porosity, particle size, micro channels, and absorption. These characteristics have been observed using various imaging techniques, such as optical microscopy and scanning electron microscopy (SEM). However, most techniques cannot provide images in water, even though graft materials in vivo are invariably in contact with different water-based fluids. Synchrotron X-ray imaging allows sample microenvironments to be controlled as X-ray beams easily penetrate air and water. In this report, we used the synchrotron X-ray imaging technique to provide in-situ images of various bone-graft materials in aqueous environments. We observed internal microstructural images of bone-graft materials in real-time in 0.9% saline solution and interactions between bone-graft materials and saline, that is, hydration patterns and bone-graft expansion.

  14. Synchrotron X-ray scattering studies at mineral-water interfaces

    SciTech Connect

    Chiarello, R.P.; Sturchio, N.C.

    1995-03-01

    Synchrotron X-ray scattering techniques provide a powerful tool for the in situ study of atomic scale processes occurring at solid-liquid interfaces. We have applied these techniques to characterize and study reactions at mineral-water interfaces. Here we present two examples. The first is the characterization of the calcite (CaCO{sub 3}) (10{bar 1}4) cleavage surface, in equilibrium with deionized water, by crystal truncation rod measurements. The second is the in situ study of the heteroepitaxial growth of otavite (CdCO{sub 3}) on the calcite (10{bar 1}4) cleavage surface. The results of such studies will lead to significant progress in understanding mineral-water interface geochemistry.

  15. Time-resolved and in-situ X-ray scattering methods beyond photoactivation: Utilizing high-flux X-ray sources for the study of ubiquitous non-photoactive proteins.

    PubMed

    Jain, Rohit; Techert, Simone

    2016-01-01

    X-ray scattering technique, comprising of small-angle/wide-angle X-ray scattering (SAXS/WAXS) techniques is increasingly used to characterize the structure and interactions of biological macromolecules and their complexes in solution. It is a method of choice to characterize the flexible, partially folded and unfolded protein systems. X-ray scattering is the last resort for proteins that cannot be investigated by crystallography or NMR and acts as a complementary technique with different biophysical techniques to answer challenging scientific questions. The marriage of the X-ray scattering technique with the fourth dimension "time" yields structural dynamics and kinetics information for protein motions in hierarchical timescales from picoseconds to days. The arrival of the high-flux X-ray beam at third generation synchrotron sources, exceptional X-ray optics, state-of-the-art detectors, upgradation of X-ray scattering beamlines with microfluidics devices and advanced X-ray scattering data analysis procedures are the important reasons behind the shining years of X-ray scattering technique. The best days of the X-ray scattering technique are on the horizon with the advent of the nanofocus X-ray scattering beamlines and fourth generation X-ray lightsources, i.e., free electron lasers (XFELs). Complementary to the photon-triggered time-resolved X-ray scattering techniques, we will present an overview of the time-resolved and in-situ X-ray scattering techniques for structural dynamics of ubiquitous non-photoactive proteins.

  16. Time-resolved and in-situ X-ray scattering methods beyond photoactivation: Utilizing high-flux X-ray sources for the study of ubiquitous non-photoactive proteins.

    PubMed

    Jain, Rohit; Techert, Simone

    2016-01-01

    X-ray scattering technique, comprising of small-angle/wide-angle X-ray scattering (SAXS/WAXS) techniques is increasingly used to characterize the structure and interactions of biological macromolecules and their complexes in solution. It is a method of choice to characterize the flexible, partially folded and unfolded protein systems. X-ray scattering is the last resort for proteins that cannot be investigated by crystallography or NMR and acts as a complementary technique with different biophysical techniques to answer challenging scientific questions. The marriage of the X-ray scattering technique with the fourth dimension "time" yields structural dynamics and kinetics information for protein motions in hierarchical timescales from picoseconds to days. The arrival of the high-flux X-ray beam at third generation synchrotron sources, exceptional X-ray optics, state-of-the-art detectors, upgradation of X-ray scattering beamlines with microfluidics devices and advanced X-ray scattering data analysis procedures are the important reasons behind the shining years of X-ray scattering technique. The best days of the X-ray scattering technique are on the horizon with the advent of the nanofocus X-ray scattering beamlines and fourth generation X-ray lightsources, i.e., free electron lasers (XFELs). Complementary to the photon-triggered time-resolved X-ray scattering techniques, we will present an overview of the time-resolved and in-situ X-ray scattering techniques for structural dynamics of ubiquitous non-photoactive proteins. PMID:26732244

  17. Electrochemical in-situ reaction cell for X-ray scattering, diffraction and spectroscopy

    SciTech Connect

    Braun, Artur; Granlund, Eric; Cairns, Elton J.

    2003-01-27

    An electrochemical in-situ reaction cell for hard X-ray experiments with battery electrodes is described. Applications include the small angle scattering, diffraction, and near-edge spectroscopy of lithium manganese oxide electrodes.

  18. An in situ atomic force microscope for normal-incidence nanofocus X-ray experiments.

    PubMed

    Vitorino, M V; Fuchs, Y; Dane, T; Rodrigues, M S; Rosenthal, M; Panzarella, A; Bernard, P; Hignette, O; Dupuy, L; Burghammer, M; Costa, L

    2016-09-01

    A compact high-speed X-ray atomic force microscope has been developed for in situ use in normal-incidence X-ray experiments on synchrotron beamlines, allowing for simultaneous characterization of samples in direct space with nanometric lateral resolution while employing nanofocused X-ray beams. In the present work the instrument is used to observe radiation damage effects produced by an intense X-ray nanobeam on a semiconducting organic thin film. The formation of micrometric holes induced by the beam occurring on a timescale of seconds is characterized. PMID:27577764

  19. Quantifying the Nucleation and Growth Kinetics of Microwave Nanochemistry Enabled by in Situ High-Energy X-ray Scattering.

    PubMed

    Liu, Qi; Gao, Min-Rui; Liu, Yuzi; Okasinski, John S; Ren, Yang; Sun, Yugang

    2016-01-13

    The fast reaction kinetics presented in the microwave synthesis of colloidal silver nanoparticles was quantitatively studied, for the first time, by integrating a microwave reactor with in situ X-ray diffraction at a high-energy synchrotron beamline. Comprehensive data analysis reveals two different types of reaction kinetics corresponding to the nucleation and growth of the Ag nanoparticles. The formation of seeds (nucleation) follows typical first-order reaction kinetics with activation energy of 20.34 kJ/mol, while the growth of seeds (growth) follows typical self-catalytic reaction kinetics. Varying the synthesis conditions indicates that the microwave colloidal chemistry is independent of concentration of surfactant. These discoveries reveal that the microwave synthesis of Ag nanoparticles proceeds with reaction kinetics significantly different from the synthesis present in conventional oil bath heating. The in situ X-ray diffraction technique reported in this work is promising to enable further understanding of crystalline nanomaterials formed through microwave synthesis.

  20. K-Edge Subtraction Angiography with Synchrotron X-Rays

    SciTech Connect

    Giacomini, John C.

    1996-12-31

    The purpose of this project was to utilize dual energy, monochromatic X-rays produced from synchrotrons radiation in order to obtain noninvasive medical imaging. The application of synchrotrons radiation to medical imaging is based on the principle of iodine dichromography, first described by Bertil Jacobson of the Karolinska Institute in 1953. Medical imaging using synchrotrons radiation and K-edge dichromography was pioneered at Stanford University under the leadership of Dr. Ed Rubenstein, and the late Nobel Laureate in Physics, Dr. Robert Hofstadter. With progressive refinements in hardware, clinical-quality images were obtained of human coronary arteries utilizing peripheral injections of iodinated contrast agent. These images even now are far superior to those being presented by investigators using MRI as an imaging tool for coronary arteries. However, new supplies and instruments in the cardiac catheterization laboratory have served to transform coronary angiography into an outpatient procedure, with relatively little morbidity. We extended the principles learned with coronary angiography to noninvasive imaging of the human bronchial tree. For these images, we utilized xenon as the contrast agent, as it has a K-edge very similar to that of iodine. In this case, there is no true competing diagnostic test, and pulmonary neoplasm is an enormous public health concern. In early experiments, we demonstrated remarkably clear images of the human bronchial tree. These images have been shown internationally; however, funding difficulties primarily with the Department of Energy have not allowed for progression of this promising avenue of research. One potential criticism of the project is that in order to obtain these images, we utilized national laboratories. Some have questioned whether this would lead to a practical imaging modality. However, we have shown that the technology exists to allow for construction of a miniature storage ring, with a superconducting

  1. CT imaging of small animals using monochromatized synchrotron x rays

    SciTech Connect

    Dilmanian, F.A.; Rarback, H.; Nachaliel, E.; Rivers, M.; Thomlinson, W.C.; Chapman, L.D.; Oversluizen, T.; Slatkin, D.N.; Spanne, P.; Spector, S. ); Garrett, R.F. ); Luke, P.N.; Pehl, R.; Thompson, A.C. ); Appel, R.; Miller, M.H. (A

    1992-01-01

    Rats and chicken embryos were imaged in vivo with a prototype Multiple Energy Computed Tomography (MECT) system using monochromatized x rays from the X17 superconducting wiggler at the National Synchrotron Light Source. The CT configuration coated of a horizontal low-divergence, fan-shaped beam, 70 mm wide and 0.5 mm high, and a subject rotating about a vertical aids. A linear-array high-purity Ge detector with 140 elements, each 0.5 mm wide and 6 mm thick, was used with a data acquisition system that provides a linear response over almost six orders of magnitude of detector current. The dual photon absorptiometry (DPA) algorithm was applied to images of the rat head acquired at 20 and 45 keV to obtain two new images, one representing the low-Z, and the other the intermediate-Z clement group. The results indicate that the contrast resolution and the quantification accuracy of the images improve stepwise; first, with the monochromatic beam and, second, the DPA method. The system is a prototype for a brain scanner.

  2. Microbial biofilm study by synchrotron X-ray microscopy

    NASA Astrophysics Data System (ADS)

    Pennafirme, S.; Lima, I.; Bitencourt, J. A.; Crapez, M. A. C.; Lopes, R. T.

    2015-11-01

    Microbial biofilm has already being used to remove metals and other pollutants from wastewater. In this sense, our proposal was to isolate and cultivate bacteria consortia from mangrove's sediment resistant to Zn (II) and Cu (II) at 50 mg L-1 and to observe, through synchrotron X-ray fluorescence microscopy (microXRF), whether the biofilm sequestered the metal. The biofilm area analyzed was 1 mm2 and a 2D map was generated (pixel size 20×20 μm2, counting time 5 s/point). The biofilm formation and retention followed the sequence Zn>Cu. Bacterial consortium zinc resistant formed dense biofilm and retained 63.83% of zinc, while the bacterial consortium copper resistant retained 3.21% of copper, with lower biofilm formation. Dehydrogenase activity of Zn resistant bacterial consortium was not negatively affect by 50 mg ml-1 zinc input, whereas copper resistant bacterial consortium showed a significant decrease on dehydrogenase activity (50 mg mL-1 of Cu input). In conclusion, biofilm may protect bacterial cells, acting as barrier against metal toxicity. The bacterial consortia Zn resistant, composed by Nitratireductor spp. and Pseudomonas spp formed dense biofilm and sequestered metal from water, decreasing the metal bioavailability. These bacterial consortia can be used in bioreactors and in bioremediation programs.

  3. Synchrotron Radiation from Outer Space and the Chandra X-Ray Observatory

    NASA Technical Reports Server (NTRS)

    Weisskopf, M. C.

    2006-01-01

    The universe provides numerous extremely interesting astrophysical sources of synchrotron X radiation. The Chandra X-ray Observatory and other X-ray missions provide powerful probes of these and other cosmic X-ray sources. Chandra is the X-ray component of NASA's Great Observatory Program which also includes the Hubble Space telescope, the Spitzer Infrared Telescope Facility, and the now defunct Compton Gamma-Ray Observatory. The Chandra X-Ray Observatory provides the best angular resolution (sub-arcsecond) of any previous, current, or planned (for the foreseeable near future) space-based X-ray instrumentation. We present here a brief overview of the technical capability of this X-Ray observatory and some of the remarkable discoveries involving cosmic synchrotron sources.

  4. Oxidation Induced Doping of Nanoparticles Revealed by in Situ X-ray Absorption Studies.

    PubMed

    Kwon, Soon Gu; Chattopadhyay, Soma; Koo, Bonil; Dos Santos Claro, Paula Cecilia; Shibata, Tomohiro; Requejo, Félix G; Giovanetti, Lisandro J; Liu, Yuzi; Johnson, Christopher; Prakapenka, Vitali; Lee, Byeongdu; Shevchenko, Elena V

    2016-06-01

    Doping is a well-known approach to modulate the electronic and optical properties of nanoparticles (NPs). However, doping at nanoscale is still very challenging, and the reasons for that are not well understood. We studied the formation and doping process of iron and iron oxide NPs in real time by in situ synchrotron X-ray absorption spectroscopy. Our study revealed that the mass flow of the iron triggered by oxidation is responsible for the internalization of the dopant (molybdenum) adsorbed at the surface of the host iron NPs. The oxidation induced doping allows controlling the doping levels by varying the amount of dopant precursor. Our in situ studies also revealed that the dopant precursor substantially changes the reaction kinetics of formation of iron and iron oxide NPs. Thus, in the presence of dopant precursor we observed significantly faster decomposition rate of iron precursors and substantially higher stability of iron NPs against oxidation. The same doping mechanism and higher stability of host metal NPs against oxidation was observed for cobalt-based systems. Since the internalization of the adsorbed dopant at the surface of the host NPs is driven by the mass transport of the host, this mechanism can be potentially applied to introduce dopants into different oxidized forms of metal and metal alloy NPs providing the extra degree of compositional control in material design. PMID:27152970

  5. The X-ray Fluorescence Microscopy Beamline at the Australian Synchrotron

    SciTech Connect

    Paterson, D.; Jonge, M. D. de; Howard, D. L.; Lewis, W.; McKinlay, J.; Starritt, A.; Kusel, M.; Ryan, C. G.; Kirkham, R.; Moorhead, G.; Siddons, D. P.

    2011-09-09

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

  6. IN SITU SURFACE X-RAY SCATTERING STUDIES OF ELECTROSORPTION

    SciTech Connect

    WANG,J.X.; ADZIC,R.R.; OCKO,B.M.

    1998-07-01

    A short review of the application of surface x-ray scattering techniques to the electrode/electrolyte interfaces is presented. Recent results on metal, halide, and metal-halide adlayers with three specific systems: Bi on Au(100) and Au(110); Br on Au(100) and Ag(100); and the coadsorption of Tl with Br or I on Au(111), are given as an illustration. Factors affecting ordering of pure metal and halide adlayers and the metal-halide surface compounds are discussed in some detail.

  7. 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

    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.

  8. MeV per nucleon ion irradiation of nuclear materials with high energy synchrotron X-ray characterization

    NASA Astrophysics Data System (ADS)

    Pellin, M. J.; Yacout, Abdellatif M.; Mo, Kun; Almer, Jonathan; Bhattacharya, S.; Mohamed, Walid; Seidman, D.; Ye, Bei; Yun, D.; Xu, Ruqing; Zhu, Shaofei

    2016-04-01

    The combination of MeV/Nucleon ion irradiation (e.g. 133 MeV Xe) and high energy synchrotron x-ray characterization (e.g. at the Argonne Advanced Photon Source, APS) provides a powerful characterization method to understand radiation effects and to rapidly screen materials for the nuclear reactor environment. Ions in this energy range penetrate ∼10 μm into materials. Over this range, the physical interactions vary (electronic stopping, nuclear stopping and added interstitials). Spatially specific x-ray (and TEM and nanoindentation) analysis allow individual quantification of these various effects. Hard x-rays provide the penetration depth needed to analyze even nuclear fuels. Here, this combination of synchrotron x-ray and MeV/Nucleon ion irradiation is demonstrated on U-Mo fuels. A preliminary look at HT-9 steels is also presented. We suggest that a hard x-ray facility with in situ MeV/nucleon irradiation capability would substantially accelerate the rate of discovery for extreme materials.

  9. Hydride precipitation kinetics in Zircaloy-4 studied using synchrotron X-ray diffraction

    NASA Astrophysics Data System (ADS)

    Courty, Olivier F.; Motta, Arthur T.; Piotrowski, Christopher J.; Almer, Jonathan D.

    2015-06-01

    As a result of in-reactor corrosion during operation in nuclear reactors, hydrogen can enter the zirconium fuel cladding and precipitate as brittle hydride particles, which may reduce cladding ductility. Dissolved hydrogen responds to temperature gradients, resulting in transport and precipitation into cold spots so that the distribution of hydrides in the cladding is inhomogeneous. The hydrogen precipitation kinetics plays a strong role in the spatial distribution of the hydrides in the cladding. The precipitation rate is normally described as proportional to the supersaturation of hydrogen in solid solution. The proportionality constant, α2, for hydride precipitation in Zircaloy-4 is measured directly using in situ synchrotron X-Ray diffraction, at different temperatures and with three different initial hydrogen concentrations. The results validate the linear approximation of the phenomenological model and a near constant value of α2 = 4.5 × 10-4 s-1 was determined for the temperature range studied.

  10. Hydride precipitation kinetics in Zircaloy-4 studied using synchrotron X-ray diffraction

    SciTech Connect

    Courty, Olivier Fabrice; Motta, Arthur T.; Piotrowski, Christopher J.; Almer, Jonathan D.

    2015-01-01

    As a result of in-reactor corrosion during operation in nuclear reactors, hydrogen can enter the zirconium fuel cladding and precipitate as brittle hydride particles, which may reduce cladding ductility. Dissolved hydrogen responds to temperature gradients, resulting in transport and precipitation into cold spots so that the distribution of hydrides in the cladding is inhomogeneous. The hydrogen precipitation kinetics plays a strong role in the spatial distribution of the hydrides in the cladding. The precipitation rate is normally described as proportional to the supersaturation of hydrogen in solid solution. The proportionality constant, α2, for hydride precipitation in Zircaloy-4 is measured directly using in situ synchrotron X-Ray diffraction, at different temperatures and with three different initial hydrogen concentrations. The results validate the linear approximation of the phenomenological model and a near constant value of α2 = 4.5 × 10-4 s-1 was determined for the temperature range studied.

  11. Synchrotron X-Ray Microdiffraction Studies of Electromigration in Interconnect lines at the Advanced Light Source

    SciTech Connect

    Tamura, Nobumichi; Chen, Kai; Kunz, Martin

    2009-12-01

    Synchrotron polychromatic X-ray microdiffraction is a particularly suitable technique to study in situ the effect of electromigration in metal interconnects as add spatial resolution to grain orientation and strain sensitivity. This technique has been extensively used at the Advanced Light Source to monitor changes in aluminum and copper interconnect test structures while high-density current is passed into them during accelerated tests at elevated temperature. One of the principal findings is the observation of electromigration-induced plasticity in the metal lines that appear during the very early stages of electromigration. In some of the lines, high density of geometrically necessary dislocation are formed leading to additional diffusion paths causing an enhancement of electromigration effect at test temperature.

  12. Differentiation of Deformation Modes in Nanocrystalline Pd Films Inferred from Peak Asymmetry Evolution Using In Situ X-Ray Diffraction

    NASA Astrophysics Data System (ADS)

    Lohmiller, Jochen; Baumbusch, Rudolf; Kraft, Oliver; Gruber, Patric A.

    2013-02-01

    Synchrotron-based in situ tensile testing was used to study the dominant deformation mechanisms of nanocrystalline Pd thin films on a compliant substrate. An x-ray diffraction peak profile analysis reveals an (hkl) independent deformation induced peak asymmetry. It is argued that the asymmetry is caused by a broad distribution of elastic strains among individual grains and the complexity of accommodation processes. The reversal of peak asymmetry manifests the transition from heterogeneous microplasticity to dislocation-based macroplasticity. Independently, stress-driven grain boundary migration is active.

  13. X-ray photochemical alteration of planetary samples during in situ micro-XRF analysis

    NASA Astrophysics Data System (ADS)

    Flannery, D. T.; Tuite, M. L., Jr.; Hodyss, R. P.; Allwood, A.; Bhartia, R.; Abbey, W. J.; Williford, K. H.

    2015-12-01

    PIXL (Planetary Instrument for X-ray Lithochemistry; selected for the Mars 2020 mission contact science payload) uses a polycapillary to focus X-rays to a ~100 μm spot on sample surfaces, providing higher spatial resolution, higher X-ray flux, and higher fluorescence counts compared to previously flown planetary XRF instruments. Photochemical changes in organic materials occurring during investigations employing x-rays have been reported, particularly for biological samples examined in synchrotrons (e.g. George et al., J. Synchrotron Radiation, 19:875-876). However, little is known about the effect energies and fluxes typical to micro-XRF instruments may have on the organic molecules that are commonly preserved in rocks and sediments. In particular, it is essential to understand the effect of micro-XRF on organics preserved near surfaces that are later subjected to contact science that focuses on organic geochemistry (e.g. UV Raman/fluorescence instruments). We report results of an investigation in which samples containing organic molecules were exposed to X-ray energies and fluxes typical to micro-XRF. Samples containing alkanes and polycyclic aromatic hydrocarbons were characterized by GC-MS and UV Raman/fluorescence before being subjected to various X-ray energies and fluxes typical of PIXL. Following x-ray irradiation, samples were again characterized by GC-MS and UV Raman/fluorescence in order to characterize photochemical effects.

  14. Time-resolved materials science opportunities using synchrotron x-ray sources

    SciTech Connect

    Larson, B.C.; Tischler, J.Z.

    1995-06-01

    The high brightness, high intensity, and pulsed time-structure of synchrotron sources provide new opportunities for time-resolved x-ray diffraction investigations. With third generation synchrotron sources coming on line, high brilliance and high brightness are now available in x-ray beams with the highest flux. In addition to the high average flux, the instantaneous flux available in synchrotron beams is greatly enhanced by the pulsed time structure, which consists of short bursts of x-rays that are separated by {approximately}tens to hundreds of nanoseconds. Time-resolved one- and two-dimensional position sensitive detection techniques that take advantage of synchrotron radiation for materials science x-ray diffraction investigations are presented, and time resolved materials science applications are discussed in terms of recent diffraction and spectroscopy results and materials research opportunities.

  15. Optoelectronic measurement of x-ray synchrotron pulses: A proof of concept demonstration

    SciTech Connect

    Durbin, Stephen M.; Caffee, Marc; Savikhin, Sergei; Mahmood, Aamer; Dufresne, Eric M.; Wen, Haidan; Li, Yuelin

    2013-02-04

    Optoelectronic detection using photoconductive coplanar stripline devices has been applied to measuring the time profile of x-ray synchrotron pulses, a proof of concept demonstration that may lead to improved time-resolved x-ray studies. Laser sampling of current vs time delay between 12 keV x-ray and 800 nm laser pulses reveal the {approx}50 ps x-ray pulse width convoluted with the {approx}200 ps lifetime of the conduction band carriers. For GaAs implanted with 8 MeV protons, a time profile closer to the x-ray pulse width is observed. The protons create defects over the entire depth sampled by the x-rays, trapping the x-ray excited conduction electrons and minimizing lifetime broadening of the electrical excitation.

  16. A portable X-ray diffraction apparatus for in situ analyses of masters' paintings

    NASA Astrophysics Data System (ADS)

    Eveno, Myriam; Duran, Adrian; Castaing, Jacques

    2010-09-01

    It is rare that the analyses of materials in paintings can be carried out by taking micro-samples. Valuable works of art are best studied in situ by non-invasive techniques. For that purpose, a portable X-ray diffraction and fluorescence apparatus has been designed and constructed at the C2RMF. This apparatus has been used for paintings of Rembrandt, Leonardo da Vinci, Van Gogh, Mantegna, etc. Results are given to illustrate the performance of X-ray diffraction, especially when X-ray fluorescence does not bring sufficient information to conclude.

  17. Studies of LSO:Tb radio-luminescence properties using white beam hard X-ray synchrotron irradiation

    NASA Astrophysics Data System (ADS)

    Cecilia, A.; Rack, A.; Pelliccia, D.; Douissard, P.-A.; Martin, T.; Couchaud, M.; Dupré, K.; Baumbach, T.

    A radio-luminescence set-up was installed at the synchrotron light source ANKA to characterise scintillators under the high X-ray photon flux density of white beam synchrotron radiation. The system allows for investigating the radio-luminescence spectrum of the material under study as well as analysing in situ changes of its scintillation behaviour (e.g. under heat load and/or intensive ionising radiation). In this work we applied the radio-luminescence set-up for investigating the radiation damage effects on the luminescence properties of a new kind of thin single crystal scintillator for high resolution X-ray imaging based on a layer of modified Lu2SiO5 grown by liquid phase epitaxy on a dedicated substrate within the framework of an EC project (SCINTAX).

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

    PubMed

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

    2016-03-01

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

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

    DOEpatents

    Gibson, David M.; Gibson, Walter M.; Huang, Huapeng

    2007-06-26

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

  20. In situ anodization of aluminum surfaces studied by x-ray reflectivity and electrochemical impedance spectroscopy

    NASA Astrophysics Data System (ADS)

    Bertram, F.; Zhang, F.; Evertsson, J.; Carlà, F.; Pan, J.; Messing, M. E.; Mikkelsen, A.; Nilsson, J.-O.; Lundgren, E.

    2014-07-01

    We present results from the anodization of an aluminum single crystal [Al(111)] and an aluminum alloy [Al 6060] studied by in situ x-ray reflectivity, in situ electrochemical impedance spectroscopy and ex situ scanning electron microscopy. For both samples, a linear increase of oxide film thickness with increasing anodization voltage was found. However, the slope is much higher in the single crystal case, and the break-up of the oxide film grown on the alloy occurs at a lower anodization potential than on the single crystal. The reasons for these observations are discussed as are the measured differences observed for x-ray reflectivity and electrochemical impedance spectroscopy.

  1. In situ anodization of aluminum surfaces studied by x-ray reflectivity and electrochemical impedance spectroscopy

    SciTech Connect

    Bertram, F. Evertsson, J.; Messing, M. E.; Mikkelsen, A.; Lundgren, E.; Zhang, F.; Pan, J.; Carlà, F.; Nilsson, J.-O.

    2014-07-21

    We present results from the anodization of an aluminum single crystal [Al(111)] and an aluminum alloy [Al 6060] studied by in situ x-ray reflectivity, in situ electrochemical impedance spectroscopy and ex situ scanning electron microscopy. For both samples, a linear increase of oxide film thickness with increasing anodization voltage was found. However, the slope is much higher in the single crystal case, and the break-up of the oxide film grown on the alloy occurs at a lower anodization potential than on the single crystal. The reasons for these observations are discussed as are the measured differences observed for x-ray reflectivity and electrochemical impedance spectroscopy.

  2. Synchrotron X-ray Studies of Vulcanized Rubbers and Thermoplastic Elastomers

    SciTech Connect

    Toki,S.; Hsiao, B.; Kohjiya, S.; Tosaka, M.; Tosaka, A.; Tsou, A.; Datta, S.

    2006-01-01

    Synchrotron X-ray diffraction technique has revealed strain-induced crystallization and molecular orientation in vulcanized rubbers and thermoplastic elastomers (TPE) during deformation in real time. The stress-strain curves and wide angle X-ray diffraction (WAXD) patterns in vulcanized rubbers and TPE were measured simultaneously. In-situ WAXD patterns were taken not only at different strains during uniaxial deformation but also at different temperatures at a constant strain. Results lead to several new insights. (i) Strain-induced crystallization is a common phenomenon in vulcanized rubbers, except SBR (styrene-butadiene rubber), and in TPE (with crystalline hard segments). (ii) Strain-induced crystallization decreases the stress and increases the elongation in the strained rubber. (iii) The hybrid structure of chemical networks and strain-induced crystallites is responsible to the tensile strength and elongation at break for both systems. (iiii) Some original crystal fraction (hard segment domain) in TPE is destroyed. During deformation, strain-induced crystallization increases with strain. Upon retraction even to stress zero, the majority of oriented strain-induced crystallites remains in tack with preferred orientation.

  3. Synchrotron X-Ray Microdiffraction Studies of Electromigration in Interconnect lines at the Advanced Light Source

    SciTech Connect

    Tamura, Nobumichi; Chen, Kai; Kunz, Martin

    2009-05-01

    Synchrotron polychromatic X-ray microdiffraction is a particularly suitable technique to study in situ the effect of electromigration in metal interconnects as add spatial resolution to grain orientation and strain sensitivity. This technique has been extensively used at the Advanced Light Source to monitor changes in aluminum and copper interconnect test structures while high-density current is passed into them during accelerated tests at elevated temperature. One of the principal findings is the observation of electromigration-induced plasticity in the metal lines that appear during the very early stages of electromigration. In some of the lines, high density of geometrically necessary dislocation are formed leading to additional diffusion paths causing an enhancement of electromigration effect at test temperature. This paper presents an overview of the principal results obtained from X-ray microdiffraction studies of electromigration effects on aluminum and copper interconnects at the ALS throughout continuous efforts that spanned over a decade (1998-2008) from approximately 40 weeks of combined beamtime.

  4. X-ray irradiation of soda-lime glasses studied in situ with surface plasmon resonance spectroscopy

    SciTech Connect

    Serrano, A.; Galvez, F.; Rodriguez de la Fuente, O.; Garcia, M. A.

    2013-03-21

    We present here a study of hard X-ray irradiation of soda-lime glasses performed in situ and in real time. For this purpose, we have used a Au thin film grown on glass and studied the excitation of its surface plasmon resonance (SPR) while irradiating the sample with X-rays, using a recently developed experimental setup at a synchrotron beamline [Serrano et al., Rev. Sci. Instrum. 83, 083101 (2012)]. The extreme sensitivity of the SPR to the features of the glass substrate allows probing the modifications caused by the X-rays. Irradiation induces color centers in the soda-lime glass, modifying its refractive index. Comparison of the experimental results with simulated data shows that both, the real and the imaginary parts of the refractive index of soda-lime glasses, change upon irradiation in time intervals of a few minutes. After X-ray irradiation, the effects are partially reversible. The defects responsible for these modifications are identified as non-bridging oxygen hole centers, which fade by recombination with electrons after irradiation. The kinetics of the defect formation and fading process are also studied in real time.

  5. Rapid thermal processing chamber for in-situ x-ray diffraction

    SciTech Connect

    Ahmad, Md. Imteyaz; Van Campen, Douglas G.; Yu, Jiafan; Pool, Vanessa L.; Van Hest, Maikel F. A. M.; Toney, Michael F.; Fields, Jeremy D.; Parilla, Philip A.; Ginley, David S.

    2015-01-15

    Rapid thermal processing (RTP) is widely used for processing a variety of materials, including electronics and photovoltaics. Presently, optimization of RTP is done primarily based on ex-situ studies. As a consequence, the precise reaction pathways and phase progression during the RTP remain unclear. More awareness of the reaction pathways would better enable process optimization and foster increased adoption of RTP, which offers numerous advantages for synthesis of a broad range of materials systems. To achieve this, we have designed and developed a RTP instrument that enables real-time collection of X-ray diffraction data with intervals as short as 100 ms, while heating with ramp rates up to 100 °Cs{sup −1}, and with a maximum operating temperature of 1200 °C. The system is portable and can be installed on a synchrotron beamline. The unique capabilities of this instrument are demonstrated with in-situ characterization of a Bi{sub 2}O{sub 3}-SiO{sub 2} glass frit obtained during heating with ramp rates 5 °C s{sup −1} and 100 °C s{sup −1}, revealing numerous phase changes.

  6. An apparatus for in situ x-ray scattering studies of polymer melts during homogenous uniaxial extensional flow

    NASA Astrophysics Data System (ADS)

    Burghardt, Wesley; Mao, Ruinan

    2011-03-01

    In situ x-ray scattering methods have been broadly applied to study the structural dynamics of polymers and other complex fluids under flow, and can provide deep insights into the microstructural origins of complex non-Newtonian flow characteristics. Most studies in this vein have employed either homogenous shear flow, or processing flows such as fiber spinning which are complicated by inhomogenous deformation histories and/or nonisothermal operation. Here we present the design and implementation of a new apparatus for in situ x-ray scattering studies of polymer melts during homogenous uniaxial extensional flow. The experiment is based on the commercially-available SER extensional flow fixture, which employs two counter- rotating drums to deform a sample strip of polymer melt. This fixture has been incorporated into a custom-fabricated convection oven designed to facilitate x-ray access to the sample, and operation in a typical synchrotron beam line environment. Preliminary data on extensional flow induced orientation of ordered block copolymers will be used to illustrate the capabilities of this device.

  7. Determination of the solubility of tin indium oxide using in situ and ex x-ray diffraction

    SciTech Connect

    Gonzalez, G. B.; Mason, T. O.; Okasinski, J. S.; Buslaps, T.; Honkimaki, V.

    2012-02-01

    A novel approach to determine the thermodynamic solubility of tin in indium oxide via the exsolution from tin overdoped nano-ITO powders is presented. High-energy, in situ and ex situ synchrotron X-ray diffraction was utilized to study the solubility limit at temperatures ranging from 900 C to 1375 C. The tin exsolution from overdoped nanopowders and the formation of In{sub 4}Sn{sub 3}O{sub 12} were observed in situ during the first 4-48 h of high-temperature treatment. Samples annealed between 900 C and 1175 C were also studied ex situ with heat treatments for up to 2060 h. Structural results obtained from Rietveld analysis include compositional phase analysis, atomic positions, and lattice parameters. The tin solubility in In{sub 2}O{sub 3} was determined using the phase analysis compositions from X-ray diffraction and the elemental compositions obtained from X-ray fluorescence. Experimental complications that can lead to incorrect tin solubility values in the literature are discussed.

  8. 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.

  9. Thermal management of next-generation contact-cooled synchrotron x-ray mirrors

    SciTech Connect

    Khounsary, A.

    1999-10-29

    In the past decade, several third-generation synchrotrons x-ray sources have been constructed and commissioned around the world. Many of the major problems in the development and design of the optical components capable of handling the extremely high heat loads of the generated x-ray beams have been resolved. It is expected, however, that in the next few years even more powerful x-ray beams will be produced at these facilities, for example, by increasing the particle beam current. In this paper, the design of a next generation of synchrotron x-ray mirrors is discussed. The author shows that the design of contact-cooled mirrors capable of handing x-ray beam heat fluxes in excess of 500 W/mm{sup 2} - or more than three times the present level - is well within reach, and the limiting factor is the thermal stress rather then thermally induced slope error.

  10. Synchrotron soft X-ray absorption spectroscopy study of carbon and silicon nanostructures for energy applications.

    PubMed

    Zhong, Jun; Zhang, Hui; Sun, Xuhui; Lee, Shuit-Tong

    2014-12-10

    Carbon and silicon materials are two of the most important materials involved in the history of the science and technology development. In the last two decades, C and Si nanoscale materials, e.g., carbon nanotubes, graphene, and silicon nanowires, and quantum dots, have also emerged as the most interesting nanomaterials in nanoscience and nanotechnology for their myriad promising applications such as for electronics, sensors, biotechnology, etc. In particular, carbon and silicon nanostructures are being utilized in energy-related applications such as catalysis, batteries, solar cells, etc., with significant advances. Understanding of the nature of surface and electronic structures of nanostructures plays a key role in the development and improvement of energy conversion and storage nanosystems. Synchrotron soft X-ray absorption spectroscopy (XAS) and related techniques, such as X-ray emission spectroscopy (XES) and scanning transmission X-ray microscopy (STXM), show unique capability in revealing the surface and electronic structures of C and Si nanomaterials. In this review, XAS is demonstrated as a powerful technique for probing chemical bonding, the electronic structure, and the surface chemistry of carbon and silicon nanomaterials, which can greatly enhance the fundamental understanding and also applicability of these nanomaterials in energy applications. The focus is on the unique advantages of XAS as a complementary tool to conventional microscopy and spectroscopy for effectively providing chemical and structural information about carbon and silicon nanostructures. The employment of XAS for in situ, real-time study of property evolution of C and Si nanostructures to elucidate the mechanisms in energy conversion or storage processes is also discussed.

  11. In-situ scanning transmission X-ray microscopy of catalytic solids and related nanomaterials.

    PubMed

    de Groot, Frank M F; de Smit, Emiel; van Schooneveld, Matti M; Aramburo, Luis R; Weckhuysen, Bert M

    2010-04-01

    The present status of in-situ scanning transmission X-ray microscopy (STXM) is reviewed, with an emphasis on the abilities of the STXM technique in comparison with electron microscopy. The experimental aspects and interpretation of X-ray absorption spectroscopy (XAS) are briefly introduced and the experimental boundary conditions that determine the potential applications for in-situ XAS and in-situ STXM studies are discussed. Nanoscale chemical imaging of catalysts under working conditions is outlined using cobalt and iron Fischer-Tropsch catalysts as showcases. In the discussion, we critically compare STXM-XAS and STEM-EELS (scanning transmission electron microscopy-electron energy loss spectroscopy) measurements and indicate some future directions of in-situ nanoscale imaging of catalytic solids and related nanomaterials.

  12. Functional materials analysis using in situ and in operando X-ray and neutron scattering

    PubMed Central

    Peterson, Vanessa K.; Papadakis, Christine M.

    2015-01-01

    In situ and in operando studies are commonplace and necessary in functional materials research. This review highlights recent developments in the analysis of functional materials using state-of-the-art in situ and in operando X-ray and neutron scattering and analysis. Examples are given covering a number of important materials areas, alongside a description of the types of information that can be obtained and the experimental setups used to acquire them. PMID:25866665

  13. Synchrotron Radiation and X-ray FEL Projects in Korea

    NASA Astrophysics Data System (ADS)

    Cho, M. H.

    2012-03-01

    There are two on-going major projects in Pohang Accelerator Laboratory (PAL), the PLS-II light source upgrade and the construction of PAL-XFEL facility. PLS-II is a new light source upgraded from PLS(Pohang Light Source) which had been operated for 16 years from 1995 and shut down in Dec. 2010. The performance will be improved from ``18.9 nm-rad, 2.5 GeV, and 200 mA'' to ``5.8 nm-rad, 3 GeV, and 400 mA'' using three superconducting RF cavities. The old storage ring has been completely dismantled and new DBA ring has been re-installed in the same tunnel within 6 months, and is under commissioning now. The unique feature of PLS-II is the compact employment of 20 insertion-devices including 14 in-vacuum undulators. The PALXFEL is a 0.1-nm hard X-ray FEL construction project started in 2011 and to compete in 2014 with a total budget of 400 M. The PAL-XFEL is designed to have hard X-ray undulator lines at the end of 10-GeV linac, and a dog-leg branch line at 2.65 GeV point for a soft X-ray undulator line simultaneously and independently from hard X-ray FEL undulator line. The overview of two projects with current status is presented.

  14. Assessment of Barium Sulphate Formation and Inhibition at Surfaces with Synchrotron X-ray Diffraction (SXRD)

    SciTech Connect

    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-phosphinocarboxylic 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.

  15. Experimental measurement of lattice strain pole figures using synchrotron x rays

    SciTech Connect

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

    2005-11-15

    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) x 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.

  16. (Synchrotron studies of x-ray reflectivity from surfaces)

    SciTech Connect

    Pershan, P.S.

    1992-03-03

    Following a long period of theoretical interest, but only limited measurements, there has recently been an increased number of attempts to expand the relative paucity of experimental information on the structure of liquid surfaces using techniques as diverse as ellipsometry, micro-force balances, non-linear optics, Auger and photoelectron spectroscopy, and x-ray scattering. Our group has played a leading role in the currently expanding application of scattering techniques to the general problem of characterizing the microscopic structure of liquid surfaces and we propose here that this work be extended specifically to liquid metals. In the following sections we will briefly describe the salient features of x-ray scattering that are relevant to the current project, the progress that we have made in the current grant period and the work that we propose to carry out in the forthcoming grant period.

  17. Neutron and Synchrotron X-Ray Scattering Studies of Superconductors

    SciTech Connect

    Tranquada,J.M.

    2008-09-01

    Superconductors hold the promise for a more stable and efficient electrical grid, but new isotropic, high-temperature superconductors are needed in order to reduce cable manufacturing costs. The effort to understand high-temperature superconductivity, especially in the layered cuprates, provides guidance to the search for new superconductors. Neutron scattering has long provided an important probe of the collective excitations that are involved in the pairing mechanism. For the cuprates, neutron and x-ray diffraction techniques also provide information on competing types of order, such as charge and spin stripes, that appear to be closely connected to the superconductivity. Recently, inelastic x-ray scattering has become competitive for studying phonons and may soon provide valuable information on electronic excitations. Examples of how these techniques contribute to our understanding of superconductivity are presented.

  18. X-ray Synchrotron Radiation in a Plasma Wiggler

    SciTech Connect

    Wang, Shuoquin; /UCLA /SLAC, SSRL

    2005-09-27

    A relativistic electron beam can radiate due to its betatron motion inside an ion channel. The ion channel is induced by the electron bunch as it propagates through an underdense plasma. In the theory section of this thesis the formation of the ion channel, the trajectories of beam electrons inside the ion channel, the radiation power and the radiation spectrum of the spontaneous emission are studied. The comparison between different plasma wiggler schemes is made. The difficulties in realizing stimulated emission as the beam traverses the ion channel are investigated, with particular emphasis on the bunching mechanism, which is important for the ion channel free electron laser. This thesis reports an experiment conducted at the Stanford Linear Accelerator Center (SLAC) to measure the betatron X-ray radiations for the first time. They first describe the construction and characterization of the lithium plasma source. In the experiment, the transverse oscillations of the SLAC 28.5 GeV electron beam traversing through a 1.4 meter long lithium plasma source are clearly seen. These oscillations lead to a quadratic density dependence of the spontaneously emitted betatron X-ray radiation. The divergence angle of the X-ray radiation is measured. The absolute photon yield and the spectral brightness at 14.2 KeV photon energy are estimated and seen to be in reasonable agreement with theory.

  19. 3D-analysis of plant microstructures: advantages and limitations of synchrotron X-ray microtomography

    NASA Astrophysics Data System (ADS)

    Matsushima, U.; Graf, W.; Zabler, S.; Manke, I.; Dawson, M.; Choinka, G.; Hilger, A.; Herppich, W. B.

    2013-01-01

    Synchrotron X-ray computer microtomography was used to analyze the microstructure of rose peduncles. Samples from three rose cultivars, differing in anatomy, were scanned to study the relation between tissue structure and peduncles mechanical strength. Additionally, chlorophyll fluorescence imaging and conventional light microscopy was applied to quantify possible irradiation-induced damage to plant physiology and tissue structure. The spatial resolution of synchrotron X-ray computer microtomography was sufficiently high to investigate the complex tissues of intact rose peduncles without the necessity of any preparation. However, synchrotron X-radiation induces two different types of damage on irradiated tissues. First, within a few hours after first X-ray exposure, there is a direct physical destruction of cell walls. In addition, a slow and delayed destruction of chlorophyll and, consequently, of photosynthetic activity occurred within hours/ days after the exposure. The results indicate that synchrotron X-ray computer microtomography is well suited for three-dimensional visualization of the microstructure of rose peduncles. However, in its current technique, synchrotron X-ray computer microtomography is not really non-destructive but induce tissue damage. Hence, this technique needs further optimization before it can be applied for time-series investigations of living plant materials

  20. Mapping strain fields induced in Zr-based bulk metallic glasses during in-situ nanoindentation by X-ray nanodiffraction

    NASA Astrophysics Data System (ADS)

    Gamcová, J.; Mohanty, G.; Michalik, Š.; Wehrs, J.; Bednarčík, J.; Krywka, C.; Breguet, J. M.; Michler, J.; Franz, H.

    2016-01-01

    A pioneer in-situ synchrotron X-ray nanodiffraction approach for characterization and visualization of strain fields induced by nanoindentation in amorphous materials is introduced. In-situ nanoindentation experiments were performed in transmission mode using a monochromatic and highly focused sub-micron X-ray beam on 40 μm thick Zr-based bulk metallic glass under two loading conditions. Spatially resolved X-ray diffraction scans in the deformed volume of Zr-based bulk metallic glass covering an area of 40 × 40 μm2 beneath the pyramidal indenter revealed two-dimensional map of elastic strains. The largest value of compressive elastic strain calculated from diffraction data at 1 N load was -0.65%. The region of high elastic compressive strains (<-0.3%) is located beneath the indenter tip and has radius of 7 μm.

  1. 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.

  2. Note: Sample chamber for in situ x-ray absorption spectroscopy studies of battery materials

    SciTech Connect

    Pelliccione, CJ; Timofeeva, EV; Katsoudas, JP; Segre, CU

    2014-12-01

    In situ x-ray absorption spectroscopy (XAS) provides element-specific characterization of both crystalline and amorphous phases and enables direct correlations between electrochemical performance and structural characteristics of cathode and anode materials. In situ XAS measurements are very demanding to the design of the experimental setup. We have developed a sample chamber that provides electrical connectivity and inert atmosphere for operating electrochemical cells and also accounts for x-ray interactions with the chamber and cell materials. The design of the sample chamber for in situ measurements is presented along with example XAS spectra from anode materials in operating pouch cells at the Zn and Sn K-edges measured in fluorescence and transmission modes, respectively. (C) 2014 AIP Publishing LLC.

  3. Facility for combined in situ magnetron sputtering and soft x-ray magnetic circular dichroism

    SciTech Connect

    Telling, N. D.; Laan, G. van der; Georgieva, M. T.; Farley, N. R. S.

    2006-07-15

    An ultrahigh vacuum chamber that enables the in situ growth of thin films and multilayers by magnetron sputtering techniques is described. Following film preparation, x-ray absorption spectroscopy (XAS) and x-ray magnetic circular dichroism (XMCD) measurements are performed by utilizing an in vacuum electromagnet. XMCD measurements on sputtered thin films of Fe and Co yield spin and orbital moments that are consistent with those obtained previously on films measured in transmission geometry and grown in situ by evaporation methods. Thin films of FeN prepared by reactive sputtering are also examined and reveal an apparent enhancement in the orbital moment for low N content samples. The advantages of producing samples for in situ XAS and XMCD studies by magnetron sputtering are discussed.

  4. Note: Dynamic strain field mapping with synchrotron X-ray digital image correlation

    SciTech Connect

    Lu, L.; Fan, D.; Luo, S. N.; Bie, B. X.; Ran, X. X.; Qi, M. L.; Parab, N.; Sun, J. Z.; Liao, H. J.; Hudspeth, M. C.; Claus, B.; Fezzaa, K.; Sun, T.; Chen, W.; Gong, X. L.

    2014-07-15

    We present a dynamic strain field mapping method based on synchrotron X-ray digital image correlation (XDIC). Synchrotron X-ray sources are advantageous for imaging with exceptional spatial and temporal resolutions, and X-ray speckles can be produced either from surface roughness or internal inhomogeneities. Combining speckled X-ray imaging with DIC allows one to map strain fields with high resolutions. Based on experiments on void growth in Al and deformation of a granular material during Kolsky bar/gas gun loading at the Advanced Photon Source beamline 32ID, we demonstrate the feasibility of dynamic XDIC. XDIC is particularly useful for dynamic, in-volume, measurements on opaque materials under high strain-rate, large, deformation.

  5. Synthesis of metallic nanoparticles through X-ray radiolysis using synchrotron radiation

    NASA Astrophysics Data System (ADS)

    Yamaguchi, Akinobu; Okada, Ikuo; Fukuoka, Takao; Sakurai, Ikuya; Utsumi, Yuichi

    2016-05-01

    The potential to fabricate metallic nanoparticles directly on silicon substrates from liquid solutions is ideal for three-dimensional lithography systems, drug delivery materials, and sensing applications. Here, we report the successful synthesis of Au, Cu, and Fe nanoparticles from the corresponding liquid solutions [gold(I) trisodium disulphite, copper(II) sulfate, and potassium ferricyanide] by synchrotron (SR) X-ray irradiation. The deposition of gold nanoparticles in the gold(I) trisodium disulphite solution was performed by monochromatic X-ray exposure from synchrotron radiation. The use of ethanol as an additive enabled the nucleation and growth of Cu particles, while no Cu particles were produced in the copper sulfate solution without ethanol with polychromatic SR X-ray irradiation. Fe particles were generated by direct polychromatic SR X-ray irradiation. These results demonstrate the behavior of three-dimensional printers, enabling us to build composite material structures with metallic and plastic materials.

  6. In-situ Scanning Transmission X-ray Microscopy of catalytic materials under reaction conditions

    NASA Astrophysics Data System (ADS)

    de Smit, Emiel; Creemer, J. Fredrik; Zandbergen, Henny W.; Weckhuysen, Bert M.; de Groot, Frank M. F.

    2009-11-01

    In-situ Scanning X-ray Transmission Microscopy (STXM) allows the measurement of the soft X-ray absorption spectra with 10 to 30 nm spatial resolution under realistic reaction conditions. We show that STXM-XAS in combination with a micromachined nanoreactor can image a catalytic system under relevant reaction conditions, and provide detailed information on the morphology and composition of the catalyst material. The nanometer resolution combined with powerful chemical speciation by XAS and the ability to image materials under realistic conditions opens up new opportunities to study many chemical processes.

  7. In-situ x-ray measurements of pit solutions during localized corrosion

    SciTech Connect

    Cho, J.H.; Davenport, A.J.; Isaacs, H.S.

    1991-01-01

    In this work, in-situ x-ray absorption spectroscopy (XAS) measurements of the ion concentrations within an artificial pit are presented to study the ionic species present and mass transport phenomena during localized corrosion taking place on metal surfaces. The x-ray absorption by an element in a sample is markedly greater at an energy just above than just below one of its absorption edges and the energy of this edge is characteristic of the absorbing element. A pair of measurement above and below the edge serves to determine both the presence and the amount of the element sought. 9 refs., 3 figs.

  8. DEVELOPMENTS IN SYNCHROTRON X-RAY COMPUTED MICROTOMOGRAPHY AT THE NATIONAL SYNCHROTRON LIGHT SOURCE.

    SciTech Connect

    DOWD,B.A.

    1999-07-23

    Last year, the X27A beamline at the National Synchrotron Light Source (NSLS) became dedicated solely to X-Ray Computed Microtomography (XCMT). This is a third-generation instrument capable of producing tomographic volumes of 1-2 micron resolution over a 2-3mm field of view. Recent enhancements will be discussed. These have focused on two issues: the desire for real-time data acquisition and processing and the need for highly monochromatic beam (.1 % energy bandpass). The latter will permit k-edge subtraction studies and will provide improved image contrast from below the Cr (6 keV) up to the Cs (36 keV) k-edge. A range of applications that benefit from these improvements will be discussed as well. These two goals are somewhat counterproductive, however; higher monochromaticity yields a lower flux forcing longer data acquisition times. To balance the two, a more efficient scintillator for X-ray conversion is being developed. Some testing of a prototype scintillator has been performed; preliminary results will be presented here. In the meantime, data reconstruction times have been reduced, and the entire tomographic acquisition, reconstruction and volume rendering process streamlined to make efficient use of synchrotron beam time. A Fast Filtered Back Transform (FFBT) reconstruction program recently developed helped to reduce the time to reconstruct a volume of 150 x 150 x 250 pixels{sup 3} (over 5 million voxels) from the raw camera data to 1.5 minutes on a dual R10,000 CPU. With these improvements, one can now obtain a ''quick look'' of a small tomographic volume ({approximately}10{sup 6}voxels) in just over 15 minutes from the start of data acquisition.

  9. Ultra-high vacuum compatible optical chopper system for synchrotron x-ray scanning tunneling microscopy

    NASA Astrophysics Data System (ADS)

    Chang, Hao; Cummings, Marvin; Shirato, Nozomi; Stripe, Benjamin; Rosenmann, Daniel; Preissner, Curt; Freeland, John W.; Kersell, Heath; Hla, Saw-Wai; Rose, Volker

    2016-01-01

    High-speed beam choppers are a crucial part of time-resolved x-ray studies as well as a necessary component to enable elemental contrast in synchrotron x-ray scanning tunneling microscopy (SX-STM). However, many chopper systems are not capable of operation in vacuum, which restricts their application to x-ray studies with high photon energies, where air absorption does not present a significant problem. To overcome this limitation, we present a fully ultra-high vacuum (UHV) compatible chopper system capable of operating at variable chopping frequencies up to 4 kHz. The lightweight aluminum chopper disk is coated with Ti and Au films to provide the required beam attenuation for soft and hard x-rays with photon energies up to about 12 keV. The chopper is used for lock-in detection of x-ray enhanced signals in SX-STM.

  10. Short-period cyclic loading system for in situ X-ray observation of anelastic properties at high pressure

    NASA Astrophysics Data System (ADS)

    Yoshino, Takashi; Yamazaki, Daisuke; Tange, Yoshinori; Higo, Yuji

    2016-10-01

    To determine the anelastic properties of materials of the Earth's interior, a short-period cyclic loading system was installed for in situ X-ray radiographic observation under high pressure to the multi-anvil deformation DIA press at the bending magnet beam line BL04B1 at SPring-8. The hydraulic system equipped with a piston controlled by a solenoid was designed so as to enable producing smooth sinusoidal stress in a wide range of oscillation period from 0.2 to 100 s and generating variable amplitudes. Time resolved X-ray radiography imaging of the sample and reference material provides their strain as a function of time during cyclic loading. A synchrotron X-ray radiation source allows us to resolve their strain variation with time even at the short period (<1 s). The minimum resolved strain is as small as 10-4, and the shortest oscillation period to detect small strain is 0.5 s. Preliminary experimental results exhibited that the new system can resolve attenuation factor Q-1 at upper mantle conditions. These results are in quantitative agreement with previously reported data obtained at lower pressures.

  11. Omega Dante soft x-ray power diagnostic component calibration at the National Synchrotron Light Source

    NASA Astrophysics Data System (ADS)

    Campbell, K. M.; Weber, F. A.; Dewald, E. L.; Glenzer, S. H.; Landen, O. L.; Turner, R. E.; Waide, P. A.

    2004-10-01

    The Dante soft x-ray spectrometer, installed on the Omega laser facility at the Laboratory for Laser Energetics, University of Rochester, is a 12-channel filter-edge defined soft x-ray power diagnostic. It is used to measure the spectrally resolved, absolute flux from direct drive, indirect drive (hohlraums) and other plasma sources. Dante component calibration efforts using two beam lines, U3C (50 eV-1 keV) and X8A (1-6 keV) at the National Synchrotron Light Source have been implemented to improve the accuracy of these measurements. We have calibrated metallic vacuum x-ray diodes, mirrors and filters.

  12. 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.

  13. Omega Dante Soft X-Ray Power Diagnostic Component Calibration at the National Synchrotron Light Source

    SciTech Connect

    Campbell, K; Weber, F; Dewald, E; Glenzer, S; Landen, O; Turner, R; Waide, P

    2004-04-15

    The Dante soft x-ray spectrometer installed on the Omega laser facility at the Laboratory for Laser Energetics, University of Rochester is a twelve-channel filter-edge defined x-ray power diagnostic. It is used to measure the absolute flux from direct drive, indirect drive (hohlraums) and other plasma sources. Calibration efforts using two beam lines, U3C (50eV-1keV) and X8A (1keV-6keV) at the National Synchrotron Light Source (NSLS) have been implemented to insure the accuracy of these measurements. We have calibrated vacuum x-ray diodes, mirrors and filters.

  14. Rare earth element concentrations in geological and synthetic samples using synchrotron X-ray fluorescence analysis

    USGS Publications Warehouse

    Chen, J.R.; Chao, E.C.T.; Back, J.M.; Minkin, J.A.; Rivers, M.L.; Sutton, S.R.; Cygan, G.L.; Grossman, J.N.; Reed, M.J.

    1993-01-01

    The concentrations of rare earth elements (REEs) in specific mineral grains from the Bayan Obo ore deposit and synthetic high-silica glass samples have been measured by synchrotron X-ray fluorescence (SXRF) analysis using excitation of the REE K lines between 33 and 63 keV. Because SXRF, a nondestructive analytical technique, has much lower minimum detection limits (MDLs) for REEs, it is an important device that extends the in situ analytical capability of electron probe microanalysis (EPMA). The distribution of trace amounts of REEs in common rock-forming minerals, as well as in REE minerals and minerals having minor quantities of REEs, can be analyzed with SXRF. Synchrotron radiation from a bending magnet and a wiggler source at the National Synchrotron Light Source, Brookhaven National Laboratory, was used to excite the REEs. MDLs of 6 ppm (La) to 26 ppm (Lu) for 3600 s in 60-??m-thick standard samples were obtained with a 25-??m diameter wiggler beam. The MDLs for the light REEs were a factor of 10-20 lower than the MDLs obtained with a bending magnet beam. The SXRF REE concentrations in mineral grains greater than 25 ??m compared favorably with measurements using EPMA. Because EPMA offered REE MDLs as low as several hundred ppm, the comparison was limited to the abundant light REEs (La, Ce, Pr, Nd). For trace values of medium and heavy REEs, the SXRF concentrations were in good agreement with measurements using instrumental neutron activation analysis (INAA), a bulk analysis technique. ?? 1993.

  15. Evaluation of different synchrotron beamline configurations for X-ray fluorescence analysis of environmental samples.

    PubMed

    Barberie, Sean R; Iceman, Christopher R; Cahill, Catherine F; Cahill, Thomas M

    2014-08-19

    Synchrotron radiation X-ray fluorescence (SR-XRF) is a powerful elemental analysis tool, yet synchrotrons are large, multiuser facilities that are generally not amenable to modification. However, the X-ray beamlines from synchrotrons can be modified by simply including X-ray filters or removing monochromators to improve the SR-XRF analysis. In this study, we evaluated four easily applied beamline configurations for the analysis of three representative environmental samples, namely a thin aerosol sample, an intermediate thickness biological sample, and a thick rare earth mineral specimen. The results showed that the "white beam" configuration, which was simply the full, polychromatic output of the synchrotron, was the optimal configuration for the analysis of thin samples with little mass. The "filtered white beam" configuration removed the lower energy X-rays from the excitation beam so it gave better sensitivity for elements emitting more energetic X-rays. The "filtered white beam-filtered detector" configuration sacrifices the lower energy part of the spectrum (<15 keV) for improved sensitivity in the higher end (∼26 to 48 keV range). The use of a monochromatic beam, which tends to be the standard mode of operation for most SR-XRF analyses reported in the literature, gave the least sensitive analysis.

  16. In situ measurements of X-ray peak profile asymmetry from individual grains

    NASA Astrophysics Data System (ADS)

    Wejdemann, C.; Lienert, U.; Pantleon, W.

    2010-07-01

    Two copper samples, pre-deformed in tension to 5% plastic strain, are subjected to an in situ tensile deformation of 1% plastic strain while X-ray peak profiles from individual bulk grains are obtained. One sample is oriented with the in situ tensile axis parallel to the pre-deformation axis, and peak profiles are obtained with the scattering vector parallel to this direction. The profiles show the expected asymmetry explained by the composite model as caused by intra-grain stresses. The other sample is oriented with the in situ tensile axis perpendicular to the pre-deformation axis, and peak profiles are obtained with the scattering vector parallel to the in situ tensile axis. In this case the profiles initially show an opposite asymmetry, but during the in situ deformation the asymmetry reverses sign as the deformation under new loading conditions leads to changes in the intra-grain stresses.

  17. In situ measurements of x-ray peak profile asymmetry from individual grains.

    SciTech Connect

    Wejdemann, C.; Lienert, U.; Pantleon, W.; X-Ray Science Division; Univ. of Denmark

    2010-01-01

    Two copper samples, pre-deformed in tension to 5% plastic strain, are subjected to an in situ tensile deformation of 1% plastic strain while X-ray peak profiles from individual bulk grains are obtained. One sample is oriented with the in situ tensile axis parallel to the pre-deformation axis, and peak profiles are obtained with the scattering vector parallel to this direction. The profiles show the expected asymmetry explained by the composite model as caused by intra-grain stresses. The other sample is oriented with the in situ tensile axis perpendicular to the pre-deformation axis, and peak profiles are obtained with the scattering vector parallel to the in situ tensile axis. In this case the profiles initially show an opposite asymmetry, but during the in situ deformation the asymmetry reverses sign as the deformation under new loading conditions leads to changes in the intra-grain stresses.

  18. Custom AFM for X-ray beamlines: in situ biological investigations under physiological conditions.

    PubMed

    Gumí-Audenis, B; Carlà, F; Vitorino, M V; Panzarella, A; Porcar, L; Boilot, M; Guerber, S; Bernard, P; Rodrigues, M S; Sanz, F; Giannotti, M I; Costa, L

    2015-11-01

    A fast atomic force microscope (AFM) has been developed that can be installed as a sample holder for grazing-incidence X-ray experiments at solid/gas or solid/liquid interfaces. It allows a wide range of possible investigations, including soft and biological samples under physiological conditions (hydrated specimens). The structural information obtained using the X-rays is combined with the data gathered with the AFM (morphology and mechanical properties), providing a unique characterization of the specimen and its dynamics in situ during an experiment. In this work, lipid monolayers and bilayers in air or liquid environment have been investigated by means of AFM, both with imaging and force spectroscopy, and X-ray reflectivity. In addition, this combination allows the radiation damage induced by the beam on the sample to be studied, as has been observed on DOPC and DPPC supported lipid bilayers under physiological conditions. PMID:26524300

  19. In Situ X-Ray Probing Reveals Fingerprints of Surface Platinum Oxide

    SciTech Connect

    Friebel, Daniel

    2011-08-24

    In situ x-ray absorption spectroscopy (XAS) at the Pt L{sub 3} edge is a useful probe for Pt-O interactions at polymer electrolyte membrane fuel cell (PEMFC) cathodes. We show that XAS using the high energy resolution fluorescence detection (HERFD) mode, applied to a well-defined monolayer Pt/Rh(111) sample where the bulk penetrating hard x-rays probe only surface Pt atoms, provides a unique sensitivity to structure and chemical bonding at the Pt-electrolyte interface. Ab initio multiple-scattering calculations using the FEFF8 code and complementary extended x-ray absorption fine structure (EXAFS) results indicate that the commonly observed large increase of the white-line at high electrochemical potentials on PEMFC cathodes originates from platinum oxide formation, whereas previously proposed chemisorbed oxygen-containing species merely give rise to subtle spectral changes.

  20. Custom AFM for X-ray beamlines: in situ biological investigations under physiological conditions

    PubMed Central

    Gumí-Audenis, B.; Carlà, F.; Vitorino, M. V.; Panzarella, A.; Porcar, L.; Boilot, M.; Guerber, S.; Bernard, P.; Rodrigues, M. S.; Sanz, F.; Giannotti, M. I.; Costa, L.

    2015-01-01

    A fast atomic force microscope (AFM) has been developed that can be installed as a sample holder for grazing-incidence X-ray experiments at solid/gas or solid/liquid interfaces. It allows a wide range of possible investigations, including soft and biological samples under physiological conditions (hydrated specimens). The structural information obtained using the X-rays is combined with the data gathered with the AFM (morphology and mechanical properties), providing a unique characterization of the specimen and its dynamics in situ during an experiment. In this work, lipid monolayers and bilayers in air or liquid environment have been investigated by means of AFM, both with imaging and force spectroscopy, and X-ray reflectivity. In addition, this combination allows the radiation damage induced by the beam on the sample to be studied, as has been observed on DOPC and DPPC supported lipid bilayers under physiological conditions. PMID:26524300

  1. Ultra-fast in-situ X-ray studies of evolving columnar dendrites in solidifying steel weld pools

    NASA Astrophysics Data System (ADS)

    Mirihanage, W. U.; Di Michiel, M.; Mathiesen, R. H.

    2015-06-01

    High-brilliance polychromatic synchrotron radiation has been used to conduct in-situ studies of the solidification microstructure evolution during simulated welding. The welding simulations were realized by rapidly fusing ∼ 5 mm spot in Fe-Cr-Ni steel. During the solid- liquid-solid phase transformations, a section of the weld pool was placed in an incident 50-150 keV polychromatic synchrotron X-ray beam, in a near-horizontal position at a very low inclination angle. Multiple high-resolution 2D detectors with very high frame rates were utilized to capture time resolved X-ray diffraction data from suitably oriented solid dendrites evolving in the weld pool. Comprehensive analysis of the diffraction data revealed individual and overall dendritic growth characteristics and relevant melt and solid flow dynamics during weld pool solidification, which was completed within 1.5 s. Columnar dendrite tip velocities were estimated from the experimental data and during early stages of solidification were exceeded 4 mm/s. The most remarkable observation revealed through the time-resolved reciprocal space observations are correlated to significant tilting of columnar type dendrites at their root during solidification, presumably caused by convective currents in the weld pool. When the columnar dendrite tilting are transformed to respective metric linear tilting velocities at the dendrite tip; tilting velocities are found to be in the same order of magnitude as the columnar tip growth velocities, suggesting a highly transient nature of growth conditions.

  2. Compton scattering imaging of a working battery using synchrotron high-energy X-rays.

    PubMed

    Itou, Masayoshi; Orikasa, Yuki; Gogyo, Yuma; Suzuki, Kosuke; Sakurai, Hiroshi; Uchimoto, Yoshiharu; Sakurai, Yoshiharu

    2015-01-01

    Results of studies on Compton scattering imaging using synchrotron high-energy X-rays are reported. The technique is applied to a discharging coin cell, and the intensity of Compton scattered X-rays from the inside of the cell has been measured as a function of position and time. The position-time intensity map captures the migration of lithium ions in the positive electrode and reveals the structural change due to the volume expansion of the electrode. This experiment is a critical step in developing synchrotron-based Compton scattering imaging for electrochemical cells at a product level.

  3. Micro-structural characterization of materials using synchrotron hard X-ray imaging techniques

    SciTech Connect

    Agrawal, Ashish Singh, Balwant; Kashyap, Yogesh; Sarkar, P. S.; Shukla, Mayank; Sinha, Amar

    2015-06-24

    X-ray imaging has been an important tool to study the materials microstructure with the laboratory based sources however the advent of third generation synchrotron sources has introduced new concepts in X-ray imaging such as phase contrast imaging, micro-tomography, fluorescence imaging and diffraction enhance imaging. These techniques are being used to provide information of materials about their density distribution, porosity, geometrical and morphological characteristics at sub-micron scalewith improved contrast. This paper discusses the development of various imaging techniques at synchrotron based imaging beamline Indus-2 and few recent experiments carried out at this facility.

  4. In-situ transmission x-ray microscopy study of photon-induced oxidation of silver nanowires

    NASA Astrophysics Data System (ADS)

    Yu, Le; Sun, Yugang; Wang, Yuxin; Cai, Zhonghou; Han, Ping; Cheng, X. M.

    Oxidation of metal nanoparticles usually follows a Kirkendall process to transform solid nanoparticles to hollow metal oxide nanoshells. However the morphological trajectory of nanoparticles and the mass diffusion kinetics involved in the nanoscale Kirkendall process are complex. In this presentation we report the use of in-situ transmission x-ray microscopy (TXM) to directly image individual silver nanowires under oxidation atmosphere, which are created from radiolysis of air under illumination of the focused synchrotron x-ray beam. The in-situ results clearly show the morphological transformation from solid silver nanowires to hollow nanotubes in the course of oxidation reaction of silver. Quantitative analysis of the time-resolved TXM images provides unprecedented details on reaction kinetics and mass diffusion kinetics associated with the oxidation process. Work at Bryn Mawr College is supported by NSF Grant #1207085. Use of the Advanced Photon Source and the Center for Nanoscale Materials at Argonne National Laboratory was supported by the U. S. Department of Energy, Office of Science, Office of Basic Energy Sciences, under Contract No. DE-AC02-06CH11357.

  5. 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.

  6. Cyclic olefin homopolymer-based microfluidics for protein crystallization and in situ X-ray diffraction

    SciTech Connect

    Emamzadah, Soheila; Petty, Tom J.; De Almeida, Victor; Nishimura, Taisuke; Joly, Jacques; Ferrer, Jean-Luc; Halazonetis, Thanos D.

    2009-09-01

    A cyclic olefin homopolymer-based microfluidics system has been established for protein crystallization and in situ X-ray diffraction. Microfluidics is a promising technology for the rapid identification of protein crystallization conditions. However, most of the existing systems utilize silicone elastomers as the chip material which, despite its many benefits, is highly permeable to water vapour. This limits the time available for protein crystallization to less than a week. Here, the use of a cyclic olefin homopolymer-based microfluidics system for protein crystallization and in situ X-ray diffraction is described. Liquid handling in this system is performed in 2 mm thin transparent cards which contain 500 chambers, each with a volume of 320 nl. Microbatch, vapour-diffusion and free-interface diffusion protocols for protein crystallization were implemented and crystals were obtained of a number of proteins, including chicken lysozyme, bovine trypsin, a human p53 protein containing both the DNA-binding and oligomerization domains bound to DNA and a functionally important domain of Arabidopsis Morpheus’ molecule 1 (MOM1). The latter two polypeptides have not been crystallized previously. For X-ray diffraction analysis, either the cards were opened to allow mounting of the crystals on loops or the crystals were exposed to X-rays in situ. For lysozyme, an entire X-ray diffraction data set at 1.5 Å resolution was collected without removing the crystal from the card. Thus, cyclic olefin homopolymer-based microfluidics systems have the potential to further automate protein crystallization and structural genomics efforts.

  7. Minimally Invasive Coronary Angiography with Monochromatic X-Rays Developmental Studies Utilizing Synchrotron Radiation.

    NASA Astrophysics Data System (ADS)

    Otis, John Noel

    Iodine-containing compounds are used as contrast agents in obtaining X-ray images of blood vessels for medical diagnosis. If the X-ray contrast produced by iodine can be enhanced sufficiently relative to that produced by the intervening body tissues, it becomes possible to obtain images of arteries by introducing the contrast agent into the venous circulation rather than through an arterial catheter directly into the vessel under examination. This prospect is attractive because invasion of the arterial system is the chief cause of the medical complications that are encountered in the application of current angiographic procedures. An imaging system that shows promise of accomplishing this goal for examination of the coronary arteries has been developed for operation in an X-ray beam at the Stanford Synchrotron Radiation Laboratory. Iodine-selective contrast enhancement is achieved by logarithmic subtraction of two images of the same field. One of these images is formed by monochromatic X-rays of energy just above the characteristic iodine K-absorption edge at 33.17 keV, the other by X-rays of energy just below the edge. The computer-controlled imaging system acquires digitized images line by line while scanning the subject through a stationary X-ray beam of linear profile. At present, only synchrotron radiation can provide monochromatic X-ray beams of intensity sufficient to image the small and rapidly moving coronary arteries. Preliminary studies of static phantoms and in vivo studies of dogs establish the feasibility of using synchrotron radiation as the X-ray source for iodine-selective imaging with sensitivity and speed adequate for providing sharp images of coronary arteries after intravenous introduction of contrast agent. Application of the method to human subjects began with imaging studies of three patients in May, 1986.

  8. A seven-crystal Johann-type hard x-ray spectrometer at the Stanford Synchrotron Radiation Lightsource

    SciTech Connect

    Sokaras, D.; Weng, T.-C.; Nordlund, D.; Velikov, P.; Wenger, D.; Garachtchenko, A.; George, M.; Borzenets, V.; Johnson, B.; Rabedeau, T.; Alonso-Mori, R.; Bergmann, U.

    2013-05-15

    We present a multicrystal Johann-type hard x-ray spectrometer ({approx}5-18 keV) recently developed, installed, and operated at the Stanford Synchrotron Radiation Lightsource. The instrument is set at the wiggler beamline 6-2 equipped with two liquid nitrogen cooled monochromators - Si(111) and Si(311) - as well as collimating and focusing optics. The spectrometer consists of seven spherically bent crystal analyzers placed on intersecting vertical Rowland circles of 1 m of diameter. The spectrometer is scanned vertically capturing an extended backscattering Bragg angular range (88 Degree-Sign -74 Degree-Sign ) while maintaining all crystals on the Rowland circle trace. The instrument operates in atmospheric pressure by means of a helium bag and when all the seven crystals are used (100 mm of projected diameter each), has a solid angle of about 0.45% of 4{pi} sr. The typical resolving power is in the order of (E/{Delta}E){approx}10 000. The spectrometer's high detection efficiency combined with the beamline 6-2 characteristics permits routine studies of x-ray emission, high energy resolution fluorescence detected x-ray absorption and resonant inelastic x-ray scattering of very diluted samples as well as implementation of demanding in situ environments.

  9. Electrochemical flowcell for in-situ investigations by soft x-ray absorption and emission spectroscopy

    SciTech Connect

    Schwanke, C.; Lange, K. M.; Golnak, R.; Xiao, J.

    2014-10-15

    A new liquid flow-cell designed for electronic structure investigations at the liquid-solid interface by soft X-ray absorption and emission spectroscopy is presented. A thin membrane serves simultaneously as a substrate for the working electrode and solid state samples as well as for separating the liquid from the surrounding vacuum conditions. In combination with counter and reference electrodes this approach allows in-situ studies of electrochemical deposition processes and catalytic reactions at the liquid-solid interface in combination with potentiostatic measurements. As model system in-situ monitoring of the deposition process of Co metal from a 10 mM CoCl{sub 2} aqueous solution by X-ray absorption and emission spectroscopy is presented.

  10. Development of in situ, at-wavelength metrology for soft x-ray nano-focusing

    SciTech Connect

    Yuan, Sheng Sam; Yashchuk, Valeriy V.; Goldberg, Kenneth A.; Celestre, Richard; McKinney, Wayne R.; Morrison, Gregory Y.; Warwick, Tony; Padmore, Howard A.

    2010-09-19

    At the Advanced Light Source (ALS), we are developing broadly applicable, high-accuracy, in situ, at-wavelength wavefront slope measurement techniques for Kirkpatrick-Baez (KB) mirror nano-focusing. We describe here details of the metrology beamline endstation, the at-wavelength tests, and an original alignment method that have already allowed us to precisely set a bendable KB mirror to achieve a FWHM focused spot size of ~;;120 nm, at 1-nm soft x-ray wavelength.

  11. 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

  12. Biomimetic growth of calcium oxalate crystals: synchrotron X-ray studies

    NASA Astrophysics Data System (ADS)

    Uysal, Ahmet; Stripe, Benjamin; Dutta, Pulak

    2010-03-01

    Oriented crystals of calcium oxalate monohydrate (COM) form one of the major constituents of kidney stones in humans, and these crystals are also found in many plants. It is widely accepted that an organic matrix of lipids and proteins is involved in the crystallization of COM, though their role is not well-understood [1]. Langmuir monolayers of lipids on supersaturated aqueous solutions can be used to mimic the lipid-crystal interface during mineralization. We have studied nucleation and growth of COM crystals under heneicosanoic acid monolayers at the air-water interface. We used synchrotron x-rays in the grazing incidence geometry to determine the structure of the organic monolayer and the orientation of COM crystals in-situ during crystallization. We see that the (-101) faces of COM crystals are parallel to the organic matrix. There is a commensurate relationship between the heneicosanoic acid monolayer and the (-101) crystal face that may be responsible from the oriented growth. Evolution of the monolayer structure with time will be described. [1]S. R. Khan, Calcium Oxalate in Biological Systems, CRC Press, Boca Raton, 1995

  13. Diamond for high-heat-load synchrotron x-ray applications

    SciTech Connect

    Lee, Wah-Keat

    1994-12-31

    Synchrotron facilities worldwide provide scientists with useful radiation in the ultraviolet to the x-ray regime. Third-generation synchrotron sources win deliver photon fluxes in the 10{sup 15} photons/s/0.1%BW range, with brilliance on the order of 10{sup 18} photons/s/0.1%BW/mrad{sup 2}/mm{sup 2}. Along with the increase in flux and brilliance is an increase in the power and power densities of the x-ray beam. Depending on the particular insertion device, the x-ray beam can have total power in excess of 10 kW and peak power, density of more than 400 W/mm{sup 2}. Such high heat loads are a major challenge in the design and fabrication of x-ray beamline components. The superior thermal and mechanical properties of diamond make it a good candidate as material in these components. Single crystal diamonds can be used as x-ray monochromators, while polycrystalline or CVD diamonds can be used in a variety of ways on the front-end beamline components. This paper discusses the issues regarding the feasibility of using diamond in third-generation synchrotron beamline components.

  14. Synchrotron Radiation X-Ray Spectroscopy for Investigations of Intracellular Metallointercalators: X-Ray Fluorescence Imaging and X-Ray Absorption Spectroscopy

    NASA Astrophysics Data System (ADS)

    Dillon, Carolyn T.

    In an effort to determine the therapeutic feasibility of DNA metallointercalators as potential anticancer drugs it is important to confirm that they are capable of targeting DNA in cancer cells or tumours - as is the intended purpose of their design. Microprobe synchrotron radiation X-ray fluorescence (micro-SRXRF) spectroscopy is an ideal technique for investigating the cellular uptake and distribution of metallointercalators. The technique is capable of submicron elemental imaging so that samples as small as individual cells (~10 μm diameter), and the features within them, can be resolved. Consequently, the technique can ascertain whether intracellular metallointercalators colocalise with DNA; namely, in the nucleus during interphase or at the chromosomes during middle prophase to late anaphase. Metals, such as those commonly incorporated into metallointercalators (e.g., Cr, Ni, Co, Pd, Pt, Ru, Rh), are often naturally present in negligible quantities in cancer cells. This fact, together with their higher atomic number, Z, makes them ideal for direct probing using hard X-ray microprobes (as discussed in Sect. 11.2). There is no need for the incorporation of fluorescent tracker dyes or radioactive labels into their chemical structure. This is advantageous since it is unknown whether such chemical modifications alter the uptake kinetics of the metallointercalator [1, 2].

  15. Contemporary X-ray electron-density studies using synchrotron radiation

    PubMed Central

    Jørgensen, Mads R. V.; Hathwar, Venkatesha R.; Bindzus, Niels; Wahlberg, Nanna; Chen, Yu-Sheng; Overgaard, Jacob; Iversen, Bo B.

    2014-01-01

    Synchrotron radiation has many compelling advantages over conventional radiation sources in the measurement of accurate Bragg diffraction data. The variable photon energy and much higher flux may help to minimize critical systematic effects such as absorption, extinction and anomalous scattering. Based on a survey of selected published results from the last decade, the benefits of using synchrotron radiation in the determination of X-ray electron densities are discussed, and possible future directions of this field are examined. PMID:25295169

  16. Low-dose phase-based X-ray imaging techniques for in situ soft tissue engineering assessments.

    PubMed

    Izadifar, Zohreh; Honaramooz, Ali; Wiebe, Sheldon; Belev, George; Chen, Xiongbiao; Chapman, Dean

    2016-03-01

    In tissue engineering, non-invasive imaging of biomaterial scaffolds and tissues in living systems is essential to longitudinal animal studies for assessments without interrupting the repair process. Conventional X-ray imaging is inadequate for use in soft tissue engineering due to the limited absorption difference between the soft tissue and biomaterial scaffolds. X-ray phase-based imaging techniques that derive contrast from refraction or phase effects rather than absorption can provide the necessary contrast to see low-density biomaterial scaffolds and tissues in large living systems. This paper explores and compares three synchrotron phase-based X-ray imaging techniques-computed tomography (CT)-diffraction enhanced imaging (DEI), -analyzer based imaging (ABI), and -phase contrast imaging (PCI)-for visualization and characterization of low-density biomaterial scaffolds and tissues in situ for non-invasive soft tissue engineering assessments. Intact pig joints implanted with polycaprolactone scaffolds were used as the model to assess and compare the imaging techniques in terms of different qualitative and quantitative criteria. For long-term in vivo live animal imaging, different strategies for reducing the imaging radiation dose and scan time-reduced number of CT projections, region of interest, and low resolution imaging-were examined with the presented phase-based imaging techniques. The results demonstrated promising capabilities of the phase-based techniques for visualization of biomaterial scaffolds and soft tissues in situ. The low-dose imaging strategies were illustrated effective for reducing the radiation dose to levels appropriate for live animal imaging. The comparison among the imaging techniques suggested that CT-DEI has the highest efficiency in retaining image contrast at considerably low radiation doses.

  17. X-ray fluorescence spectrometry for high throughput analysis of atmospheric aerosol samples: The benefits of synchrotron X-rays

    NASA Astrophysics Data System (ADS)

    Bukowiecki, Nicolas; Lienemann, Peter; Zwicky, Christoph N.; Furger, Markus; Richard, Agnes; Falkenberg, Gerald; Rickers, Karen; Grolimund, Daniel; Borca, Camelia; Hill, Matthias; Gehrig, Robert; Baltensperger, Urs

    2008-09-01

    The determination of trace element mass concentrations in ambient air with a time resolution higher than one day represents an urgent need in atmospheric research. It involves the application of a specific technique both for the aerosol sampling and the subsequent analysis of the collected particles. Beside the intrinsic sensitivity of the analytical method, the sampling interval and thus the quantity of collected material that is available for subsequent analysis is a major factor driving the overall trace element detection power. This is demonstrated for synchrotron radiation X-ray fluorescence spectrometry (SR-XRF) of aerosol samples collected with a rotating drum impactor (RDI) in hourly intervals and three particle size ranges. The total aerosol mass on the 1-h samples is in the range of 10 µg. An experimental detection of the nanogram amounts of trace elements with the help of synchrotron X-rays was only achievable by the design of a fit-for-purpose sample holder system, which considered the boundary conditions both from particle sampling and analysis. A 6-µm polypropylene substrate film has evolved as substrate of choice, due to its practical applicability during sampling and its suitable spectroscopic behavior. In contrast to monochromatic excitation conditions, the application of a 'white' beam led to a better spectral signal-to-background ratio. Despite the low sample mass, a counting time of less than 30 s per 1-h aerosol sample led to sufficient counting statistics. Therefore the RDI-SR-XRF method represents a high-throughput analysis procedure without the need for any sample preparation. The analysis of a multielemental mass standard film by SR-XRF, laboratory-based wavelength-dispersive XRF spectrometry and laboratory-based micro XRF spectrometry showed that the laboratory-based methods were no alternatives to the SR-XRF method with respect to sensitivity and efficiency of analysis.

  18. Design of a miniature flow cell for in situ x-ray imaging of redox flow batteries

    NASA Astrophysics Data System (ADS)

    Jervis, Rhodri; Brown, Leon D.; Neville, Tobias P.; Millichamp, Jason; Finegan, Donal P.; Heenan, Thomas M. M.; Brett, Dan J. L.; Shearing, Paul R.

    2016-11-01

    Flow batteries represent a possible grid-scale energy storage solution, having many advantages such as scalability, separation of power and energy capabilities, and simple operation. However, they can suffer from degradation during operation and the characteristics of the felt electrodes are little understood in terms of wetting, compression and pressure drops. Presented here is the design of a miniature flow cell that allows the use of x-ray computed tomography (CT) to study carbon felt materials in situ and operando, in both lab-based and synchrotron CT. Through application of the bespoke cell it is possible to observe felt fibres, electrolyte and pore phases and therefore enables non-destructive characterisation of an array of microstructural parameters during the operation of flow batteries. Furthermore, we expect this design can be readily adapted to the study of other electrochemical systems.

  19. Versatile plug flow catalytic cell for in situ transmission/fluorescence x-ray absorption fine structure measurements

    NASA Astrophysics Data System (ADS)

    Centomo, P.; Meneghini, C.; Zecca, M.

    2013-05-01

    A novel flow-through catalytic cell has been developed for in situ x-ray absorption spectroscopy (XAS) experiments on heterogeneous catalysts under working conditions and in the presence of a liquid and a gas phase. The apparatus allows to carry out XAS measurements in both the transmission and fluorescence modes, at moderate temperature (from RT to 50-80 °C) and low-medium gas pressure (up to 7-8 bars). The materials employed are compatible with several chemicals such as those involved in the direct synthesis of hydrogen peroxide (O2, H2, H2O2, methanol). The versatile design of the cell allows to fit it to different experimental setups in synchrotron radiation beamlines. It was used successfully for the first time to test nanostructured Pd catalysts during the direct synthesis of hydrogen peroxide (H2O2) in methanol solution from dihydrogen and dioxygen.

  20. Comparison of synchrotron x-ray microanalysis with electron and proton microscopy for individual particle analysis

    SciTech Connect

    Janssens, K.H.; van Langevelde, F.; Adams, F.C.; Vis, R.D.; Sutton, S.R.; Rivers, M.L.; Jones, K.W.; Bowen, D.K.

    1991-12-31

    This paper is concerned with the evaluation of the use of synchrotron/radiation induced x-ray fluorescences ({mu}-SRXRF) as implemented at two existing X-ray microprobes for the analysis of individual particles. As representative environmental particulates, National Institutes of Science and Technology (NIST) K227, K309, K441 and K961 glass microspheres were analyzed using two types of X-ray micro probes: the white light microprobe at beamline X26A of the monochromatic (15 keV) X-ray microprobe at station 7.6 of the SRS. For reference, the particles were also analyzed with microanalytical techniques more commonly employed for individual particles analysis such as EPMA and micro-PIXE.

  1. Comparison of synchrotron x-ray microanalysis with electron and proton microscopy for individual particle analysis

    SciTech Connect

    Janssens, K.H.; van Langevelde, F.; Adams, F.C. ); Vis, R.D. ); Sutton, S.R.; Rivers, M.L. ); Jones, K.W. ); Bowen, D.K. )

    1991-01-01

    This paper is concerned with the evaluation of the use of synchrotron/radiation induced x-ray fluorescences ({mu}-SRXRF) as implemented at two existing X-ray microprobes for the analysis of individual particles. As representative environmental particulates, National Institutes of Science and Technology (NIST) K227, K309, K441 and K961 glass microspheres were analyzed using two types of X-ray micro probes: the white light microprobe at beamline X26A of the monochromatic (15 keV) X-ray microprobe at station 7.6 of the SRS. For reference, the particles were also analyzed with microanalytical techniques more commonly employed for individual particles analysis such as EPMA and micro-PIXE.

  2. Initial feasibility study of a dedicated synchrotron radiation light source for ultrafast X-ray science

    SciTech Connect

    Corlett, John N.; DeSantis, S.; Hartman, N.; Heimann, P.; LaFever, R.; Li, D.; Padmore, H.; Rimmer, R.; Robinson, K.; Schoenlein, R.; Tanabe, J.; Wang, S.; Zholents, A.; Kairan, D.

    2001-10-26

    We present an initial feasibility summary of a femtosecond synchrotron radiation x-ray source based on a flat-beam rf gun and a recirculating superconducting linac that provides beam to an array of undulators and bend magnets. Optical pulse durations of < 100 fs are obtained by a combination of electron pulse compression, transverse temporal correlation of the electrons, and x-ray pulse compression. After an introduction and initial scientific motivation, we cover the following aspects of the design: layout and lattice, ultra-fast x-ray pulse production, flat electron-beam production, the rf gun, rf systems, cryogenic systems, collective effects, photon production, and synchronization of x-ray and laser pulses. We conclude with a summary of issues and areas of development that remain to be addressed.

  3. On diamond windows for high power synchrotron x-ray beams

    SciTech Connect

    Khounsary, A.M.; Kuzay, T.M.

    1991-01-01

    Recent advances in chemical vapor deposition (CVD) technology has made available thin, free-standing polycrystalline diamond foils that can be used as the window material on high heat load synchrotron x-ray beamlines. Diamond windows have many advantages that stem from the exceptionally attractive thermal, structural, and physical properties of diamond. Numerical simulations indicate that diamond windows can offer an attractive and at times the only alternative to beryllium windows for use on the third generation x-ray synchrotron radiation beamlines. Utilization, design, and fabrication aspects of diamond windows for high heat load x-ray beamlines are discussed, and analytical and numerical results are presented to provide a basis for the design and testing of such windows.

  4. On diamond windows for high power synchrotron x-ray beams

    SciTech Connect

    Khounsary, A.M.; Kuzay, T.M.

    1991-12-31

    Recent advances in chemical vapor deposition (CVD) technology has made available thin, free-standing polycrystalline diamond foils that can be used as the window material on high heat load synchrotron x-ray beamlines. Diamond windows have many advantages that stem from the exceptionally attractive thermal, structural, and physical properties of diamond. Numerical simulations indicate that diamond windows can offer an attractive and at times the only alternative to beryllium windows for use on the third generation x-ray synchrotron radiation beamlines. Utilization, design, and fabrication aspects of diamond windows for high heat load x-ray beamlines are discussed, and analytical and numerical results are presented to provide a basis for the design and testing of such windows.

  5. Biomedical elemental analysis and imaging using synchrotron x-ray microscopy

    SciTech Connect

    Jones, K.W.; Gordon, B.M.; Schidlovsky, G.; Spanne, P.; Dejun, Xue ); Bockman, R.S. ); Saubermann, A.J. . Health Science Center)

    1990-01-01

    The application of synchrotron x-ray microscopy to biomedical research is currently in progress at the Brookhaven National Synchrotron Light Source (NSLS). The current status of the x-ray microscope (XRM) is reviewed from a technical standpoint. Some of the items considered are photon flux, spatial resolution, quantitation, minimum detection limits, and beam-induced specimen damage. Images can be produced by measurement of fluorescent x rays or of the attenuation of the incident beam by the specimen. Maps of the elemental distributions or linear attenuation of the incident beam by the specimen. Maps of the elemental distributions or linear attenuation coefficients can be made by scanning the specimen past the beam. Computed microtomography (CMT) can be used for non- destructive images through the specimen in either the emission or absorption mode. Examples of measurements made with the XRM are given.

  6. Fabrication of nested elliptical KB mirrors using profile coating for synchrotron radiation X-ray focusing

    SciTech Connect

    Liu, Chian; Ice, Gene E; Liu, Wenjun; Assoufid, Lahsen; Qian, J; Shi, B.; Khachatryan, Ruben; Wieczorek, M.; Zschack, P.; Tischler, Jonathan Zachary

    2012-01-01

    This paper describes fabrication methods used to demonstrate the advantages of nested or Montel optics for micro/nanofocusing of synchrotron X-ray beams. A standard Kirkpatrick-Baez (KB) mirror system uses two separated elliptical mirrors at glancing angles to the X-ray beam and sequentially arranged at 90{sup o} to each other to focus X-rays successively in the vertical and horizontal directions. A nested KB mirror system has the two mirrors positioned perpendicular and side-by-side to each other. Compared to a standard KB mirror system, Montel optics can focus a larger divergence and the mirrors can have a shorter focal length. As a result, nested mirrors can be fabricated with improved demagnification factor and ultimately smaller focal spot, than with a standard KB arrangement. The nested system is also more compact with an increased working distance, and is more stable, with reduced complexity of mirror stages. However, although Montel optics is commercially available for laboratory X-ray sources, due to technical difficulties they have not been used to microfocus synchrotron radiation X-rays, where ultra-precise mirror surfaces are essential. The main challenge in adapting nested optics for synchrotron microfocusing is to fabricate mirrors with a precise elliptical surface profile at the very edge where the two mirrors meet and where X-rays scatter. For example, in our application to achieve a sub-micron focus with high efficiency, a surface figure root-mean-square (rms) error on the order of 1 nm is required in the useable area along the X-ray footprint with a {approx} 0.1 mm-diameter cross section. In this paper we describe promising ways to fabricate precise nested KB mirrors using our profile coating technique and inexpensive flat Si substrates.

  7. Synchrotron-based transmission x-ray microscopy for improved extraction in shale during hydraulic fracturing

    NASA Astrophysics Data System (ADS)

    Kiss, Andrew M.; Jew, Adam D.; Joe-Wong, Claresta; Maher, Kate M.; Liu, Yijin; Brown, Gordon E.; Bargar, John

    2015-09-01

    Engineering topics which span a range of length and time scales present a unique challenge to researchers. Hydraulic fracturing (fracking) of oil shales is one of these challenges and provides an opportunity to use multiple research tools to thoroughly investigate a topic. Currently, the extraction efficiency from the shale is low but can be improved by carefully studying the processes at the micro- and nano-scale. Fracking fluid induces chemical changes in the shale which can have significant effects on the microstructure morphology, permeability, and chemical composition. These phenomena occur at different length and time scales which require different instrumentation to properly study. Using synchrotron-based techniques such as fluorescence tomography provide high sensitivity elemental mapping and an in situ micro-tomography system records morphological changes with time. In addition, the transmission X-ray microscope (TXM) at the Stanford Synchrotron Radiation Lightsource (SSRL) beamline 6-2 is utilized to collect a nano-scale three-dimensional representation of the sample morphology with elemental and chemical sensitivity. We present the study of a simplified model system, in which pyrite and quartz particles are mixed and exposed to oxidizing solution, to establish the basic understanding of the more complex geology-relevant oxidation reaction. The spatial distribution of the production of the oxidation reaction, ferrihydrite, is retrieved via full-field XANES tomography showing the reaction pathway. Further correlation between the high resolution TXM data and the high sensitivity micro-probe data provides insight into potential morphology changes which can decrease permeability and limit hydrocarbon recovery.

  8. Atomic physics with hard X-rays from high brilliance synchrotron light sources

    SciTech Connect

    Southworth, S.; Gemmell, D.

    1996-08-01

    A century after the discovery of x rays, the experimental capability for studying atomic structure and dynamics with hard, bright synchrotron radiation is increasing remarkably. Tempting opportunities arise for experiments on many-body effects, aspects of fundamental photon-atom interaction processes, and relativistic and quantum-electrodynamic phenomena. Some of these possibilities are surveyed in general terms.

  9. 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

  10. Variable magnification with Kirkpatrick-Baez optics for synchrotron X-ray microscopy

    DOE PAGES

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

    2006-05-01

    In this study, 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 (Kohler illumination).

  11. A new miniature microchannel plate X-ray detector for synchrotron radiation

    NASA Astrophysics Data System (ADS)

    Rosemeier, Ronald G.; Green, Robert E.

    A state-of-the-art microchannel plate detector has been developed which allows real time X-ray imagin of X-ray diffraction as well as a radiographic phenomenon. Advantages of the device include a 50 mm X-ray input, length less than 4″, and a weight of less than 1 lb. Since the use of synchrotron radiation is greatly facilitated by the capability of remote viewing of X-ray diffraction or radiographic images in real time, a prototype electro-optical system has been designed which couples the X-ray microchannel plate detector with a solid state television camera. Advantages of the miniature, lightweight, X-ray synchroton camera include a large 50 mm X-ray input window, an output signal that is available in both analog format for display on a television monitor and in digital format for computer processing, and a completely modular design which allows all the components to be exchanged for other components optimally suited for the desired applications.

  12. X-ray photonic microsystems for the manipulation of synchrotron light

    PubMed Central

    Mukhopadhyay, D.; Walko, D. A.; Jung, I. W.; Schwartz, C. P.; Wang, Jin; López, D.; Shenoy, G. K.

    2015-01-01

    Photonic microsystems played an essential role in the development of integrated photonic devices, thanks to their unique spatiotemporal control and spectral shaping capabilities. Similar capabilities to markedly control and manipulate X-ray radiation are highly desirable but practically impossible due to the massive size of the silicon single-crystal optics currently used. Here we show that micromechanical systems can be used as X-ray optics to create and preserve the spatial, temporal and spectral correlation of the X-rays. We demonstrate that, as X-ray reflective optics they can maintain the wavefront properties with nearly 100% reflectivity, and as a dynamic diffractive optics they can generate nanosecond time windows with over 100-kHz repetition rates. Since X-ray photonic microsystems can be easily incorporated into lab-based and next-generation synchrotron X-ray sources, they bring unprecedented design flexibility for future dynamic and miniature X-ray optics for focusing, wavefront manipulation, multicolour dispersion, and pulse slicing. PMID:25940542

  13. X-ray photonic microsystems for the manipulation of synchrotron light

    DOE PAGES

    Mukhopadhyay, D.; Walko, D. A.; Jung, I. W.; Schwartz, C. P.; Wang, Jin; López, D.; Shenoy, G. K.

    2015-05-05

    In this study, photonic microsystems played an essential role in the development of integrated photonic devices, thanks to their unique spatiotemporal control and spectral shaping capabilities. Similar capabilities to markedly control and manipulate X-ray radiation are highly desirable but practically impossible due to the massive size of the silicon single-crystal optics currently used. Here we show that micromechanical systems can be used as X-ray optics to create and preserve the spatial, temporal and spectral correlation of the X-rays. We demonstrate that, as X-ray reflective optics they can maintain the wavefront properties with nearly 100% reflectivity, and as a dynamic diffractivemore » optics they can generate nanosecond time windows with over 100-kHz repetition rates. Since X-ray photonic microsystems can be easily incorporated into lab-based and next-generation synchrotron X-ray sources, they bring unprecedented design flexibility for future dynamic and miniature X-ray optics for focusing, wavefront manipulation, multicolour dispersion, and pulse slicing.« less

  14. X-ray photonic microsystems for the manipulation of synchrotron light

    SciTech Connect

    Mukhopadhyay, D.; Walko, D. A.; Jung, I. W.; Schwartz, C. P.; Wang, Jin; López, D.; Shenoy, G. K.

    2015-05-05

    In this study, photonic microsystems played an essential role in the development of integrated photonic devices, thanks to their unique spatiotemporal control and spectral shaping capabilities. Similar capabilities to markedly control and manipulate X-ray radiation are highly desirable but practically impossible due to the massive size of the silicon single-crystal optics currently used. Here we show that micromechanical systems can be used as X-ray optics to create and preserve the spatial, temporal and spectral correlation of the X-rays. We demonstrate that, as X-ray reflective optics they can maintain the wavefront properties with nearly 100% reflectivity, and as a dynamic diffractive optics they can generate nanosecond time windows with over 100-kHz repetition rates. Since X-ray photonic microsystems can be easily incorporated into lab-based and next-generation synchrotron X-ray sources, they bring unprecedented design flexibility for future dynamic and miniature X-ray optics for focusing, wavefront manipulation, multicolour dispersion, and pulse slicing.

  15. Mapping and load response of overload strain fields: Synchrotron X-ray measurements

    SciTech Connect

    Shukla, V; Jisrawi, N M; Sadangi, R K; Pao, P S; Horvath, K; Sadananda, K; Ignatov, A; Skaritka, J; Tsakalakos, T

    2009-02-05

    High energy synchrotron X-ray diffraction measurements have been performed to provide quantitative microscopic guidance for modeling of fatigue crack growth. Specifically we report local strain mapping, along with in situ loading strain response, results on 4140 steel fatigue specimens exhibiting the crack growth retardation 'overload effect'. Detailed, 2D, {epsilon}{gamma}{gamma}-strain field mapping shows that a single overload (OL) cycle creates a compressive strain field extending millimeters above and below the crack plane. The OL strain field structures are shown to persist after the crack tip has grown well beyond the OL position. The specimen exhibiting the maximal crack growth rate retardation following overload exhibits a tensile residual strain region at the crack tip. Strain field results, on in situ tensile loaded specimens, show a striking critical threshold load, F{sub c}, phenomenon in their strain response. At loads below F{sub c} the strain response is dominated by a rapid suppression of the compressive OL feature with modest response at the crack tip. At loads above F{sub c} the strain response at the OL position terminates and the response at the crack tip becomes large. This threshold load response behavior is shown to exhibit lower F{sub c} values, and dramatically enhanced rates of strain change with load as the crack tip propagates farther beyond the OL position. The OL strain feature behind the crack tip also is shown to be suppressed by removing the opposing crack faces via an electron discharge cut passing through the crack tip. Finally unique 2D strain field mapping (imaging) results, through the depth of the specimen, of the fatigue crack front and the OL feature in the wake are also presented.

  16. X-ray fluorescence spectrometry using Synchrotron Radiation with applications in unmanned aircraft environmental sensing

    NASA Astrophysics Data System (ADS)

    Barberie, Sean Richard Gopal

    In this thesis I present an analytical optimization of the Synchrotron Radiation X-Ray Fluorescence (SR-XRF) technique for applications in unmanned aircraft aerosol studies. In environmental and atmospheric science, there is a pressing need for aerosol measurements at various altitudes in the atmosphere and spanning large regions. This need is currently either ignored, or met to a limited degree by studies that employ manned aircraft. There is, however, a great deal of opportunity to improve and expand on these studies using the emerging technology of unmanned aircraft systems. A newly developed aerosol sampler makes this opportunity a near-reality by its ability to collect aerosol samples in-situ from unmanned aircraft platforms. The challenge lies in analyzing these samples for elemental composition. In airborne aerosol studies, the ability to resolve where a sample was collected both spatially and temporally is limited by the sensitivity of the analysis technique. In aircraft-based aerosol collection, the length of the aerosol sample spot corresponds to distance. Thus the spatial resolution of an airborne study is limited by the amount of mass that must be collected for analysis. The SR-XRF optimizations outlined in this thesis decrease the amount of sample mass required for detectable elemental concentrations, allowing aerosol samples to be analyzed in smaller areas corresponding to smaller time steps. Since, in a flight path, time steps are directly correlated with distance, analysis of smaller time steps results in the ability to measure aerosols at higher spatial resolution. Four SR-XRF analysis configurations were experimentally tested: monochromatic beam, white beam, filtered white beam, and filtered white beam-filtered detector to determine which configuration gave the highest elemental sensitivity and selectivity. Of these tested methods, the straight polychromatic white beam configuration resulted in the best sensitivity for elements across a large

  17. Strategies for in situ laser heating in the diamond anvil cell at an X-ray diffraction beamline.

    PubMed

    Petitgirard, Sylvain; Salamat, Ashkan; Beck, Pierre; Weck, Gunnar; Bouvier, Pierre

    2014-01-01

    An overview of several innovations regarding in situ laser-heating techniques in the diamond anvil cell at the high-pressure beamline ID27 of the European Synchrotron Radiation Facility is presented. Pyrometry measurements have been adapted to allow simultaneous double-sided temperature measurements with the installation of two additional online laser systems: a CO2 and a pulsed Nd:YAG laser system. This reiteration of laser-heating advancements at ID27 is designed to pave the way for a new generation of state-of-the-art experiments that demand the need for synchrotron diffraction techniques. Experimental examples are provided for each major development. The capabilities of the double pyrometer have been tested with the Nd:YAG continuous-wave lasers but also in a time-resolved configuration using the nanosecond-pulsed Nd:YAG laser on a Fe sample up to 180 GPa and 2900 K. The combination of time-resolved X-ray diffraction with in situ CO2 laser heating is shown with the crystallization of a high-pressure phase of the naturally found pyrite mineral MnS2 (11 GPa, 1100-1650 K). PMID:24365921

  18. A sample chamber for in situ high-energy X-ray studies of crystal growth at deeply buried interfaces in harsh environments

    NASA Astrophysics Data System (ADS)

    de Jong, A. E. F.; Vonk, V.; Honkimäki, V.; Gorges, B.; Vitoux, H.; Vlieg, E.

    2015-06-01

    We introduce a high pressure high temperature chamber for in situ synchrotron X-ray studies. The chamber design allows for in situ studies of thin film growth from solution at deeply buried interfaces in harsh environments. The temperature can be controlled between room temperature and 1073 K while the pressure can be set as high as 50 bar using a variety of gases including N2 and NH3. The formation of GaN on the surface of a Ga13Na7 melt at 1073 K and 50 bar of N2 is presented as a performance test.

  19. Portable apparatus for in situ x-ray diffraction and fluorescence analyses of artworks.

    PubMed

    Eveno, Myriam; Moignard, Brice; Castaing, Jacques

    2011-10-01

    A portable X-ray fluorescence/X-ray diffraction (XRF/XRD) system for artwork studies has been designed constructed and tested. It is based on Debye Scherrer XRD in reflection that takes advantage of many recent improvements in the handling of X-rays (polycapillary optics; advanced two-dimensional detection). The apparatus is based on a copper anode air cooled X-ray source, and the XRD analysis is performed on a 5-20 μm thick layer from the object surface. Energy dispersive XRF elemental analysis can be performed at the same point as XRD, giving elemental compositions that support the interpretation of XRD diagrams. XRF and XRD analyses were tested to explore the quality and the limits of the analytical technique. The XRD diagrams are comparable in quality with diagrams obtained with conventional laboratory equipment. The mineral identification of materials in artwork is routinely performed with the portable XRF-XRD system. Examples are given for ceramic glazes containing crystals and for paintings where the determination of pigments is still a challenge for nondestructive analysis. For instance, lead compounds that provide a variety of color pigments can be easily identified as well as a pigment such as lapis lazuli that is difficult to identify by XRF alone. More than 70 works of art have been studied in situ in museums, monuments, etc. In addition to ceramics and paintings, these works include bronzes, manuscripts, etc., which permit improvement in the comprehension of ancient artistic techniques. PMID:21615981

  20. Portable apparatus for in situ x-ray diffraction and fluorescence analyses of artworks.

    PubMed

    Eveno, Myriam; Moignard, Brice; Castaing, Jacques

    2011-10-01

    A portable X-ray fluorescence/X-ray diffraction (XRF/XRD) system for artwork studies has been designed constructed and tested. It is based on Debye Scherrer XRD in reflection that takes advantage of many recent improvements in the handling of X-rays (polycapillary optics; advanced two-dimensional detection). The apparatus is based on a copper anode air cooled X-ray source, and the XRD analysis is performed on a 5-20 μm thick layer from the object surface. Energy dispersive XRF elemental analysis can be performed at the same point as XRD, giving elemental compositions that support the interpretation of XRD diagrams. XRF and XRD analyses were tested to explore the quality and the limits of the analytical technique. The XRD diagrams are comparable in quality with diagrams obtained with conventional laboratory equipment. The mineral identification of materials in artwork is routinely performed with the portable XRF-XRD system. Examples are given for ceramic glazes containing crystals and for paintings where the determination of pigments is still a challenge for nondestructive analysis. For instance, lead compounds that provide a variety of color pigments can be easily identified as well as a pigment such as lapis lazuli that is difficult to identify by XRF alone. More than 70 works of art have been studied in situ in museums, monuments, etc. In addition to ceramics and paintings, these works include bronzes, manuscripts, etc., which permit improvement in the comprehension of ancient artistic techniques.

  1. Real world issues for the new soft x-ray synchrotron sources

    SciTech Connect

    Kincaid, B.M.

    1991-05-01

    A new generation of synchrotron radiation light sources covering the VUV, soft x-ray and hard x-ray spectral regions is under construction in several countries. They are designed specifically to use periodic magnetic undulators and low-emittance electron or positron beams to produce high-brightness near-diffraction-limited synchrotron radiation beams. An introduction to the properties of undulator radiation is followed by a discussion of some of the challenges to be faced at the new facilities. Examples of predicted undulator output from the Advanced Light Source, a third generation 1--2 GeV storage ring optimized for undulator use, are used to highlight differences from present synchrotron radiation sources, including high beam power, partial coherence, harmonics, and other unusual spectral and angular properties of undulator radiation. 8 refs., 2 figs.

  2. On the Correlation Between Fatigue Striation Spacing and Crack Growth Rate: A Three-Dimensional (3-D) X-ray Synchrotron Tomography Study

    NASA Astrophysics Data System (ADS)

    Williams, Jason J.; Yazzie, Kyle E.; Connor Phillips, N.; Chawla, Nikhilesh; Xiao, Xinghui; de Carlo, Francesco; Iyyer, Nagaraja; Kittur, Maddan

    2011-12-01

    In situ three-dimensional (3-D) X-ray synchrotron tomography of fatigue crack growth was conducted in a 7075-T6 aluminum alloy. Local measurements of da/ dN were possible with the 3-D data sets obtained from tomography. A comparison with fatigue striation spacings obtained from scanning electron microscopy of the fracture surfaces yielded excellent correlation with da/ dN obtained from tomography. The X-ray tomography technique can be used to obtain a highly accurate and representative measurements of crack growth locally in the microstructure of the material.

  3. Soil characterization by energy dispersive X-ray fluorescence: sampling strategy for in situ analysis.

    PubMed

    Custo, Graciela; Boeykens, Susana; Dawidowski, L; Fox, L; Gómez, D; Luna, F; Vázquez, Cristina

    2005-07-01

    This work describes a sampling strategy that will allow the use of portable EDXRF (energy dispersive X-ray fluorescence) instruments for "in situ" soil analysis. The methodology covers a general approach to planning field investigations for any type of environmental studies and it was applied for a soil characterization study in the zone of Campana, Argentina, by evaluating data coming from an EDXRF spectrometer with a radioisotope excitation source. Simulating non-treated sampled as "in situ" samples and a soil characterization for Campana area was intended. "In situ" EDXRF methodology is a powerful analytical modality with the advantage of providing data immediately, allowing a fast general screening of the soil composition. PMID:16038489

  4. Microscopic x-ray imaging system for biomedical applications using synchrotron radiation

    NASA Astrophysics Data System (ADS)

    Umetani, Keiji; Kobatake, Makito; Yamamoto, Akira; Yamashita, Takenori; Imai, Shigeki

    2007-02-01

    An X-ray direct-conversion type detector with a spatial resolution of 10-11 μm was developed for real-time biomedical imaging. The detector incorporates the X-ray SATICON pickup tube with a photoconductive target layer of amorphous selenium. For high-resolution imaging, the X-ray image is directly converted into an electric signal in the photoconductive layer without image blur. Microangiography experiments were carried out for depicting angiogenic vessels in a rabbit model of cancer using the direct-conversion detector and a third generation synchrotron radiation source at SPring-8. In synchrotron radiation radiography, a long source-to-object distance and a small source spot can produce high-resolution images. After transplantation of cancer cells into the rabbit auricle, small tumor blood vessels with diameters of 20-30 μm in an immature vascular network produced by angiogenesis were visualized by contrast material injection into the auricular artery at a monochromatic X-ray energy of 33.2 keV just above the iodine K-edge energy. The synchrotron radiation system is a useful tool to evaluate the micro-angioarchitecture of malignant tumors in animal models of cancer for in vivo preclinical studies.

  5. Synchrotron-based Scattered Radiation from Phantom Materials used in X-ray CT

    SciTech Connect

    Rao, D.; Swapna, M; Cesareo, R; Brunetti, A; Akatsuka, T; Yuasa, T; Takeda, T; Gigante, G

    2010-01-01

    Synchrotron-based scattered radiation form low-contrast phantom materials prepared from polyethylene, polystyrene, nylon, and Plexiglas is used as test objects in X-ray CT was examined with 8, 10 and 12 keV X-rays. These phantom materials of medical interest will contains varying proportions of low atomic number elements. The assessment will allowed us to estimate the fluorescence to total scattered radiation. Detected the fluorescence spectra and the associated scattered radiation from calcium hydroxyapatite phantom with 8, 10 and 12 keV synchrotron X-rays. Samples with Bonefil (60% and 70% of calcium hydroxyapatite) and Bone cream (35-45% of calcium hydroxyapatite), were used. Utilized the X-ray micro-spectroscopy beamline facility, X27A, available at NSLS, BNL, USA. The primary beam with a spot size of the order of {approx}10 {micro}m, has been used for focusing. With this spatial resolution and high flux throuput, the synchrotron-based scattered radiation from the phantom materials were measured using a liquid-nitrogen-cooled 13-element energy-dispersive high-purity germanium detector.

  6. Aerodynamic levitator for in situ x-ray structure measurements on high temperature and molten nuclear fuel materials.

    PubMed

    Weber, J K R; Tamalonis, A; Benmore, C J; Alderman, O L G; Sendelbach, S; Hebden, A; Williamson, M A

    2016-07-01

    An aerodynamic levitator with carbon dioxide laser beam heating was integrated with a hermetically sealed controlled atmosphere chamber and sample handling mechanism. The system enabled containment of radioactive samples and control of the process atmosphere chemistry. The chamber was typically operated at a pressure of approximately 0.9 bars to ensure containment of the materials being processed. Samples 2.5-3 mm in diameter were levitated in flowing gas to achieve containerless conditions. Levitated samples were heated to temperatures of up to 3500 °C with a partially focused carbon dioxide laser beam. Sample temperature was measured using an optical pyrometer. The sample environment was integrated with a high energy (100 keV) x-ray synchrotron beamline to enable in situ structure measurements to be made on levitated samples as they were heated, melted, and supercooled. The system was controlled from outside the x-ray beamline hutch by using a LabVIEW program. Measurements have been made on hot solid and molten uranium dioxide and binary uranium dioxide-zirconium dioxide compositions. PMID:27475566

  7. Aerodynamic levitator for in situ x-ray structure measurements on high temperature and molten nuclear fuel materials.

    PubMed

    Weber, J K R; Tamalonis, A; Benmore, C J; Alderman, O L G; Sendelbach, S; Hebden, A; Williamson, M A

    2016-07-01

    An aerodynamic levitator with carbon dioxide laser beam heating was integrated with a hermetically sealed controlled atmosphere chamber and sample handling mechanism. The system enabled containment of radioactive samples and control of the process atmosphere chemistry. The chamber was typically operated at a pressure of approximately 0.9 bars to ensure containment of the materials being processed. Samples 2.5-3 mm in diameter were levitated in flowing gas to achieve containerless conditions. Levitated samples were heated to temperatures of up to 3500 °C with a partially focused carbon dioxide laser beam. Sample temperature was measured using an optical pyrometer. The sample environment was integrated with a high energy (100 keV) x-ray synchrotron beamline to enable in situ structure measurements to be made on levitated samples as they were heated, melted, and supercooled. The system was controlled from outside the x-ray beamline hutch by using a LabVIEW program. Measurements have been made on hot solid and molten uranium dioxide and binary uranium dioxide-zirconium dioxide compositions.

  8. Aerodynamic levitator for in situ x-ray structure measurements on high temperature and molten nuclear fuel materials

    NASA Astrophysics Data System (ADS)

    Weber, J. K. R.; Tamalonis, A.; Benmore, C. J.; Alderman, O. L. G.; Sendelbach, S.; Hebden, A.; Williamson, M. A.

    2016-07-01

    An aerodynamic levitator with carbon dioxide laser beam heating was integrated with a hermetically sealed controlled atmosphere chamber and sample handling mechanism. The system enabled containment of radioactive samples and control of the process atmosphere chemistry. The chamber was typically operated at a pressure of approximately 0.9 bars to ensure containment of the materials being processed. Samples 2.5-3 mm in diameter were levitated in flowing gas to achieve containerless conditions. Levitated samples were heated to temperatures of up to 3500 °C with a partially focused carbon dioxide laser beam. Sample temperature was measured using an optical pyrometer. The sample environment was integrated with a high energy (100 keV) x-ray synchrotron beamline to enable in situ structure measurements to be made on levitated samples as they were heated, melted, and supercooled. The system was controlled from outside the x-ray beamline hutch by using a LabVIEW program. Measurements have been made on hot solid and molten uranium dioxide and binary uranium dioxide-zirconium dioxide compositions.

  9. Quick extended x-ray absorption fine structure instrument with millisecond time scale, optimized for in situ applications.

    PubMed

    Khalid, S; Caliebe, W; Siddons, P; So, I; Clay, B; Lenhard, T; Hanson, J; Wang, Q; Frenkel, A I; Marinkovic, N; Hould, N; Ginder-Vogel, M; Landrot, G L; Sparks, D L; Ganjoo, A

    2010-01-01

    In order to learn about in situ structural changes in materials at subseconds time scale, we have further refined the techniques of quick extended x-ray absorption fine structure (QEXAFS) and quick x-ray absorption near edge structure (XANES) spectroscopies at beamline X18B at the National Synchrotron Light Source. The channel cut Si (111) monochromator oscillation is driven through a tangential arm at 5 Hz, using a cam, dc motor, pulley, and belt system. The rubber belt between the motor and the cam damps the mechanical noise. EXAFS scan taken in 100 ms is comparable to standard data. The angle and the angular range of the monochromator can be changed to collect a full EXAFS or XANES spectrum in the energy range 4.7-40.0 KeV. The data are recorded in ascending and descending order of energy, on the fly, without any loss of beam time. The QEXAFS mechanical system is outside the vacuum system, and therefore changing the mode of operation from conventional to QEXAFS takes only a few minutes. This instrument allows the acquisition of time resolved data in a variety of systems relevant to electrochemical, photochemical, catalytic, materials, and environmental sciences.

  10. Energy Dependence of Synchrotron X-Ray Rims in Tycho's Supernova Remnant

    NASA Technical Reports Server (NTRS)

    Tran, Aaron; Williams, Brian J.; Petre, Robert; Ressler, Sean M.; Reynolds, Stephen P.

    2015-01-01

    Several young supernova remnants exhibit thin X-ray bright rims of synchrotron radiation at their forward shocks. Thin rims require strong magnetic field amplification beyond simple shock compression if rim widths are only limited by electron energy losses. But, magnetic field damping behind the shock could produce similarly thin rims with less extreme field amplification. Variation of rim width with energy may thus discriminate between competing influences on rim widths. We measured rim widths around Tycho's supernova remnant in 5 energy bands using an archival 750 ks Chandra observation. Rims narrow with increasing energy and are well described by either loss-limited or damped scenarios, so X-ray rim width-energy dependence does not uniquely specify a model. But, radio counterparts to thin rims are not loss-limited and better reflect magnetic field structure. Joint radio and X-ray modeling favors magnetic damping in Tycho's SNR with damping lengths approximately 1-5% of remnant radius and magnetic field strengths approximately 50-400 micron G assuming Bohm diffusion. X-ray rim widths are approximately 1% of remnant radius, somewhat smaller than inferred damping lengths. Electron energy losses are important in all models of X-ray rims, suggesting that the distinction between loss-limited and damped models is blurred in soft X-rays. All loss-limited and damping models require magnetic fields approximately greater than 20 micron G, arming the necessity of magnetic field amplification beyond simple compression.

  11. ENERGY DEPENDENCE OF SYNCHROTRON X-RAY RIMS IN TYCHO’S SUPERNOVA REMNANT

    SciTech Connect

    Tran, Aaron; Williams, Brian J.; Petre, Robert; Reynolds, Stephen P.

    2015-10-20

    Several young supernova remnants (SNRs) exhibit thin X-ray bright rims of synchrotron radiation at their forward shocks. Thin rims require strong magnetic field amplification beyond simple shock compression if rim widths are only limited by electron energy losses. But, magnetic field damping behind the shock could produce similarly thin rims with less extreme field amplification. Variation of rim width with energy may thus discriminate between competing influences on rim widths. We measured rim widths around Tycho's SNR in five energy bands using an archival 750 ks Chandra observation. Rims narrow with increasing energy and are well described by either loss-limited or damped scenarios, so X-ray rim width-energy dependence does not uniquely specify a model. But, radio counterparts to thin rims are not loss-limited and better reflect magnetic field structure. Joint radio and X-ray modeling favors magnetic damping in Tycho's SNR with damping lengths ∼1%–5% of remnant radius and magnetic field strengths ∼50–400 μG assuming Bohm diffusion. X-ray rim widths are ∼1% of remnant radius, somewhat smaller than inferred damping lengths. Electron energy losses are important in all models of X-ray rims, suggesting that the distinction between loss-limited and damped models is blurred in soft X-rays. All loss-limited and damping models require magnetic fields ≳20 μG, affirming the necessity of magnetic field amplification beyond simple compression.

  12. A furnace and environmental cell for the in situ investigation of molten salt electrolysis using high-energy X-ray diffraction.

    PubMed

    Styles, Mark J; Rowles, Matthew R; Madsen, Ian C; McGregor, Katherine; Urban, Andrew J; Snook, Graeme A; Scarlett, Nicola V Y; Riley, Daniel P

    2012-01-01

    This paper describes the design, construction and implementation of a relatively large controlled-atmosphere cell and furnace arrangement. The purpose of this equipment is to facilitate the in situ characterization of materials used in molten salt electrowinning cells, using high-energy X-ray scattering techniques such as synchrotron-based energy-dispersive X-ray diffraction. The applicability of this equipment is demonstrated by quantitative measurements of the phase composition of a model inert anode material, which were taken during an in situ study of an operational Fray-Farthing-Chen Cambridge electrowinning cell, featuring molten CaCl(2) as the electrolyte. The feasibility of adapting the cell design to investigate materials in other high-temperature environments is also discussed. PMID:22186642

  13. A furnace and environmental cell for the in situ investigation of molten salt electrolysis using high-energy X-ray diffraction.

    PubMed

    Styles, Mark J; Rowles, Matthew R; Madsen, Ian C; McGregor, Katherine; Urban, Andrew J; Snook, Graeme A; Scarlett, Nicola V Y; Riley, Daniel P

    2012-01-01

    This paper describes the design, construction and implementation of a relatively large controlled-atmosphere cell and furnace arrangement. The purpose of this equipment is to facilitate the in situ characterization of materials used in molten salt electrowinning cells, using high-energy X-ray scattering techniques such as synchrotron-based energy-dispersive X-ray diffraction. The applicability of this equipment is demonstrated by quantitative measurements of the phase composition of a model inert anode material, which were taken during an in situ study of an operational Fray-Farthing-Chen Cambridge electrowinning cell, featuring molten CaCl(2) as the electrolyte. The feasibility of adapting the cell design to investigate materials in other high-temperature environments is also discussed.

  14. Synchrotron X-ray Fluorescence Microtomography in Geo-, Cosmo-, and Bio- chemistry

    NASA Astrophysics Data System (ADS)

    Lanzirotti, A.; Sutton, S. R.; Rivers, M.; Tappero, R.

    2009-05-01

    Synchrotron-based X-ray fluorescence computed microtomography (xrfCMT) is a unique method for imaging major and trace element distributions within natural materials nondestructively and with high spatial resolution. The technique is particularly useful in imaging and quantifying elemental abundance in small objects that may be too precious or too difficult to section, or in the analysis of materials in which sectioning may potentially alter elemental distributions. This presentation will highlight how this technique is being applied at beamlines X26A and X27A at the National Synchrotron Light Source (Brookhaven National Laboratory) and at 13-ID at the Advanced Photon Source (Argonne National Laboratory). These instruments utilize 1-10 μm diameter focused, monochromatic X-ray beams to non- destructively measure x-ray fluorescence from a sample as it is translated and rotated within the beam. The resultant fluorescence intensities are then reconstructed as either two-dimensional cross sectional or three- dimensional elemental distribution using a fast fourier transform based computational reconstruction algorithm. Reconstruction of multi-elemental distributions at concentrations down to approximately 1 μg g-1 (element dependent) can be obtained. By collecting and storing full energy dispersive spectra from a multi-channel analyzer for every pixel (rather than regions of interest), it is possible to evaluate a reconstructed spectrum within the object for more robust elemental analysis. For high density matrices in particular, corrections are necessary to account for x-ray absorption by the object of both incoming X-rays and outgoing fluorescent X-rays. These effects limit the size of objects and elements that can be imaged; however reasonable corrections can be made if an estimate of linear absorption coefficient through the material is made. It is also possible to couple fluorescence tomography with microbeam x-ray absorption and diffraction analysis. When coupled

  15. Role of the Template in Model Biomineralization: Synchrotron X-ray Scattering Experiments

    NASA Astrophysics Data System (ADS)

    Uysal, Ahmet

    Synthesis of functional nanoparticles in cheap and environment friendly ways is one of the big challenges we face today. Interestingly, many biological systems are already expert at this task. Living organisms can grow nanocrystals of inorganic minerals with certain orientations and shapes and use them together with organic material to build structures with properties superior to the sum of their components. This process is called biomineralization. It has been previously shown that floating monolayers of amphiphilic molecules (Langmuir monolayers) can be used to simulate this process. This project covers the study of three different minerals, calcium oxalate, hydroxyapatite and gold, in an attempt to understand the role of the organic template in the model biomineralization experiments. We used in situ synchrotron x-ray scattering techniques to monitor the organic-inorganic interface during nucleation and growth of inorganic crystals. We also used scanning and transmission electron microscopy to study the structure of mature crystals ex situ . Although kidney stones (mostly calcium oxalate) are pathological in humans and animals, their microscopic structures exhibit considerable orientation and order, probably caused by organic molecules. Our x-ray scattering experiments revealed, first time, that in the early stages of the crystallization calcium oxalate crystals adapt a structure different from their known bulk structures. In the later stages, the crystals relax back to the bulk structure while changing the organization of the organic molecules next to them. We developed a model that explains these interactions in terms of the organic-inorganic interface potential energy. Hydroxyapatite is the main inorganic constituent of the vertebrate bone. In spite of the vast literature about bone mineralization, there is little known about the organic-inorganic interactions at the molecular level. In this thesis, we report the first in situ x-ray scattering experiments

  16. In situ X-ray pair distribution function analysis of geopolymer gel nanostructure formation kinetics.

    PubMed

    White, Claire E; Provis, John L; Bloomer, Breaunnah; Henson, Neil J; Page, Katharine

    2013-06-14

    With the ever-increasing environmentally-driven demand for technologically advanced structural materials, geopolymer cement is fast becoming a viable alternative to traditional cements due to its proven engineering characteristics and the reduction in CO2 emitted during manufacturing (as much as 80% less CO2 emitted in manufacture, compared to ordinary Portland cement). Nevertheless, much remains unknown regarding the kinetics of reaction responsible for nanostructural evolution during the geopolymerisation process. Here, in situ X-ray total scattering measurements and pair distribution function (PDF) analysis are used to quantify the extent of reaction as a function of time for alkali-activated metakaolin/slag geopolymer binders, including the impact of various activators (alkali hydroxide/silicate) on the kinetics of the geopolymerisation reaction. Quantifying the reaction process in situ from X-ray PDF data collected during the initial ten hours can provide an estimate of the total reaction extent, but when combined with data obtained at longer times (128 days here) enables more accurate determination of the overall rate of reaction. To further assess the initial stages of the geopolymerisation reaction process, a pseudo-single step first order rate equation is fitted to the extent of reaction data, which reveals important mechanistic information regarding the role of free silica in the activators in the evolution of the binder systems. Hence, it is shown that in situ X-ray PDF analysis is an ideal experimental local structure tool to probe the reaction kinetics of complex reacting systems involving transitions between disordered/amorphous phases, of which geopolymerisation is an important example.

  17. In situ X-ray pair distribution function analysis of geopolymer gel nanostructure formation kinetics.

    PubMed

    White, Claire E; Provis, John L; Bloomer, Breaunnah; Henson, Neil J; Page, Katharine

    2013-06-14

    With the ever-increasing environmentally-driven demand for technologically advanced structural materials, geopolymer cement is fast becoming a viable alternative to traditional cements due to its proven engineering characteristics and the reduction in CO2 emitted during manufacturing (as much as 80% less CO2 emitted in manufacture, compared to ordinary Portland cement). Nevertheless, much remains unknown regarding the kinetics of reaction responsible for nanostructural evolution during the geopolymerisation process. Here, in situ X-ray total scattering measurements and pair distribution function (PDF) analysis are used to quantify the extent of reaction as a function of time for alkali-activated metakaolin/slag geopolymer binders, including the impact of various activators (alkali hydroxide/silicate) on the kinetics of the geopolymerisation reaction. Quantifying the reaction process in situ from X-ray PDF data collected during the initial ten hours can provide an estimate of the total reaction extent, but when combined with data obtained at longer times (128 days here) enables more accurate determination of the overall rate of reaction. To further assess the initial stages of the geopolymerisation reaction process, a pseudo-single step first order rate equation is fitted to the extent of reaction data, which reveals important mechanistic information regarding the role of free silica in the activators in the evolution of the binder systems. Hence, it is shown that in situ X-ray PDF analysis is an ideal experimental local structure tool to probe the reaction kinetics of complex reacting systems involving transitions between disordered/amorphous phases, of which geopolymerisation is an important example. PMID:23450172

  18. In-Situ Silver Acetylide Silver Nitrate Explosive Deposition Measurements Using X-Ray Fluorescence.

    SciTech Connect

    Covert, Timothy Todd

    2014-09-01

    The Light Initiated High Explosive facility utilized a spray deposited coating of silver acetylide - silver nitrate explosive to impart a mechanical shock into targets of interest. A diagnostic was required to measure the explosive deposition in - situ. An X - ray fluorescence spectrometer was deployed at the facility. A measurement methodology was developed to measure the explosive quantity with sufficient accuracy. Through the use of a tin reference material under the silver based explosive, a field calibration relationship has been developed with a standard deviation of 3.2 % . The effect of the inserted tin material into the experiment configuration has been explored.

  19. In-situ x-ray absorption study of copper films in ground watersolutions

    SciTech Connect

    Kvashnina, K.O.; Butorin, S.M.; Modin, A.; Soroka, I.; Marcellini, M.; Nordgren, J.; Guo, J.-H.; Werme, L.

    2007-10-29

    This study illustrates how the damage from copper corrosion can be reduced by modifying the chemistry of the copper surface environment. The surface modification of oxidized copper films induced by chemical reaction with Cl{sup -} and HCO{sub 3}{sup -} in aqueous solutions was monitored by in situ X-ray absorption spectroscopy. The results show that corrosion of copper can be significantly reduced by adding even a small amount of sodium bicarbonate. The studied copper films corroded quickly in chloride solutions, whereas the same solution containing 1.1 mM HCO{sub 3}{sup -} prevented or slowed down the corrosion processes.

  20. In-situ probing of lattice response in shock compressed materials using x-ray diffraction

    SciTech Connect

    Hawreliak, J; Butterfield, M; Davies, H; El-Dasher, B; Higginbotham, A; Kalantar, D; Kimminau, G; McNaney, J; Milathianaki, D; Murphy, W; Nagler, B; Lorenzana, H; Park, N; Remington, B; Thorton, L; Whitcher, T; Wark, J; Lorenzana, H

    2007-07-17

    Lattice level measurements of material response under extreme conditions are required to build a phenomenological understanding of the shock response of solids. We have successfully used laser produced plasma x-ray sources coincident with laser driven shock waves to make in-situ measurements of the lattice response during shock compression for both single crystal and polycrystalline materials. Using a detailed analysis of shocked single crystal iron which has undergone the {alpha} - {var_epsilon} phase transition we can constrain the transition mechanism to be consistent with a compression and shuffle of alternate lattice planes.

  1. MEASURING THE PLASTIC RESPONSE IN POLYCRSYTALLINE MATERIALS USING IN-SITU X-RAY DIFFRACTION

    SciTech Connect

    Hawreliak, J; Butterfield, M; El-Dasher, B; McNaney, J; Lorenzana, H

    2008-10-01

    The insight provided by ultra-fast lattice level measurements during high strain rate high pressure experiments is key to understanding kinetic material properties like plasticity. In-situ x-ray diffraction provides a diagnostic technique which can be used to study the governing physical phenomena of plasticity at the relevant time and spatial scale. Here we discuss the recent development of a geometry capable of investigating plasticity in polycrystalline foils. We also present some preliminary data of investigations into shock compressed rolled copper foils.

  2. IN-SITU PROBING OF LATTICE RESPONSE IN SHOCK COMPRESSED MATERIALS USING X-RAY DIFFRACTION

    SciTech Connect

    Hawreliak, James; Butterfield, Martin; El-Dasher, Bassem; Kalantar, Daniel; McNaney, James; Remington, Bruce; Lorenzana, Hector; Davies, Huw; Park, Nigel; Thorton, Lee; Higginbotham, Andrew; Kimminau, Giles; Murphy, William; Nagler, Bob; Whitcher, Thomas; Wark, Justin; Milathianaki, Despina

    2007-12-12

    Lattice level measurements of material response under extreme conditions are required to build a phenomenological understanding of the shock response of solids. We have successfully used laser produced plasma x-ray sources coincident with laser driven shock waves to make in-situ measurements of the lattice response during shock compression for both single crystal and polycrystalline materials. Using a detailed analysis of shocked single crystal iron which has undergone the {alpha}-{epsilon} phase transition we can constrain the transition mechanism to be consistent with a compression and shuffle of alternate lattice planes.

  3. In situ microfluidic dialysis for biological small-angle X-ray scattering

    PubMed Central

    Skou, Magda; Skou, Søren; Jensen, Thomas G.; Vestergaard, Bente; Gillilan, Richard E.

    2014-01-01

    Owing to the demand for low sample consumption and automated sample changing capabilities at synchrotron small-angle X-ray (solution) scattering (SAXS) beamlines, X-ray microfluidics is receiving continuously increasing attention. Here, a remote-controlled microfluidic device is presented for simultaneous SAXS and ultraviolet absorption measurements during protein dialysis, integrated directly on a SAXS beamline. Microfluidic dialysis can be used for monitoring structural changes in response to buffer exchange or, as demonstrated, protein concentration. By collecting X-ray data during the concentration procedure, the risk of inducing protein aggregation due to excessive concentration and storage is eliminated, resulting in reduced sample consumption and improved data quality. The proof of concept demonstrates the effect of halted or continuous flow in the microfluidic device. No sample aggregation was induced by the concentration process at the levels achieved in these experiments. Simulations of fluid dynamics and transport properties within the device strongly suggest that aggregates, and possibly even higher-order oligomers, are preferentially retained by the device, resulting in incidental sample purification. Hence, this versatile microfluidic device enables investigation of experimentally induced structural changes under dynamically controllable sample conditions. PMID:25242913

  4. Optimizing Monocapillary Optics for Synchrotron X-ray Diffraction, Fluorescence Imaging, and Spectroscopy Applications

    NASA Astrophysics Data System (ADS)

    Bilderback, Donald H.; Kazimirov, Alexander; Gillilan, Richard; Cornaby, Sterling; Woll, Arthur; Zha, Chang-Sheng; Huang, Rong

    2007-01-01

    A number of synchrotron x-ray applications such as powder diffraction in diamond anvil cells, microbeam protein crystallography, x-ray fluorescence imaging, etc. can benefit from using hollow glass monocapillary optics to improve the flux per square micron on a sample. We currently draw glass tubing into the desired elliptical shape so that only one-bounce under total reflection conditions is needed to bring the x-ray beam to a focus at a 25 to 50 mm distance beyond the capillary tip. For modest focal spot sizes of 10 to 20 microns, we can increase the intensity per square micron by factors of 10 to 1000. We show some of the results obtained at CHESS and Hasylab with capillaries focusing 5 to 40 keV radiation, their properties, and how even better the experimental results could be if more ideal capillaries were fabricated in the future.

  5. Concentration of synchrotron beams by means of monolithic polycapillary x-ray optics

    SciTech Connect

    Ullrich, J.B.; Klotzko, I.L. |; Huang, K.G.; Owens, S.M.; Aloisi, D.C.; Hofmann, F.A.; Gao, N.; Gibson, W.M.

    1995-08-01

    Capillary Optics have proven to be a valuable tool for concentrating synchrotron radiation. Single tapered capillaries are used at several facilities. However, most of these optics collect only over a small area. this can be overcome by using larger capillary structures. Polycapillary optics can deflect x-rays by larger angles than other x-ray optics that use only one or two reflections. Conventional x-ray optics that achieve similar deflections, are much more energy selective than capillaries. Therefore, capillaries achieve very short focal distances for a wide range of energies. The measurements shown here represent first tests performed with polycapillaries of large input diameter. The performance with respect to transmission efficiency and spot size was evaluated for a set of four very different prototypes. It is shown that a significant gain may be achieved if a spot size of the order of 0.1 mm is required. Further, some characteristics of the different optics are discussed.

  6. Inclined-incidence quasi-Fresnel lens for prefocusing of synchrotron radiation x-ray beams

    NASA Astrophysics Data System (ADS)

    Kagoshima, Yasushi; Takano, Hidekazu; Takeda, Shingo

    2012-10-01

    An inclined-incidence quasi-Fresnel lens made of acrylic resin has been developed for prefocusing in synchrotron radiation x-ray beamlines. By inclining the lens, the grating aspect ratio is large enough for x-ray use. As it operates in transmission mode with negligible beam deflection and offset, little additional equipment is needed to introduce it into existing beamlines. It is fabricated by sheet-press forming, enabling inexpensive mass production. The prototype was able to focus a 730-μm-wide beam to a width of 80 μm with a photon flux density gain of 5.6 at an x-ray energy of 10 keV.

  7. Vertical synchrotron radiation beamline for proximity X-ray lithography: Theoretical analysis

    NASA Astrophysics Data System (ADS)

    Bukreeva, Inna N.; Kozhevnikov, Igor V.

    1997-02-01

    The general physical principles of operation of the vertical beamline of synchrotron radiation (SR) intended for proximity X-ray lithography are considered. An optical system provides a deflection of the SR beam to the vertical plane, a cutoff of the hard X-rays, a uniform illumination of a wafer, a normal incidence of X-ray beam onto a mask, and a small enough divergency of the radiation. A vertical SR beamline makes it possible to circumvent the expensive development of vertical-plane displacement steppers and to use the conventional horizontal ones, to exclude the scanning of the SR beam across the mask and to reduce the requirements imposed on the accuracy of alignment of a gap between the mask and the wafer.

  8. Optimizing Monocapillary Optics for Synchrotron X-ray Diffraction, Fluorescence Imaging, and Spectroscopy Applications

    SciTech Connect

    Bilderback, Donald H.; Kazimirov, Alexander; Gillilan, Richard; Cornaby, Sterling; Woll, Arthur; Zha, Chang-Sheng; Huang Rong

    2007-01-19

    A number of synchrotron x-ray applications such as powder diffraction in diamond anvil cells, microbeam protein crystallography, x-ray fluorescence imaging, etc. can benefit from using hollow glass monocapillary optics to improve the flux per square micron on a sample. We currently draw glass tubing into the desired elliptical shape so that only one-bounce under total reflection conditions is needed to bring the x-ray beam to a focus at a 25 to 50 mm distance beyond the capillary tip. For modest focal spot sizes of 10 to 20 microns, we can increase the intensity per square micron by factors of 10 to 1000. We show some of the results obtained at CHESS and Hasylab with capillaries focusing 5 to 40 keV radiation, their properties, and how even better the experimental results could be if more ideal capillaries were fabricated in the future.

  9. Diamond monochromator for high heat flux synchrotron x-ray beams

    SciTech Connect

    Khounsary, A.M.; Smither, R.K.; Davey, S.; Purohit, A.

    1993-01-28

    Single crystal silicon has been the material of choice for x-ray monochromators for the past several decades. However, the need for suitable monochromators to handle the high heat load of the next generation synchrotron x-ray beams on the one hand and the rapid and on-going advances in synthetic diamond technology on the other make a compelling case for the consideration of a diamond monochromator system. In this paper, we consider various aspects, advantages and disadvantages, and promises and pitfalls of such a system and evaluate the comparative performance of a diamond monochromator subjected to the high heat load of the most powerful x-ray beam that will become available in the next few years. The results of experiments performed to evaluate the diffraction properties of a currently available synthetic single crystal diamond are also presented. Fabrication of a diamond-based monochromator is within present technical means.

  10. Diamond monochromator for high heat flux synchrotron x-ray beams

    SciTech Connect

    Khounsary, A.M.; Smither, R.K.; Davey, S.; Purohit, A.

    1992-12-01

    Single crystal silicon has been the material of choice for x-ray monochromators for the past several decades. However, the need for suitable monochromators to handle the high heat load of the next generation synchrotron x-ray beams on the one hand and the rapid and on-going advances in synthetic diamond technology on the other make a compelling case for the consideration of a diamond mollochromator system. In this Paper, we consider various aspects, advantage and disadvantages, and promises and pitfalls of such a system and evaluate the comparative an monochromator subjected to the high heat load of the most powerful x-ray beam that will become available in the next few years. The results of experiments performed to evaluate the diffraction properties of a currently available synthetic single crystal diamond are also presented. Fabrication of diamond-based monochromator is within present technical means.

  11. Inclined-incidence quasi-Fresnel lens for prefocusing of synchrotron radiation x-ray beams

    SciTech Connect

    Kagoshima, Yasushi; Takano, Hidekazu; Takeda, Shingo

    2012-10-15

    An inclined-incidence quasi-Fresnel lens made of acrylic resin has been developed for prefocusing in synchrotron radiation x-ray beamlines. By inclining the lens, the grating aspect ratio is large enough for x-ray use. As it operates in transmission mode with negligible beam deflection and offset, little additional equipment is needed to introduce it into existing beamlines. It is fabricated by sheet-press forming, enabling inexpensive mass production. The prototype was able to focus a 730-{mu}m-wide beam to a width of 80 {mu}m with a photon flux density gain of 5.6 at an x-ray energy of 10 keV.

  12. Image Alignment for Tomography Reconstruction from Synchrotron X-Ray Microscopic Images

    PubMed Central

    Cheng, Chang-Chieh; Chien, Chia-Chi; Chen, Hsiang-Hsin; Hwu, Yeukuang; Ching, Yu-Tai

    2014-01-01

    A synchrotron X-ray microscope is a powerful imaging apparatus for taking high-resolution and high-contrast X-ray images of nanoscale objects. A sufficient number of X-ray projection images from different angles is required for constructing 3D volume images of an object. Because a synchrotron light source is immobile, a rotational object holder is required for tomography. At a resolution of 10 nm per pixel, the vibration of the holder caused by rotating the object cannot be disregarded if tomographic images are to be reconstructed accurately. This paper presents a computer method to compensate for the vibration of the rotational holder by aligning neighboring X-ray images. This alignment process involves two steps. The first step is to match the “projected feature points” in the sequence of images. The matched projected feature points in the - plane should form a set of sine-shaped loci. The second step is to fit the loci to a set of sine waves to compute the parameters required for alignment. The experimental results show that the proposed method outperforms two previously proposed methods, Xradia and SPIDER. The developed software system can be downloaded from the URL, http://www.cs.nctu.edu.tw/~chengchc/SCTA or http://goo.gl/s4AMx. PMID:24416264

  13. High resolution hard x-ray microscope on a second generation synchrotron source

    SciTech Connect

    Tian Yangchao; Li Wenjie; Chen Jie; Liu Longhua; Liu Gang; Tian Jinping; Xiong Ying; Tkachuk, Andrei; Gelb, Jeff; Hsu, George; Yun Wenbing

    2008-10-15

    A full-field, transmission x-ray microscope (TXM) operating in the energy range of 7-11 keV has been installed at the U7A beamline at the National Synchrotron Radiation Laboratory, a second generation synchrotron source operating at 0.8 GeV. Although the photon flux at sample position in the operating energy range is significantly low due to its relatively large emittance, the TXM can get high quality x-ray images with a spatial resolution down to 50 nm with acceptable exposure time. This TXM operates in either absorption or Zernike phase contrast mode with similar resolution. This TXM is a powerful analytical tool for a wide range of scientific areas, especially studies on nanoscale phenomena and structural imaging in biology, materials science, and environmental science. We present here the property of the x-ray source, beamline design, and the operation and key optical components of the x-ray TXM. Plans to improve the throughput of the TXM will be discussed.

  14. High resolution hard x-ray microscope on a second generation synchrotron source.

    PubMed

    Tian, Yangchao; Li, Wenjie; Chen, Jie; Liu, Longhua; Liu, Gang; Tkachuk, Andrei; Tian, Jinping; Xiong, Ying; Gelb, Jeff; Hsu, George; Yun, Wenbing

    2008-10-01

    A full-field, transmission x-ray microscope (TXM) operating in the energy range of 7-11 keV has been installed at the U7A beamline at the National Synchrotron Radiation Laboratory, a second generation synchrotron source operating at 0.8 GeV. Although the photon flux at sample position in the operating energy range is significantly low due to its relatively large emittance, the TXM can get high quality x-ray images with a spatial resolution down to 50 nm with acceptable exposure time. This TXM operates in either absorption or Zernike phase contrast mode with similar resolution. This TXM is a powerful analytical tool for a wide range of scientific areas, especially studies on nanoscale phenomena and structural imaging in biology, materials science, and environmental science. We present here the property of the x-ray source, beamline design, and the operation and key optical components of the x-ray TXM. Plans to improve the throughput of the TXM will be discussed. PMID:19044720

  15. High resolution hard x-ray microscope on a second generation synchrotron source

    NASA Astrophysics Data System (ADS)

    Tian, Yangchao; Li, Wenjie; Chen, Jie; Liu, Longhua; Liu, Gang; Tkachuk, Andrei; Tian, Jinping; Xiong, Ying; Gelb, Jeff; Hsu, George; Yun, Wenbing

    2008-10-01

    A full-field, transmission x-ray microscope (TXM) operating in the energy range of 7-11 keV has been installed at the U7A beamline at the National Synchrotron Radiation Laboratory, a second generation synchrotron source operating at 0.8 GeV. Although the photon flux at sample position in the operating energy range is significantly low due to its relatively large emittance, the TXM can get high quality x-ray images with a spatial resolution down to 50 nm with acceptable exposure time. This TXM operates in either absorption or Zernike phase contrast mode with similar resolution. This TXM is a powerful analytical tool for a wide range of scientific areas, especially studies on nanoscale phenomena and structural imaging in biology, materials science, and environmental science. We present here the property of the x-ray source, beamline design, and the operation and key optical components of the x-ray TXM. Plans to improve the throughput of the TXM will be discussed.

  16. Development of Ta-based STJ X-ray Detector Arrays for Synchrotron Science

    NASA Astrophysics Data System (ADS)

    Carpenter, M. H.; Friedrich, S.; Hall, J. A.; Harris, J.; Cantor, R.

    2014-08-01

    We are developing a cryogen-free Ta-based superconducting tunnel junction (STJ) detector for soft X-ray spectroscopy at synchrotrons. With an energy resolution 10 times higher than conventional solid-state X-ray detectors and count-rate capabilities above 5 kHz/pixel, STJ detectors offer potentially increased sensitivity for fluorescence-yield X-ray absorption spectroscopy (FY-XAS). We have developed 36-pixel arrays of 208 208 m Ta STJs with an energy resolution of 9 eV FWHM at the 525 eV oxygen K line. Compared to earlier Nb-based STJs, Ta-STJs offer improved energy resolution and absorption efficiency and extend the operating range to several keV. Here we describe the integration of the 36-pixel arrays into a cryogen-free, user-friendly X-ray spectrometer. A computer-controlled adiabatic demagnetization refrigerator coupled to a two-stage pulse tube refrigerator allows operation below 100 mK. The detector chip is located at the end of a 42 cm shielded snout for insertion into the analysis chamber. The system is currently being commissioned at the Advanced Light Source synchrotron.

  17. Fast photoconductor CdTe detectors for synchrotron x-ray studies

    SciTech Connect

    Yoo, Sung Shik; Faurie, J.P.; Wang, Kemei; Montano, P.A. |; Huang Qiang; Rodricks, B.

    1993-09-01

    The Advanced Photon Source will be that brightest source of synchrotron x-rays when it becomes operational in 1996. During normal operation, the ring will be filled with 20 bunches of positrons with an interbunch spacing of 177 ns and a bunch width of 119 ps. To perform experiments with x-rays generated by positrons on these time scales one needs extremely high speed detectors. To achieve the necessary high speed, we are developing MBE-grown CdTe-base photoconductive position sensitive array detectors. The arrays fabricated have 64 pixels with a gap of 100 {mu}m between pixels. The high speed response of the devices was tested using a short pulse laser. X-ray static measurements were performed using an x-ray tube and synchrotron radiation to study the device`s response to flux and wavelength changes. This paper presents the response of the devices to some of these tests and discusses different physics aspects to be considered when designing high speed detectors.

  18. Fast response amplitude scintillation detector for X-ray synchrotron radiation

    NASA Astrophysics Data System (ADS)

    Dementyev, E. N.; Sheromov, M. A.; Sokolov, A. S.

    1986-05-01

    The present paper describes a scintillation detector for X-ray synchrotron radiation. This detector has been created on the basis of a scintillator and a photoelectron multiplier (FEU-130) and its construction allows one to use the specific features of the time characteristics of synchrotron radiation from the electron storage ring. In a given range of amplitudes, the detector electronics makes a 64-channel amplitude analysis of the FEU-130 signal strobed by the revolution frequency of an electron bunch in the storage ring ( f0 = 818 kHz). There is the possibility of operating the detector at high intensities of the monochromatic radiation incident on the scintillator. Such a possibility is directly provided by the time structure of SR and is not realizable with the use of other X-ray sources. The detector will find wide application in studies on X-ray structural analysis, transmission and fluorescent EXAFS- and XANES-spectroscopy, transmission scanning microscopy and microtomography, calibration of X-ray detectors and as a monitor on SR beams from the storage ring VEPP-4.

  19. Progress in Cell Marking for Synchrotron X-ray Computed Tomography

    SciTech Connect

    Hall, Christopher; Sturm, Erica; Schultke, Elisabeth; Arfelli, Fulvia; Astolfo, Alberto; Menk, Ralf-Hendrik; Juurlink, Bernhard H. J.

    2010-07-23

    Recently there has been an increase in research activity into finding ways of marking cells in live animals for pre-clinical trials. Development of certain drugs and other therapies crucially depend on tracking particular cells or cell types in living systems. Therefore cell marking techniques are required which will enable longitudinal studies, where individuals can be examined several times over the course of a therapy or study. The benefits of being able to study both disease and therapy progression in individuals, rather than cohorts are clear. The need for high contrast 3-D imaging, without harming or altering the biological system requires a non-invasive yet penetrating imaging technique. The technique will also have to provide an appropriate spatial and contrast resolution. X-ray computed tomography offers rapid acquisition of 3-D images and is set to become one of the principal imaging techniques in this area. Work by our group over the last few years has shown that marking cells with gold nano-particles (GNP) is an effective means of visualising marked cells in-vivo using x-ray CT. Here we report the latest results from these studies. Synchrotron X-ray CT images of brain lesions in rats taken using the SYRMEP facility at the Elettra synchrotron in 2009 have been compared with histological examination of the tissues. Some deductions are drawn about the visibility of the gold loaded cells in both light microscopy and x-ray imaging.

  20. Synchrotron X-ray diffraction characterization of healthy and fluorotic human dental enamel

    NASA Astrophysics Data System (ADS)

    Colaço, M. V.; Barroso, R. C.; Porto, I. M.; Gerlach, R. F.; Costa, F. N.; Braz, D.; Droppa, R.; de Sousa, F. B.

    2012-10-01

    With the introduction of fluoride as the main anticaries agent used in preventive dentistry, and perhaps an increase in fluoride in our food chain, dental fluorosis has become an increasing world-wide problem. Visible signs of fluorosis begin to become obvious on the enamel surface as opacities, implying some porosity in the tissue. The mechanisms that conduct the formation of fluorotic enamel are unknown, but should involve modifications in the basic physical-chemistry reactions of demineralization and remineralisation of the enamel of the teeth, which is the same reaction of formation of the enamel's hydroxyapatite (HAp) in the maturation phase. The increase of the amount of fluoride inside of the apatite will result in gradual increase of the lattice parameters. The aim of this work is to characterize the healthy and fluorotic enamel in human tooth using Synchrotron X-ray diffraction. All the scattering profile measurements were carried out at the X-ray diffraction beamline (XRD1) at the Brazilian Synchrotron Light Laboratory—LNLS, Campinas, Brazil. X-ray diffraction experiments were performed both in powder samples and polished surfaces. The powder samples were analyzed to obtain the characterization of a typical healthy enamel pattern. The polished surfaces were analyzed in specific areas that have been identified as fluorotic ones. X-ray diffraction data were obtained for all samples and these data were compared with the control samples and also with the literature data.

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

    SciTech Connect

    Butterworth, A.L.; Becker, N.; Gainsforth, Z.; Lanzirotti, A.; Newville, M.; Proslier, T.; Stodolna, J.; Sutton, S.; Tyliszczak, T.; Westphal, A.J.; Zasadzinski, J.

    2012-03-13

    Quantification of synchrotron XRF analyses is typically done through comparisons with measurements on the NIST SRM 1832/1833 thin film standards. Unfortunately, these standards are inhomogeneous on small scales at the tens of percent level. We are synthesizing new homogeneous multilayer standards using the Atomic Layer Deposition technique and characterizing them using multiple analytical methods, including ellipsometry, Rutherford Back Scattering at Evans Analytical, Synchrotron X-ray Fluorescence (SXRF) at Advanced Photon Source (APS) Beamline 13-ID, Synchrotron X-ray Absorption Spectroscopy (XAS) at Advanced Light Source (ALS) Beamlines 11.0.2 and 5.3.2.1 and by electron microscopy techniques. Our motivation for developing much-needed cross-calibration of synchrotron techniques is borne from coordinated analyses of particles captured in the aerogel of the NASA Stardust Interstellar Dust Collector (SIDC). The Stardust Interstellar Dust Preliminary Examination (ISPE) team have characterized three sub-nanogram, {approx}1{micro}m-sized fragments considered as candidates to be the first contemporary interstellar dust ever collected, based on their chemistries and trajectories. The candidates were analyzed in small wedges of aerogel in which they were extracted from the larger collector, using high sensitivity, high spatial resolution >3 keV synchrotron x-ray fluorescence spectroscopy (SXRF) and <2 keV synchrotron x-ray transmission microscopy (STXM) during Stardust ISPE. The ISPE synchrotron techniques have complementary capabilities. Hard X-ray SXRF is sensitive to sub-fg mass of elements Z {ge} 20 (calcium) and has a spatial resolution as low as 90nm. X-ray Diffraction data were collected simultaneously with SXRF data. Soft X-ray STXM at ALS beamline 11.0.2 can detect fg-mass of most elements, including cosmochemically important oxygen, magnesium, aluminum and silicon, which are invisible to SXRF in this application. ALS beamline 11.0.2 has spatial resolution

  2. National Synchrotron Light Source users manual: Guide to the VUV and x-ray beam lines

    SciTech Connect

    Gmuer, N.F.; White-DePace, S.M.

    1987-08-01

    The success of the National Synchrotron Light Source in the years to come will be based, in large part, on the size of the users community and the diversity of the scientific disciplines represented by these users. In order to promote this philosophy, this National Synchrotron Light Source (NSLS) Users Manual: Guide to the VUV and X-Ray Beam Lines, has been published. This manual serves a number of purposes. In an effort to attract new research, it will present to the scientific community-at-large the current and projected architecture and capabilities of the various VUV and x-ray beam lines and storage rings. We anticipate that this publication will be updated periodically in order to keep pace with the constant changes at the NSLS.

  3. Apparatus and Techniques for Time-resolved Synchrotron X-ray Diffraction using Diamond Anvil Cells

    NASA Astrophysics Data System (ADS)

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

    2015-12-01

    Complementary advances in synchrotron sources, x-ray optics, area detectors, and sample environment control have recently made possible many time-resolved experimental techniques for studying materials at extreme pressure and temperature conditions. The High Pressure Collaborative Access Team (HPCAT) at the Advanced Photon Source has made a sustained effort to assemble a powerful collection of high-pressure apparatus for time-resolved research, and considerable time has been invested in developing techniques for collecting high-quality time-resolved x-ray scattering data. Herein we present key aspects of the synchrotron beamline and ancillary equipment, including source considerations, rapid (de)compression apparatus, high frequency imaging detectors, and software suitable for processing large volumes of data. A number of examples are presented, including fast equation of state measurements, compression rate dependent synthesis of metastable states in silicon and germanium, and ultrahigh compression rates using a piezoelectric driven diamond anvil cell.

  4. Synchrotron-based X-ray-sensitive nanoprobes for cellular imaging.

    PubMed

    Zhu, Ying; Earnest, Thomas; Huang, Qing; Cai, Xiaoqing; Wang, Zhili; Wu, Ziyu; Fan, Chunhai

    2014-12-10

    It is one of the ultimate goals in cell biology to understand the complex spatio-temporal interplay of biomolecules in the cellular context. To this end, there have been great efforts on the development of various probes to detect and localize specific biomolecules in cells with a variety of microscopic imaging techniques. In this Research News, we first summarize several types of microscopy for visualizing specific biomolecular targets. Then we focus on recent advances in the design of X-ray sensitive nanoprobes for applications in synchrotron-based cellular imaging. With the availability of advanced synchrotron techniques, there has been rapid progress toward high-resolution and multi-color X-ray imaging in cells with various types of functional nanoprobes.

  5. 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.

  6. Extending synchrotron-based atomic physics experiments into the hard X-ray region

    SciTech Connect

    LeBrun, T.

    1996-12-31

    The high-brightness, hard x-ray beams available from third-generation synchrotron sources are opening new opportunities to study the deepest inner shells of atoms, an area where little work has been done and phenomena not observed in less tightly bound inner-shells are manifested. In addition scattering processes which are weak at lower energies become important, providing another tool to investigate atomic structure as well as an opportunity to study photon/atom interactions beyond photoabsorption. In this contribution the authors discuss some of the issues related to extending synchrotron-based atomic physics experiments into the hard x-ray region from the physical and the experimental point of view. They close with a discussion of a technique, resonant Raman scattering, that may prove invaluable in determining the spectra of the very highly-excited states resulting from the excitation of deep inner shells.

  7. Tracing X-rays through an L-shaped laterally graded multilayer mirror: a synchrotron application.

    PubMed

    Honnicke, Marcelo Goncalves; Huang, Xianrong; Keister, Jeffrey W; Kodituwakku, Chaminda Nalaka; Cai, Yong Q

    2010-05-01

    A theoretical model to trace X-rays through an L-shaped (nested or Montel Kirkpatrick-Baez mirrors) laterally graded multilayer mirror to be used in a synchrotron application is presented. The model includes source parameters (size and divergence), mirror figure (parabolic and elliptic), multilayer parameters (reflectivity, which depends on layer material, thickness and number of layers) and figure errors (slope error, roughness, layer thickness fluctuation Deltad/d and imperfection in the corners). The model was implemented through MATLAB/OCTAVE scripts, and was employed to study the performance of a multilayer mirror designed for the analyzer system of an ultrahigh-resolution inelastic X-ray scattering spectrometer at National Synchrotron Light Source II. The results are presented and discussed. PMID:20400833

  8. In situ azimuthal rotation device for linear dichroism measurements in scanning transmission x-ray microscopy

    NASA Astrophysics Data System (ADS)

    Hernández-Cruz, D.; Hitchcock, A. P.; Tyliszczak, T.; Rousseau, M.-E.; Pézolet, M.

    2007-03-01

    A novel miniature rotation device used in conjunction with a scanning transmission x-ray microscope is described. It provides convenient in situ sample rotation to enable measurements of linear dichroism at high spatial resolution. The design, fabrication, and mechanical characterization are presented. This device has been used to generate quantitative maps of the spatial distribution of the orientation of proteins in several different spider and silkworm silks. Specifically, quantitative maps of the dichroic signal at the C 1s→π*amide transition in longitudinal sections of the silk fibers give information about the spatial orientation, degree of alignment, and spatial distribution of protein peptide bonds. A new approach for analyzing the dichroic signal to extract orientation distributions, in addition to magnitudes of aligned components, is presented and illustrated with results from Nephila clavipes dragline spider silk measured using the in situ rotation device.

  9. Mass Spectrometry Guided In Situ Proteolysis to Obtain Crystals for X-ray Structure Determination

    SciTech Connect

    Gheyi, Tarun; Rodgers, Logan; Romero, Richard; Sauder, J. Michael; Burley, Stephen K.

    2012-04-30

    A strategy for increasing the efficiency of protein crystallization/structure determination with mass spectrometry has been developed. This approach combines insights from limited proteolysis/mass spectrometry and crystallization via in situ proteolysis. The procedure seeks to identify protease-resistant polypeptide chain segments from purified proteins on the time-scale of crystal formation, and subsequently crystallizing the target protein in the presence of the optimal protease at the right relative concentration. We report our experience with 10 proteins of unknown structure, two of which yielded high-resolution X-ray structures. The advantage of this approach comes from its ability to select only those structure determination candidates that are likely to benefit from application of in situ proteolysis, using conditions most likely to result in formation of a stable proteolytic digestion product suitable for crystallization.

  10. In-situ reactive of x-ray optics by glow discharge

    SciTech Connect

    Johnson, E.D.; Garrett, R.F.

    1987-01-01

    We have developed a method of in-situ reactive glow discharge cleaning of x-ray optical surfaces which is capable of complete removal of carbon contamination. Our work is the first to successfully clean an entire optical system in-situ and characterize its performance at short wavelengths (as low as 10 /angstrom/). The apparatus required is quite simple and can easily be fitted to most existing UHV (ultra high vacuum) mirror boxes of monochromators. The advantages of this technique over previously available methods include dramatic improvements in instrument performance and reductions in down time since the whole process typically takes a few days. This paper will briefly describe our results and detail the experimental considerations for application of the technique on different monochromator geometries. Possible improvements and extensions of the technique are also discussed.

  11. Tracking picosecond molecular dynamics in solution using a suite of synchrotron-x-ray spectroscopic tools

    NASA Astrophysics Data System (ADS)

    March, Anne Marie; Doumy, Gilles; Kanter, Elliot P.; Lehmann, Stefan; Moonshiram, Dooshaye; Southworth, Stephen H.; Young, Linda; Assefa, Tadesse A.; Bressler, Christian; Gawelda, Wojciech; Németh, Zoltán; Vankó, György

    2015-03-01

    Laser-pump, X-ray-probe techniques are powerful tools for exploring molecular structural changes that occur in complex environments such as solutions, during a photo-initiated reaction. We are developing such methods using hard x-rays from the Advanced Photon Source, combining x-ray emission spectroscopy and x-ray absorption spectroscopy as probes of electronic and geometric structure and using high-power, MHz lasers as pumps. The high-duty-cycle pump-probe measurements efficiently utilize the synchrotron x-ray flux and enable high-fidelity measurements of the structures of transient intermediates. We present measurements on the model system [Fe(II)(CN)6]4- (ferrocyanide) in an aqueous solution after excitation with 355 nm and 266 nm laser light. The system undergoes two wavelength dependent reactions: photooxidation and photoaquation. Iron K-edge absorption spectra were obtained along with iron emission spectra. Our data support the presence of a previously unobserved pentacoordinated intermediate species in the photoaquation reaction. Its lifetime has been measured to be 4.6 ns and details of its structure will be discussed. The work was supported by the U.S. Department of Energy, Office of Science, Chemical Sciences, Geosciences, and Biosciences Division.

  12. High-energy synchrotron radiation x-ray microscopy: Present status and future prospects

    SciTech Connect

    Jones, K.W.; Gordon, B.M.; Spanne, P. ); Rivers, M.L.; Sutton, S.R. )

    1991-01-01

    High-energy radiation synchrotron x-ray microscopy is used to characterize materials of importance to the chemical and materials sciences and chemical engineering. The x-ray microscope (XRM) forms images of elemental distributions fluorescent x rays or images of mass distributions by measurement of the linear attenuation coefficient of the material. Distributions of sections through materials are obtained non-destructively using the technique of computed microtomography. The energy range of the x rays used for the XRM ranges from a few keV at the minimum value to more than 100 keV, which is sufficient to excite the K-edge of all naturally occurring elements. The work in progress at the Brookhaven NSLS X26 and X17 XRM is described in order to show the current status of the XRM. While there are many possible approaches to the XRM instrumentation, this instrument gives state-of-the-art performance in most respects and serves as a reasonable example of the present status of the instrumentation in terms of the spatial resolution and minimum detection limits obtainable. The examples of applications cited give an idea of the types of research fields that are currently under investigation. They can be used to illustrate how the field of x-ray microscopy will benefit from the use of bending magnets and insertion devices at the Advanced Photon Source. 8 refs., 5 figs.

  13. Characterization of Nano and Mesoscale Deformation Structures with Intense X-ray Synchrotron Sources

    SciTech Connect

    Ice, G.E.; Barabash, R.I.; Walker, F.J.

    2010-07-19

    Advanced polychromatic microdiffraction is sensitive to the organization of dislocations and other defects that rotate the lattice planes. Using ultra-brilliant third-generation synchrotron sources and non-dispersive X-ray focusing optics, it is now possible to analyze individual dislocation cells and walls at a submicron scale that cannot be probed by traditional methods. The method is applied to an Ir weld sample to illustrate how microdiffraction can be used to determine the locally active dislocation system.

  14. Vacuum chamber development for the synchrotron x-ray source at Argonne

    SciTech Connect

    Nielsen, R.; Moenich, J.; Wehrle, R.

    1987-03-01

    A vacuum test chamber 1.6 meters in length for the synchrotron x-ray source has been completed and tested for the evaluation of welding, sealing and ultra high vacuum (UHV) applications. A base pressure of 6.5 x 10/sup -11/ Torr (nitrogen equivalent) has been achieved. The pumping system consists of non-evaporable getter (NeG) strips. The pumpdown procedure, NeG characteristics and results are discussed.

  15. Synchrotron X-ray Investigations of Mineral-Microbe-Metal Interactions

    SciTech Connect

    Kemner, Kenneth M.; O'Loughlin, Edward J.; Kelly, Shelly D.; Boyanov, Maxim I.

    2008-06-06

    Interactions between microbes and minerals can play an important role in metal transformations (i.e. changes to an element's valence state, coordination chemistry, or both), which can ultimately affect that element's mobility. Mineralogy affects microbial metabolism and ecology in a system; microbes, in turn, can affect the system's mineralogy. Increasingly, synchrotron-based X-ray experiments are in routine use for determining an element's valence state and coordination chemistry, as well as for examining the role of microbes in metal transformations.

  16. Characteristics of radiation safety for synchrotron radiation and X-ray free electron laser facilities.

    PubMed

    Asano, Yoshihiro

    2011-07-01

    Radiation safety problems are discussed for typical electron accelerators, synchrotron radiation (SR) facilities and X-ray free electron laser (XFEL) facilities. The radiation sources at the beamline of the facilities are SR, including XFEL, gas bremsstrahlung and high-energy gamma ray and photo-neutrons due to electron beam loss. The radiation safety problems for each source are compared by using 8 GeV class SR and XFEL facilities as an example.

  17. An in situ cell for characterization of solids by soft x-ray absorption

    NASA Astrophysics Data System (ADS)

    Drake, Ian J.; Liu, Teris C. N.; Gilles, Mary; Tyliszczak, Tolek; Kilcoyne, A. L. David; Shuh, David K.; Mathies, Richard A.; Bell, Alexis T.

    2004-10-01

    A cell has been designed and fabricated for in situ characterization of catalysts and environmental materials using soft x-ray absorption spectroscopy and spectromicroscopy at photon energies above 250 eV. "Lab-on-a-chip" technologies were used to fabricate the cell on a glass wafer. The sample compartment is 1.0 mm in diameter and has a gas path length of 0.8 mm to minimize x-ray absorption in the gas phase. The sample compartment can be heated to 533 K by an Al resistive heater and gas flows up to 5.0 cm3 min-1 can be supplied to the sample compartment through microchannels. The performance of the cell was tested by acquiring Cu L3-edge x-ray appearance near-edge structure (XANES) data during the reduction and oxidation of a silica-supported Cu catalyst using the beam line 11.0.2 scanning transmission x-ray microscope (STXM) at the Advanced Light Source of Lawrence Berkeley National Laboratory (Berkeley, CA). Two-dimensional images of individual catalyst particles were recorded at photon energies between 926 and 937 eV, the energy range in which the Cu(II) and Cu(I) L3 absorption edges are observed. Oxidation state specific images of the catalyst clearly show the disappearance of Cu(II) species during the exposure of the oxidized sample to 4% CO in He while increasing the temperature from 308 to 473 K. Reoxidation restores the intensity of the image associated with Cu(II). Cu L3-edge XANES spectra obtained from stacks of STXM images show that with increasing temperature the Cu(II) peak intensity decreases as the Cu(I) peak intensity increases.

  18. Simulations of in situ x-ray diffraction from uniaxially compressed highly textured polycrystalline targets

    SciTech Connect

    McGonegle, David Wark, Justin S.; Higginbotham, Andrew; Milathianaki, Despina; Remington, Bruce A.

    2015-08-14

    A growing number of shock compression experiments, especially those involving laser compression, are taking advantage of in situ x-ray diffraction as a tool to interrogate structure and microstructure evolution. Although these experiments are becoming increasingly sophisticated, there has been little work on exploiting the textured nature of polycrystalline targets to gain information on sample response. Here, we describe how to generate simulated x-ray diffraction patterns from materials with an arbitrary texture function subject to a general deformation gradient. We will present simulations of Debye-Scherrer x-ray diffraction from highly textured polycrystalline targets that have been subjected to uniaxial compression, as may occur under planar shock conditions. In particular, we study samples with a fibre texture, and find that the azimuthal dependence of the diffraction patterns contains information that, in principle, affords discrimination between a number of similar shock-deformation mechanisms. For certain cases, we compare our method with results obtained by taking the Fourier transform of the atomic positions calculated by classical molecular dynamics simulations. Illustrative results are presented for the shock-induced α–ϵ phase transition in iron, the α–ω transition in titanium and deformation due to twinning in tantalum that is initially preferentially textured along [001] and [011]. The simulations are relevant to experiments that can now be performed using 4th generation light sources, where single-shot x-ray diffraction patterns from crystals compressed via laser-ablation can be obtained on timescales shorter than a phonon period.

  19. Synchrotron X-ray CT characterization of titanium parts fabricated by additive manufacturing. Part I. Morphology.

    PubMed

    Scarlett, Nicola Vivienne Yorke; Tyson, Peter; Fraser, Darren; Mayo, Sheridan; Maksimenko, Anton

    2016-07-01

    Synchrotron X-ray tomography has been applied to the study of titanium parts fabricated by additive manufacturing (AM). The AM method employed here was the Arcam EBM(®) (electron beam melting) process which uses powdered titanium alloy, Ti64 (Ti alloy with approximately 6%Al and 4%V), as the feed and an electron beam for the sintering/welding. The experiment was conducted on the Imaging and Medical Beamline of the Australian Synchrotron. Samples were chosen to examine the effect of build direction and complexity of design on the surface morphology and final dimensions of the piece.

  20. POLARIZATION STUDIES OF CdZnTe DETECTORS USING SYNCHROTRON X-RAY RADIATION.

    SciTech Connect

    CAMARDA,G.S.; BOLOTNIKOV, A.E.; CUI, Y.; HOSSAIN, A.; JAMES, R.B.

    2007-07-01

    New results on the effects of small-scale defects on the charge-carrier transport in single-crystal CdZnTe (CZT) material were produced. We conducted detailed studies of the role of Te inclusions in CZT by employing a highly collimated synchrotron x-ray radiation source available at Brookhaven's National Synchrotron Light Source (NSLS). We were able to induce polarization effects by irradiating specific areas with the detector. These measurements allowed the first quantitative comparison between areas that are free of Te inclusions and those with a relatively high concentration of inclusions. The results of these polaration studies will be reported.

  1. Synchrotron X-ray CT characterization of titanium parts fabricated by additive manufacturing. Part I. Morphology.

    PubMed

    Scarlett, Nicola Vivienne Yorke; Tyson, Peter; Fraser, Darren; Mayo, Sheridan; Maksimenko, Anton

    2016-07-01

    Synchrotron X-ray tomography has been applied to the study of titanium parts fabricated by additive manufacturing (AM). The AM method employed here was the Arcam EBM(®) (electron beam melting) process which uses powdered titanium alloy, Ti64 (Ti alloy with approximately 6%Al and 4%V), as the feed and an electron beam for the sintering/welding. The experiment was conducted on the Imaging and Medical Beamline of the Australian Synchrotron. Samples were chosen to examine the effect of build direction and complexity of design on the surface morphology and final dimensions of the piece. PMID:27359150

  2. Synchrotron based X-ray fluorescence activities at Indus-2: An overview

    SciTech Connect

    Tiwari, M. K.

    2014-04-24

    X-Ray fluorescence (XRF) spectrometry is a powerful non-destructive technique for elemental analysis of materials at bulk and trace concentration levels. Taking into consideration several advantages of the synchrotron based XRF technique and to fulfill the requirements of Indian universities users we have setup a microfocus XRF beamline (BL-16) on Indus-2 synchrotron light source. The beamline offers a wide range of usages – both from research laboratories and industries; and for researchers working in diverse fields. A brief overview of the measured performance of the beamline, design specifications including various attractive features and recent research activities carried out on the BL-16 beamline are presented.

  3. Characterization of a next-generation piezo bimorph X-ray mirror for synchrotron beamlines

    PubMed Central

    Alcock, Simon G.; Nistea, Ioana; Sutter, John P.; Sawhney, Kawal; Fermé, Jean-Jacques; Thellièr, Christophe; Peverini, Luca

    2015-01-01

    Piezo bimorph mirrors are versatile active optics used on many synchrotron beamlines. However, many bimorphs suffer from the ‘junction effect’: a periodic deformation of the optical surface which causes major aberrations to the reflected X-ray beam. This effect is linked to the construction of such mirrors, where piezo ceramics are glued directly below the thin optical substrate. In order to address this problem, a next-generation bimorph with piezos bonded to the side faces of a monolithic substrate was developed at Thales-SESO and optimized at Diamond Light Source. Using metrology feedback from the Diamond-NOM, the optical slope error was reduced to ∼0.5 µrad r.m.s. for a range of ellipses. To maximize usability, a novel holder was built to accommodate the substrate in any orientation. When replacing a first-generation bimorph on a synchrotron beamline, the new mirror significantly improved the size and shape of the reflected X-ray beam. Most importantly, there was no evidence of the junction effect even after eight months of continuous beamline usage. It is hoped that this new design will reinvigorate the use of active bimorph optics at synchrotron and free-electron laser facilities to manipulate and correct X-ray wavefronts. PMID:25537582

  4. Characterization of a next-generation piezo bimorph X-ray mirror for synchrotron beamlines.

    PubMed

    Alcock, Simon G; Nistea, Ioana; Sutter, John P; Sawhney, Kawal; Fermé, Jean Jacques; Thellièr, Christophe; Peverini, Luca

    2015-01-01

    Piezo bimorph mirrors are versatile active optics used on many synchrotron beamlines. However, many bimorphs suffer from the `junction effect': a periodic deformation of the optical surface which causes major aberrations to the reflected X-ray beam. This effect is linked to the construction of such mirrors, where piezo ceramics are glued directly below the thin optical substrate. In order to address this problem, a next-generation bimorph with piezos bonded to the side faces of a monolithic substrate was developed at Thales-SESO and optimized at Diamond Light Source. Using metrology feedback from the Diamond-NOM, the optical slope error was reduced to ∼ 0.5 µrad r.m.s. for a range of ellipses. To maximize usability, a novel holder was built to accommodate the substrate in any orientation. When replacing a first-generation bimorph on a synchrotron beamline, the new mirror significantly improved the size and shape of the reflected X-ray beam. Most importantly, there was no evidence of the junction effect even after eight months of continuous beamline usage. It is hoped that this new design will reinvigorate the use of active bimorph optics at synchrotron and free-electron laser facilities to manipulate and correct X-ray wavefronts.

  5. In-situ X-ray photoelectron spectroscopy studies of water on metals and oxides at ambient conditions

    SciTech Connect

    Salmeron, Miquel; Yamamoto, S.; Bluhm, H.; Andersson, K.; Ketteler, G.; Ogasawara, H.; Salmeron, M.; Nilsson, A.

    2007-10-29

    X-ray photoelectron spectroscopy (XPS) is a powerful tool for surface and interface analysis, providing the elemental composition of surfaces and the local chemical environment of adsorbed species. Conventional XPS experiments have been limited to ultrahigh vacuum (UHV) conditions due to a short mean free path of electrons in a gas phase. The recent advances in instrumentation coupled with third-generation synchrotron radiation sources enables in-situ XPS measurements at pressures above 5 Torr. In this review, we describe the basic design of the ambient pressure XPS setup that combines differential pumping with an electrostatic focusing. We present examples of the application of in-situ XPS to studies of water adsorption on the surface of metals and oxides including Cu(110), Cu(111), TiO2(110) under environmental conditions of water vapor pressure. On all these surfaces we observe a general trend where hydroxyl groups form first, followed by molecular water adsorption. The importance of surface OH groups and their hydrogen bonding to water molecules in water adsorption on surfaces is discussed in detail.

  6. Beamline electrostatic levitator for in situ high energy x-ray diffraction studies of levitated solids and liquids

    SciTech Connect

    Gangopadhyay, A.K.; Lee, G.W.; Kelto, K.F.; Rogers, J.R.; Goldman, A.I.; Robinson, D.S.; Rathz, T.J.; Hyers, R.W.

    2010-07-19

    Determinations of the phase formation sequence, crystal structures and the thermo-physical properties of materials at high temperatures are hampered by contamination from the sample container and environment. Containerless processing techniques, such as electrostatic (ESL), electromagnetic, aerodynamic, and acoustic levitation, are most suitable for these studies. An adaptation of ESL for in situ structural studies of a wide range of materials using high energy (30-130 keV) x rays at a synchrotron source is described here. This beamline ESL (BESL) allows the in situ determination of the atomic structures of equilibrium solid and liquid phases, undercooled liquids and time-resolved studies of solid-solid and liquid-solid phase transformations. The use of area detectors enables the rapid acquisition of complete diffraction patterns over a wide range (0.5-14 {angstrom}{sup -1}) of reciprocal space. The wide temperature range (300-2500 K), containerless processing environment under high vacuum (10{sup -7}-10{sup -8} Torr), and fast data acquisition capability, make BESL particularly well suited for phase stability studies of high temperature solids and liquids. An additional, but important, feature of BESL is the capability for simultaneous measurements of a host of thermo-physical properties including the specific heat, enthalpy of transformation, solidus and liquidus temperatures, density, viscosity, and surface tension, all on the same sample during the structural measurements.

  7. Taking X-ray Diffraction to the Limit: Macromolecular Structures from Femtosecond X-ray Pulses and Diffraction Microscopy of Cells with Synchrotron Radiation

    SciTech Connect

    Chapman, H N; Miao, J; Kirz, J; Sayre, D; Hodgson, K O

    2003-10-01

    The methodology of X-ray crystallography has recently been successfully extended to the structure determination of non-crystalline specimens. The phase problem was solved by using the oversampling method, which takes advantage of ''continuous'' diffraction pattern from non-crystalline specimens. Here we review the principle of this newly developed technique and discuss the ongoing experiments of imaging non-periodic objects, like cells and cellular structures using coherent and bright X-rays from the 3rd generation synchrotron radiation. In the longer run, the technique may be applied to image single biomolecules by using the anticipated X-ray free electron lasers. Computer simulations have so far demonstrated two important steps: (1) by using an extremely intense femtosecond X-ray pulse, a diffraction pattern can be recorded from a macromolecule before radiation damage manifests itself, and (2) the phase information can be ab initio retrieved from a set of calculated noisy diffraction patterns of single protein molecules.

  8. Direct synchrotron x-ray measurements of local strain fields in elastically and plastically bent metallic glasses

    DOE PAGES

    Wu, Yuan; Stoica, Alexandru Dan; Ren, Yang; Ma, Dong; Gao, Yanfei F.; Bei, Hongbin

    2015-09-03

    In situ high-energy synchrotron X-ray diffraction was conducted on elastically and plastically bent bulk metallic glass (BMG) thin plates, from which distinct local elastic strain fields were mapped spatially. These directly measured residual strain fields can be nicely interpreted by our stress analysis, and also validate a previously proposed indirect residual-stress-measurement method by relating nanoindentation hardness to residual stresses. Local shear strain variations on the cross sections of these thin plates were found in the plastically bent BMG, which however cannot be determined from the indirect indentation method. As a result, this study has important implications in designing and manipulatingmore » internal strain fields in BMGs for the purpose of ductility enhancement.« less

  9. High speed synchrotron x-ray phase contrast imaging of dynamic material response to split Hopkinson bar loading

    NASA Astrophysics Data System (ADS)

    Hudspeth, M.; Claus, B.; Dubelman, S.; Black, J.; Mondal, A.; Parab, N.; Funnell, C.; Hai, F.; Qi, M. L.; Fezzaa, K.; Luo, S. N.; Chen, W.

    2013-02-01

    The successful process of amalgamating both the time-resolved imaging capabilities present at the Advanced Photon Source beamline 32ID-B and the proficiency of high-rate loading offered by the split Hopkinson or Kolsky compression/tension bar apparatus is discussed and verification of system effectiveness is expressed via dynamic experiments on various material systems. Single particle sand interaction along with glass cracking during dynamic compression, and fiber-epoxy interfacial failure, ligament-bone debonding, and single-crystal silicon fragmentation due to dynamic tension, were imaged with 0.5 μs temporal resolution and μm-level spatial resolution. Synchrotron x-ray phase contrast imaging of said material systems being loaded with the Kolsky bar apparatus demonstratively depicts the effectiveness of the novel union between these two powerful techniques, thereby allowing for in situ analysis of the interior of the material system during high-rate loading for a variety of applications.

  10. Direct synchrotron x-ray measurements of local strain fields in elastically and plastically bent metallic glasses

    SciTech Connect

    Wu, Yuan; Stoica, Alexandru Dan; Ren, Yang; Ma, Dong; Gao, Yanfei F.; Bei, Hongbin

    2015-09-03

    In situ high-energy synchrotron X-ray diffraction was conducted on elastically and plastically bent bulk metallic glass (BMG) thin plates, from which distinct local elastic strain fields were mapped spatially. These directly measured residual strain fields can be nicely interpreted by our stress analysis, and also validate a previously proposed indirect residual-stress-measurement method by relating nanoindentation hardness to residual stresses. Local shear strain variations on the cross sections of these thin plates were found in the plastically bent BMG, which however cannot be determined from the indirect indentation method. As a result, this study has important implications in designing and manipulating internal strain fields in BMGs for the purpose of ductility enhancement.

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

    PubMed

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

    2014-01-01

    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. PMID:25078347

  12. High speed synchrotron x-ray phase contrast imaging of dynamic material response to split Hopkinson bar loading

    SciTech Connect

    Hudspeth, M.; Claus, B.; Dubelman, S.; Black, J.; Mondal, A.; Parab, N.; Funnell, C.; Hai, F.; Chen, W.; Qi, M. L.; Fezzaa, K.; Luo, S. N.

    2013-02-15

    The successful process of amalgamating both the time-resolved imaging capabilities present at the Advanced Photon Source beamline 32ID-B and the proficiency of high-rate loading offered by the split Hopkinson or Kolsky compression/tension bar apparatus is discussed and verification of system effectiveness is expressed via dynamic experiments on various material systems. Single particle sand interaction along with glass cracking during dynamic compression, and fiber-epoxy interfacial failure, ligament-bone debonding, and single-crystal silicon fragmentation due to dynamic tension, were imaged with 0.5 {mu}s temporal resolution and {mu}m-level spatial resolution. Synchrotron x-ray phase contrast imaging of said material systems being loaded with the Kolsky bar apparatus demonstratively depicts the effectiveness of the novel union between these two powerful techniques, thereby allowing for in situ analysis of the interior of the material system during high-rate loading for a variety of applications.

  13. Diffuse Hard X-Ray Emission in Starburst Galaxies as Synchrotron from Very High Energy Electrons

    NASA Astrophysics Data System (ADS)

    Lacki, Brian C.; Thompson, Todd A.

    2013-01-01

    The origin of the diffuse hard X-ray (2-10 keV) emission from starburst galaxies is a long-standing problem. We suggest that synchrotron emission of 10-100 TeV electrons and positrons (e ±) can contribute to this emission, because starbursts have strong magnetic fields. We consider three sources of e ± at these energies: (1) primary electrons directly accelerated by supernova remnants, (2) pionic secondary e ± created by inelastic collisions between cosmic ray (CR) protons and gas nuclei in the dense interstellar medium of starbursts, and (3) pair e ± produced between the interactions between 10 and 100 TeV γ-rays and the intense far-infrared (FIR) radiation fields of starbursts. We create one-zone steady-state models of the CR population in the Galactic center (R <= 112 pc), NGC 253, M82, and Arp 220's nuclei, assuming a power-law injection spectrum for electrons and protons. We consider different injection spectral slopes, magnetic field strengths, CR acceleration efficiencies, and diffusive escape times, and include advective escape, radiative cooling processes, and secondary and pair e ±. We compare these models to extant radio and GeV and TeV γ-ray data for these starbursts, and calculate the diffuse synchrotron X-ray and inverse Compton (IC) luminosities of these starbursts in the models which satisfy multiwavelength constraints. If the primary electron spectrum extends to ~PeV energies and has a proton/electron injection ratio similar to the Galactic value, we find that synchrotron emission contributes 2%-20% of their unresolved, diffuse hard X-ray emission. However, there is great uncertainty in this conclusion because of the limited information on the CR electron spectrum at these high energies. IC emission is likewise a minority of the unresolved X-ray emission in these starbursts, from 0.1% in the Galactic center to 10% in Arp 220's nuclei, with the main uncertainty being the starbursts' magnetic field. We also model generic starbursts, including

  14. Development of in-line furnace for in-situ nanoscale resolution x-ray microscopy

    NASA Astrophysics Data System (ADS)

    Eng, Christopher; Chen-Wiegart, Yu-Chen K.; Wang, Jun

    2013-09-01

    Full field transmission x-ray microscopy (TXM) is a newly developed x-ray imaging technique to provide quantitative and non-destructive 3D characterization of the complex microstructure of materials at nanometer resolution. A key missing component is an in situ apparatus enabling the imaging of the complex structural evolution of the materials and to correlate the structural change with a material's functionality under real operating conditions. This work describes the design of an environmental cell which satisfies the requirements for in situ TXM studies. The limited space within the TXM presents a spatial constraint which prohibits the use of conventional heaters, as well as requiring consideration in designing for safe and controlled operation of the system and alignment of the cell with the beam. A gravity drip-fed water cooling jacket was installed in place around the heating module to maintain critical components of the microscope at safe operating temperatures. A motion control system consisting of pulse width modulated DC motor driven XYZ translation stages was developed to facilitate fine alignment of the cell. Temperature of the sample can be controlled remotely and accurately through a controller to temperatures as high as 1200 K. Heating zone measurement was carried out and shows a 500 x 500 x 500 μm3 homogeneous zone volume for sample area, which is a critical parameter to ensure accurate observation of structural evolution at nanometer scale with a sample in size of tens of microns. Application on Ni particles for in situ oxidation experiment and dehydrogenation of aluminum hydride is also discussed.

  15. X-Tream quality assurance in synchrotron X-ray microbeam radiation therapy.

    PubMed

    Fournier, Pauline; Cornelius, Iwan; Donzelli, Mattia; Requardt, Herwig; Nemoz, Christian; Petasecca, Marco; Bräuer-Krisch, Elke; Rosenfeld, Anatoly; Lerch, Michael

    2016-09-01

    Microbeam radiation therapy (MRT) is a novel irradiation technique for brain tumours treatment currently under development at the European Synchrotron Radiation Facility in Grenoble, France. The technique is based on the spatial fractionation of a highly brilliant synchrotron X-ray beam into an array of microbeams using a multi-slit collimator (MSC). After promising pre-clinical results, veterinary trials have recently commenced requiring the need for dedicated quality assurance (QA) procedures. The quality of MRT treatment demands reproducible and precise spatial fractionation of the incoming synchrotron beam. The intensity profile of the microbeams must also be quickly and quantitatively characterized prior to each treatment for comparison with that used for input to the dose-planning calculations. The Centre for Medical Radiation Physics (University of Wollongong, Australia) has developed an X-ray treatment monitoring system (X-Tream) which incorporates a high-spatial-resolution silicon strip detector (SSD) specifically designed for MRT. In-air measurements of the horizontal profile of the intrinsic microbeam X-ray field in order to determine the relative intensity of each microbeam are presented, and the alignment of the MSC is also assessed. The results show that the SSD is able to resolve individual microbeams which therefore provides invaluable QA of the horizontal field size and microbeam number and shape. They also demonstrate that the SSD used in the X-Tream system is very sensitive to any small misalignment of the MSC. In order to allow as rapid QA as possible, a fast alignment procedure of the SSD based on X-ray imaging with a low-intensity low-energy beam has been developed and is presented in this publication. PMID:27577773

  16. 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).

  17. 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

  18. Development of in-situ full-field spectroscopic imaging analysis and application on Li-ion battery using transmission x-ray microscopy

    NASA Astrophysics Data System (ADS)

    Chen-Wiegart, Yu-chen K.; Wang, Jiajun; Wang, Jun

    2013-09-01

    This paper presents the advance in spectroscopic imaging technique and analysis method from the newly developed transmission x-ray microscopy (TXM) at the beamline X8C of National Synchrotron Light Source. Through leastsquares linear combination fitting we developed on the in situ spectroscopic images, a time-dependent and spatially resolved chemical composition mapping can be obtained and quantitatively analyzed undergone chemical/electrochemical reactions. A correlation of morphological evolution, chemical state distribution changes and reaction conditions can be revealed. We successfully applied this method to study the electrochemical evolution of CuO, an anode material of Li-ion battery, during the lithiation-delitiation cycling.

  19. In Situ Mineralogical Analysis of Planetary Materials Using X-Ray Diffraction and X-Ray Fluorescence

    NASA Technical Reports Server (NTRS)

    Sarrazin, P.; Blake, D.; Vaniman, D.; Chang, Sherwood (Technical Monitor)

    1996-01-01

    Remote observations of Mars have led scientists to believe that its early climate was similar to that of the early Earth, having had abundant liquid water and a dense atmosphere. One of the most fascinating questions of recent times is whether simple bacterial life developed on Mars (as it did on the Earth) during this early element period. Analyses of SNC meteorites have broadened considerably our knowledge of the chemistry of certain types of Martian rocks, underscoring the tantalizing possibility of early hydrothermal systems and even of ancient bacterial life. Detailed analyses of SNC meteorites in Terrestrial laboratories utilize the most sophisticated organic, isotopic and microscopic techniques in existence. Indeed; it is unlikely that the key biogenic indicators used in McKay et al (ibid) could be identified by a remote instrument on the surface of Mars. As a result, it is probable that any robotic search for evidence of an ancient Martian biosphere will have as its focus the identification of key minerals in likely host rocks rather than the direct detection of organic or isotopic biomarkers. Even on a sample return mission, mineralogical screening will be utilized to choose the most likely candidate rocks. X-ray diffraction (XRD) is the only technique that can provide a direct determination of the crystal structures of the phases present within a sample. When many different crystalline phases are present, quantitative analysis is better constrained if used in conjunction with a determination of elemental composition, obtainable by X-ray fluorescence (XRF) using the same X-ray source as for XRD. For planetary surface analysis, a remote instrument combining XRD and XRF could be used for mineralogical characterization of both soils and rocks. We are designing a remote XRD/XRF instrument with this objective in mind. The instrument concept pays specific attention to constraints in sample preparation, weight, volume, power, etc. Based on the geometry of a

  20. Workshops on Science Enabled by a Coherent, CW, Synchrotron X-ray Source, June 2011

    SciTech Connect

    Brock, Joel

    2012-01-03

    In June of 2011 we held six two-day workshops called "XDL-2011: Science at the Hard X-ray Diffraction Limit". The six workshops covered (1) Diffraction-based imaging techniques, (2) Biomolecular structure from non-crystalline materials, (3) Ultra-fast science, (4) High-pressure science, (5) Materials research with nano-beams and (6) X-ray photon correlation spectroscopy (XPCS), In each workshop, invited speaker from around the world presented examples of novel experiments that require a CW, diffraction-limited source. During the workshop, each invited speaker provided a one-page description of the experiment and an illustrative graphic. The experiments identified by the workshops demonstrate the broad and deep scientific case for a CW coherent synchrotron x-ray source. The next step is to perform detailed simulations of the best of these ideas to test them quantitatively and to guide detailed x-ray beam-line designs. These designs are the first step toward developing detailed facility designs and cost estimates.

  1. Heat transfer issues in high-heat-load synchrotron x-ray beams

    SciTech Connect

    Khounsary, A.M.; Mills, D.M.

    1994-09-01

    In this paper, a short description of the synchrotron radiation x-ray sources and the associated power loads is given, followed by a brief description of typical synchrotron components and their heat load. It is emphasized that the design goals for most of these components is to limit (a) temperature, (b) stresses, or (c) strains in the system. Each design calls for a different geometry, material selection, and cooling scheme. Cooling schemes that have been utilized so far are primarily single phase and include simple macrochannel cooling, microchannel cooling, contact cooling, pin-post cooling, porous-flow cooling, jet cooling, etc. Water, liquid metals, and various cryogenic coolants have been used. Because the trend in x-ray beam development is towards brighter (i.e., more powerful) beams and assuming that no radical changes in the design of x-ray generating machines occurs in the next few years, it is fair to state that the utilization of various effective cooling schemes and, in particular, two-phase flow (e.g., subcooled boiling) warrants further investigation. This, however, requires a thorough examination of stability and reliability of two-phase flows for high-heat-flux components operating in ultrahigh vacuum with stringent reliability requirements.

  2. Synchrotron Small-Angle X-ray Scattering Study of Cross-Linked Polymeric Micelles.

    PubMed

    Kim, Hyun-Chul; Jin, Kyeong Sik; Lee, Se Guen; Kim, Eunjoo; Lee, Sung Jun; Jeong, Sang Won; Lee, Seung Woo; Kim, Kwang-Woo

    2016-06-01

    Polymeric micelles of methoxypoly(ethylene glycol)-b-poly(lactide) containing lysine units (mPEG-PLA-Lys4) were cross-linked by reacting of lysine moieties with a bifunctional bis(N-hydroxy-succinimide ester). The micelles were characterized in aqueous solution using dynamic light scattering, transmission electron microscopy, and synchrotron small-angle X-ray scattering. The mPEG-PLA-Lys4 was synthesized through the ring-opening polymerization of N6-carbobenzyloxy-L-lysine N-carboxyanhydride with amine-terminated mPEG-PLA and subsequent deprotection. The polymeric micelles showed enhanced micelle stability after cross-linking, which was confirmed by adding sodium dodecyl sulfate as a destabilizing agent. The average diameters measured via dynamic light scattering were 19.1 nm and 29.2 nm for non-cross-linked polymeric micelles (NCPMs) and cross-linked polymeric micelles (CPMs), respectively. The transmission electron microscopy images showed that the size of the polymeric micelles increased slightly due to cross-linking, which was in good agreement with the DLS measurements. The overall structures and internal structural changes of NCPMs and CPMs in aqueous solution were studied in detail using synchrotron X-ray scattering method. According to the structural parameters of X-ray scattering analysis, CPMs with a more densely packed core structure were formed by reacting bifunctional cross-linking agents with lysine amino groups located in the innermost core of the polymeric micelles. PMID:27427731

  3. Conical geometry for sagittal focusing as applied to X rays from synchrotrons

    SciTech Connect

    Ice, G.E.; Sparks, C.J.

    1993-06-01

    The authors describe a method for simultaneously focusing and monochromatization of X rays from a fan of radiation having up to 15 mrad divergence in one dimension. This geometry is well suited to synchrotron radiation sources at magnifications of one-fifth to two and is efficient for X-ray energies between 3 and 40 keV (0.48 and 6.4 fJ). The method uses crystals bent to part of a cone for sagittal focusing and allows for the collection of a larger divergence with less mixing of the horizontal into the vertical divergence than is possible with X-ray mirrors. They describe the geometry required to achieve the highest efficiency when a conical crystal follows a flat crystal in a nondispersive two-crystal monochromator. At a magnification of one-third, the geometry is identical to a cylindrical focusing design described previously. A simple theoretical calculation is shown to agree well with ray-tracing results. Minimum aberrations are observed at magnifications near one. Applications of the conical focusing geometry to existing and future synchrotron radiation facilities are discussed.

  4. Atomic Structure of Pt3Ni Nanoframe Electrocatalysts by in Situ X-ray Absorption Spectroscopy.

    PubMed

    Becknell, Nigel; Kang, Yijin; Chen, Chen; Resasco, Joaquin; Kornienko, Nikolay; Guo, Jinghua; Markovic, Nenad M; Somorjai, Gabor A; Stamenkovic, Vojislav R; Yang, Peidong

    2015-12-23

    Understanding the atomic structure of a catalyst is crucial to exposing the source of its performance characteristics. It is highly unlikely that a catalyst remains the same under reaction conditions when compared to as-synthesized. Hence, the ideal experiment to study the catalyst structure should be performed in situ. Here, we use X-ray absorption spectroscopy (XAS) as an in situ technique to study Pt3Ni nanoframe particles which have been proven to be an excellent electrocatalyst for the oxygen reduction reaction (ORR). The surface characteristics of the nanoframes were probed through electrochemical hydrogen underpotential deposition and carbon monoxide electrooxidation, which showed that nanoframe surfaces with different structure exhibit varying levels of binding strength to adsorbate molecules. It is well-known that Pt-skin formation on Pt-Ni catalysts will enhance ORR activity by weakening the binding energy between the surface and adsorbates. Ex situ and in situ XAS results reveal that nanoframes which bind adsorbates more strongly have a rougher Pt surface caused by insufficient segregation of Pt to the surface and consequent Ni dissolution. In contrast, nanoframes which exhibit extremely high ORR activity simultaneously demonstrate more significant segregation of Pt over Ni-rich subsurface layers, allowing better formation of the critical Pt-skin. This work demonstrates that the high ORR activity of the Pt3Ni hollow nanoframes depends on successful formation of the Pt-skin surface structure.

  5. X-Ray Diffraction and Fluorescence Measurements for In Situ Planetary Instruments

    NASA Astrophysics Data System (ADS)

    Hansford, G.; Hill, K. S.; Talboys, D.; Vernon, D.; Ambrosi, R.; Bridges, J.; Hutchinson, I.; Marinangeli, L.

    2011-12-01

    The ESA/NASA ExoMars mission, due for launch in 2018, has a combined X-ray fluorescence/diffraction instrument, Mars-XRD, as part of the onboard analytical laboratory. The results of some XRF (X-ray fluorescence) and XRD (X-ray diffraction) tests using a laboratory chamber with representative performance are reported. A range of standard geological reference materials and analogues were used in these tests. The XRD instruments are core components of the forthcoming NASA Mars Science Laboratory (MSL) and ESA/NASA ExoMars missions and will provide the first demonstrations of the capabilities of combined XRD/XRF instrumentation in situ on an extraterrestrial planetary surface. The University of Leicester team is part of the Italy-UK collaboration that is responsible for building the ExoMars X-ray diffraction instrument, Mars-XRD [1,2]. Mars-XRD incorporates an Fe-55 radioisotope source and three fixed-position charge-coupled devices (CCDs) to simultaneously acquire an X-ray fluorescence spectrum and a diffraction pattern providing a measurement of both elemental and mineralogical composition. The CCDs cover an angular range of 2θ = 6° to 73° enabling the analysis of a wide range of geologically important minerals including phyllosilicates, feldspars, oxides, carbonates and evaporites. The identification of hydrous minerals may help identify past Martian hydrothermal systems capable of preserving traces of life. Here we present some initial findings from XRF and XRD tests carried out at the University of Leicester using an Fe-55 source and X-ray sensitive CCD. The XRF/XRD test system consists of a single CCD on a motorised arm, an Fe-55 X-ray source, a collimator and a sample table which approximately replicate the reflection geometry of the Mars-XRD instrument. It was used to test geological reference standard materials and Martian analogues. This work was funded by the Science and Technology Facilities Council, UK. References [1] Marinangeli, L., Hutchinson, I

  6. In situ time-resolved X-ray diffraction of tobermorite formation in autoclaved aerated concrete: Influence of silica source reactivity and Al addition

    SciTech Connect

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

    2011-05-15

    The hydrothermal formation of tobermorite during the processing of autoclaved aerated concrete was investigated by in situ X-ray diffraction (XRD) analysis. High-energy X-rays from a synchrotron radiation source in combination with a newly developed autoclave cell and a photon-counting pixel array detector were used. To investigate the effects of the silica source, reactive quartz from chert and less-reactive quartz from quartz sand were used as starting materials. The effect of Al addition on tobermorite formation was also studied. In all cases, C-S-H, hydroxylellestadite and katoite were clearly observed as intermediates. Acceleration of tobermorite formation by Al addition was clearly observed. However, Al addition did not affect the dissolution rate of quartz. Two pathways, via C-S-H and katoite, were also observed in the Al-containing system. These results suggest that the structure of initially formed C-S-H is important for the subsequent tobermorite formation reactions.

  7. A glass capillary cell for in situ powder X-ray diffraction of condensed volatile compounds. Solid HCFC-123a and HCFC-124.

    PubMed

    Brunelli, Michela; Fitch, Andrew N

    2003-07-01

    A rotating glass capillary cell with a gas handling system has been built to allow in situ studies by powder X-ray diffraction. The cell can be used to condense volatile compounds, or to follow solid-state chemical reactions under vacuum or at gas pressures up to around 7 x 10(5) Pa. Using the cell, cooled by a stream of helium gas, the solid phases of 1,2-dichlorotrifluoroethane (HCFC-123a) and 2-chloro-1,1,1,2-tetrafluoroethane (HCFC-124) have been investigated using powder synchrotron X-ray radiation. These were found to have disordered hexagonal structures, with a = 4.018 (5), c = 6.553 (1) A and a = 4.048 (1), c = 6.625 (1) A, respectively, at 64 K. PMID:12824935

  8. In-situ X-ray diffraction combined with scanning AC nanocalorimetry applied to a Fe0.84Ni0.16 thin-film sample

    PubMed Central

    Gregoire, John M.; Xiao, Kechao; McCluskey, Patrick J.; Dale, Darren; Cuddalorepatta, Gayatri; Vlassak, Joost J.

    2013-01-01

    We combine the characterization techniques of scanning AC nanocalorimetry and x-ray diffraction to study phase transformations in complex materials system. Micromachined nanocalorimeters have excellent performance for high-temperature and high-scanning-rate calorimetry measurements. Time-resolved X-ray diffraction measurements during in-situ operation of these devices using synchrotron radiation provide unprecedented characterization of thermal and structural material properties. We apply this technique to a Fe0.84Ni0.16 thin-film sample that exhibits a martensitic transformation with over 350 K hysteresis, using an average heating rate of 85 K/s and cooling rate of 275 K/s. The apparatus includes an array of nanocalorimeters in an architecture designed for combinatorial studies. PMID:23825802

  9. Near-isothermal furnace for in situ and real time X-ray radiography solidification experiments.

    PubMed

    Becker, M; Dreißigacker, C; Klein, S; Kargl, F

    2015-06-01

    In this paper, we present a newly developed near-isothermal X-ray transparent furnace for in situ imaging of solidification processes in thin metallic samples. We show that the furnace is ideally suited to study equiaxed microstructure evolution and grain interaction. To observe the growth dynamics of equiaxed dendritic structures, a minimal temperature gradient across the sample is required. A uniform thermal profile inside a circular sample is achieved by positioning the sample in the center of a cylindrical furnace body surrounded by a circular heater arrangement. Performance tests with the hypo-eutectic Al-15wt.%Cu and the near-eutectic Al-33wt.%Cu alloys validate the near-isothermal character of the sample environment. Controlled cooling rates of less than 0.5 K min(-1) up to 10 K min(-1) can be achieved in a temperature range of 720 K-1220 K. Integrated in our rotatable laboratory X-ray facility, X-RISE, the furnace provides a large field of view of 10.5 mm in diameter and a high spatial resolution of ∼4 μm. With the here presented furnace, equiaxed dendrite growth models can be rigorously tested against experiments on metal alloys by, e.g., enabling dendrite growth velocities to be determined as a function of undercooling or solutal fields in front of the growing dendrite to be measured.

  10. Near-isothermal furnace for in situ and real time X-ray radiography solidification experiments

    SciTech Connect

    Becker, M. Dreißigacker, C.; Klein, S.; Kargl, F.

    2015-06-15

    In this paper, we present a newly developed near-isothermal X-ray transparent furnace for in situ imaging of solidification processes in thin metallic samples. We show that the furnace is ideally suited to study equiaxed microstructure evolution and grain interaction. To observe the growth dynamics of equiaxed dendritic structures, a minimal temperature gradient across the sample is required. A uniform thermal profile inside a circular sample is achieved by positioning the sample in the center of a cylindrical furnace body surrounded by a circular heater arrangement. Performance tests with the hypo-eutectic Al-15wt.%Cu and the near-eutectic Al-33wt.%Cu alloys validate the near-isothermal character of the sample environment. Controlled cooling rates of less than 0.5 K min{sup −1} up to 10 K min{sup −1} can be achieved in a temperature range of 720 K–1220 K. Integrated in our rotatable laboratory X-ray facility, X-RISE, the furnace provides a large field of view of 10.5 mm in diameter and a high spatial resolution of ∼4 μm. With the here presented furnace, equiaxed dendrite growth models can be rigorously tested against experiments on metal alloys by, e.g., enabling dendrite growth velocities to be determined as a function of undercooling or solutal fields in front of the growing dendrite to be measured.

  11. In Situ High-Pressure X-ray Diffraction Study of H2O Ice VII

    SciTech Connect

    Somayazulu,M.; Shu, J.; Zha, C.; Goncharov, A.; Tschauner, O.; Mao, H.; Hemley, R.

    2008-01-01

    Ice VII was examined over the entire range of its pressure stability by a suite of x-ray diffraction techniques in order to understand a number of unexplained characteristics of its high-pressure behavior. Axial and radial polycrystalline (diamond anvil cell) x-ray diffraction measurements reveal a splitting of diffraction lines accompanied by changes in sample texture and elastic anisotropy. In situ laser heating of polycrystalline samples resulted in the sharpening of diffraction peaks due to release of nonhydrostatic stresses but did not remove the splitting. Radial diffraction measurements indicate changes in strength of the material at this pressure. Taken together, these observations provide evidence for a transition in ice VII near 14 GPa involving changes in the character of the proton order/disorder. The results are consistent with previous reports of changes in phase boundaries and equation of state at this pressure. The transition can be interpreted as ferroelastic with the appearance of spontaneous strain that vanishes at the hydrogen bond symmetrization transition near 60 GPa.

  12. Compact Roll-to-Roll Coater for in Situ X-ray Diffraction Characterization of Organic Electronics Printing.

    PubMed

    Gu, Xiaodan; Reinspach, Julia; Worfolk, Brian J; Diao, Ying; Zhou, Yan; Yan, Hongping; Gu, Kevin; Mannsfeld, Stefan; Toney, Michael F; Bao, Zhenan

    2016-01-27

    We describe a compact roll-to-roll (R2R) coater that is capable of tracking the crystallization process of semiconducting polymers during solution printing using X-ray scattering at synchrotron beamlines. An improved understanding of the morphology evolution during the solution-processing of organic semiconductor materials during R2R coating processes is necessary to bridge the gap between "lab" and "fab". The instrument consists of a vacuum chuck to hold the flexible plastic substrate uniformly flat for grazing incidence X-ray scattering. The time resolution of the drying process that is achievable can be tuned by controlling two independent motor speeds, namely, the speed of the moving flexible substrate and the speed of the printer head moving in the opposite direction. With this novel design, we are able to achieve a wide range of drying time resolutions, from tens of milliseconds to seconds. This allows examination of the crystallization process over either fast or slow drying processes depending on coating conditions. Using regioregular poly(3-hexylthiophene-2,5-diyl) (P3HT) and phenyl-C61-butyric acid methyl ester (PCBM) inks based on two different solvents as a model system, we demonstrate the capability of our in situ R2R printing tool by observing two distinct crystallization processes for inks drying from the solvents with different boiling points (evaporation rates). We also observed delayed on-set point for the crystallization of P3HT polymer in the 1:1 P3HT/PCBM BHJ blend, and the inhibited crystallization of the P3HT during the late stage of the drying process. PMID:26714412

  13. Fatigue History and in-situ Loading Studies of the overload Effect Using High Resolution X-ray Strain Profiling

    SciTech Connect

    Croft,M.; Jisrawi, N.; Zhong, Z.; Holtz, R.; Sadananda, K.; Skaritka, J.; Tsakalakos, T.

    2007-01-01

    High-energy synchrotron X-ray diffraction experiments are used to perform local crack plane strain profiling of 4140 steel compact tension specimens fatigued at constant amplitude, subjected to a single overload cycle, then fatigued some more at constant amplitude. X-ray strain profiling results on a series of samples employing in-situ load cycling are correlated with the crack growth rate (da/dN) providing insight into the da/dN retardation known as the 'overload effect'. Immediately after the overload, the strain under maximum load is greatly reduced but the range of strain, between zero and maximum load, remains unchanged compared to the pre-overload values. At the point of maximum retardation, it is the strain range that is greatly reduced while the maximum-load strain has begun to recover to the pre-overload value. For a sample that has recovered to approximately half of the original da/dN value following the overload, the strain at maximum load is fully recovered while the strain range, though partially recovered, is still substantially reduced. The dominance of the strain range in the overload effect is clearly indicated. Subject to some assumptions, strong quantitative support for a crack growth rate driving force of the suggested form [(K{sub max}){sup -p}({Delta}K){sup p}]{sup {gamma}} is found. A dramatic nonlinear load dependence in the spatial distribution of the strain at maximum retardation is also demonstrated: at low load the response is dominantly at the overload position; whereas at high loads it is dominantly at the crack tip position. This transfer of load response away from the crack tip to the overload position appears fundamental to the overload effect for high R-ratio fatigue as studied here.

  14. Compact Roll-to-Roll Coater for in Situ X-ray Diffraction Characterization of Organic Electronics Printing.

    PubMed

    Gu, Xiaodan; Reinspach, Julia; Worfolk, Brian J; Diao, Ying; Zhou, Yan; Yan, Hongping; Gu, Kevin; Mannsfeld, Stefan; Toney, Michael F; Bao, Zhenan

    2016-01-27

    We describe a compact roll-to-roll (R2R) coater that is capable of tracking the crystallization process of semiconducting polymers during solution printing using X-ray scattering at synchrotron beamlines. An improved understanding of the morphology evolution during the solution-processing of organic semiconductor materials during R2R coating processes is necessary to bridge the gap between "lab" and "fab". The instrument consists of a vacuum chuck to hold the flexible plastic substrate uniformly flat for grazing incidence X-ray scattering. The time resolution of the drying process that is achievable can be tuned by controlling two independent motor speeds, namely, the speed of the moving flexible substrate and the speed of the printer head moving in the opposite direction. With this novel design, we are able to achieve a wide range of drying time resolutions, from tens of milliseconds to seconds. This allows examination of the crystallization process over either fast or slow drying processes depending on coating conditions. Using regioregular poly(3-hexylthiophene-2,5-diyl) (P3HT) and phenyl-C61-butyric acid methyl ester (PCBM) inks based on two different solvents as a model system, we demonstrate the capability of our in situ R2R printing tool by observing two distinct crystallization processes for inks drying from the solvents with different boiling points (evaporation rates). We also observed delayed on-set point for the crystallization of P3HT polymer in the 1:1 P3HT/PCBM BHJ blend, and the inhibited crystallization of the P3HT during the late stage of the drying process.

  15. The GALAXIES beamline at the SOLEIL synchrotron: inelastic X-ray scattering and photoelectron spectroscopy in the hard X-ray range.

    PubMed

    Rueff, J P; Ablett, J M; Céolin, D; Prieur, D; Moreno, Th; Balédent, V; Lassalle-Kaiser, B; Rault, J E; Simon, M; Shukla, A

    2015-01-01

    The GALAXIES beamline at the SOLEIL synchrotron is dedicated to inelastic X-ray scattering (IXS) and photoelectron spectroscopy (HAXPES) in the 2.3-12 keV hard X-ray range. These two techniques offer powerful complementary methods of characterization of materials with bulk sensitivity, chemical and orbital selectivity, resonant enhancement and high resolving power. After a description of the beamline components and endstations, the beamline capabilities are demonstrated through a selection of recent works both in the solid and gas phases and using either IXS or HAXPES approaches. Prospects for studies on liquids are discussed.

  16. The GALAXIES beamline at the SOLEIL synchrotron: inelastic X-ray scattering and photoelectron spectroscopy in the hard X-ray range.

    PubMed

    Rueff, J P; Ablett, J M; Céolin, D; Prieur, D; Moreno, Th; Balédent, V; Lassalle-Kaiser, B; Rault, J E; Simon, M; Shukla, A

    2015-01-01

    The GALAXIES beamline at the SOLEIL synchrotron is dedicated to inelastic X-ray scattering (IXS) and photoelectron spectroscopy (HAXPES) in the 2.3-12 keV hard X-ray range. These two techniques offer powerful complementary methods of characterization of materials with bulk sensitivity, chemical and orbital selectivity, resonant enhancement and high resolving power. After a description of the beamline components and endstations, the beamline capabilities are demonstrated through a selection of recent works both in the solid and gas phases and using either IXS or HAXPES approaches. Prospects for studies on liquids are discussed. PMID:25537606

  17. In situ X-ray polymerization: from swollen lamellae to polymer-surfactant complexes.

    PubMed

    Agzenai, Yahya; Lindman, Björn; Alfredsson, Viveka; Topgaard, Daniel; Renamayor, Carmen S; Pacios, Isabel E

    2014-01-30

    The influence of the monomer diallyldimethylammonium chloride (D) on the lamellar liquid crystal formed by the anionic surfactant aerosol OT (AOT) and water is investigated, determining the lamellar spacings by SAXS and the quadrupolar splittings by deuterium NMR, as a function of the D or AOT concentrations. The cationic monomer D induces a destabilization of the AOT lamellar structure such that, at a critical concentration higher than 5 wt %, macroscopic phase separation takes place. When the monomer, which is dissolved in the AOT lamellae, is polymerized in situ by X-ray initiation, a new collapsed lamellar phase appears, corresponding to the complexation of the surfactant with the resulting polymer. A theoretical model is employed to analyze the variation of the interactions between the AOT bilayers and the stability of the lamellar structure.

  18. In-situ x-ray characterization of wurtzite formation in GaAs nanowires

    SciTech Connect

    Krogstrup, Peter; Hannibal Madsen, Morten; Nygaard, Jesper; Feidenhans'l, Robert; Hu Wen; Kozu, Miwa; Nakata, Yuka; Takahasi, Masamitu

    2012-02-27

    In-situ monitoring of the crystal structure formation during Ga-assisted GaAs nanowire growth on Si(111) substrates has been performed in a combined molecular beam epitaxy growth and x-ray characterization experiment. Under Ga rich conditions, we show that an increase in the V/III ratio increases the formation rate of the wurtzite structure. Moreover, the response time for changes in the structural phase formation to changes in the beam fluxes is observed to be much longer than predicted time scales of adatom kinetics and liquid diffusion. This suggests that the morphology of the growth interface plays the key role for the relative growth structure formation rates.

  19. Advanced in situ metrology for x-ray beam shaping with super precision.

    PubMed

    Wang, Hongchang; Sutter, John; Sawhney, Kawal

    2015-01-26

    We report a novel method for in situ metrology of an X-ray bimorph mirror by using the speckle scanning technique. Both the focusing beam and the "tophat" defocussed beam have been generated by optimizing the bimorph mirror in a single iteration. Importantly, we have demonstrated that the angular sensitivity for measuring the slope error of an optical surface can reach accuracy in the range of two nanoradians. When compared with conventional ex-situ metrology techniques, the method enables a substantial increase of around two orders of magnitude in the angular sensitivity and opens the way to a previously inaccessible region of slope error measurement. Such a super precision metrology technique will be beneficial for both the manufacture of polished mirrors and the optimization of beam shaping.

  20. Kinetics of Methane Hydrate Decomposition Studied via in Situ Low Temperature X-ray Powder Diffraction

    SciTech Connect

    Everett, Susan M; Rawn, Claudia J; Keffer, David J.; Mull, Derek L; Payzant, E Andrew; Phelps, Tommy Joe

    2013-01-01

    Gas hydrates are known to have a slowed decomposition rate at ambient pressure and temperatures below the melting point of ice termed self-preservation or anomalous preservation. As hydrate exothermically decomposes, gas is released and water of the clathrate cages transforms into ice. Two regions of slowed decomposition for methane hydrate, 180 200 K and 230 260 K, were observed, and the kinetics were studied by in situ low temperature x-ray powder diffraction. The kinetic constants for ice formation from methane hydrate were determined by the Avrami model within each region and activation energies, Ea, were determined by the Arrhenius plot. Ea determined from the data for 180 200 K was 42 kJ/mol and for 230 260 K was 22 kJ/mol. The higher Ea in the colder temperature range was attributed to a difference in the microstructure of ice between the two regions.

  1. Unidirectional freezing of ceramic suspensions: in situ X-ray investigation of the effects of additives.

    PubMed

    Delattre, Benjamin; Bai, Hao; Ritchie, Robert O; De Coninck, Joël; Tomsia, Antoni P

    2014-01-01

    Using in situ X-ray radiography, we investigated unidirectional freezing of titanium dioxide suspensions. We showed how processing additives, which are generally used for ice-templating, strongly modified freezing dynamics during the solidification process. We observed and identified different freezing regimes by varying the amount of dispersant, binder, or poly(ethylene glycol) (PEG). We demonstrated that because each regime corresponds to a given final structure understanding the particle motion and redistribution at the ice-front level was essential. We also examined the transition from a random particles-entrapment regime to a well-defined lamellar regime and proposed and discussed two mechanisms by which additives might affect the solidification process.

  2. Tracking the catalyzed growth process of nanowires by in situ x-ray diffraction

    NASA Astrophysics Data System (ADS)

    Kirkham, Melanie; Wang, Zhong Lin; Snyder, Robert L.

    2010-07-01

    Quasi-one-dimensional nanostructures of silicon, oxides, and other materials show great promise for a variety of applications. These nanostructures are commonly grown using metal catalyst nanoparticles. This paper investigates the growth mechanism of Au-catalyzed Si nanowires through in situ x-ray diffraction, and the results are compared to previously studied Au-catalyzed ZnO nanorods. The Si nanowires were found to grow from molten catalyst particles, however, the ZnO nanorods were found to grow from solid catalyst particles through a surface diffusion process. From this comparison, the relative bonding types of the catalyst and source material are determined to have a significant effect on the growth mechanism.

  3. Synchrotron hard X-ray imaging of shock-compressed metal powders

    NASA Astrophysics Data System (ADS)

    Rutherford, Michael E.; Chapman, David J.; Collinson, Mark A.; Jones, David R.; Music, Jasmina; Stafford, Samuel J. P.; Tear, Gareth R.; White, Thomas G.; Winters, John B. R.; Drakopoulos, Michael; Eakins, Daniel E.

    2015-06-01

    This poster will present the application of a new, high-energy (50 to 250 keV) synchrotron X-ray radiography technique to the study of shock-compressed granular materials. Following plate-impact loading, transmission radiography was used to quantitatively observe the compaction and release processes in a range of high-Z metal powders (e.g. Fe, Ni, Cu). By comparing the predictions of 3D numerical models initialized from X-ray tomograms-captured prior to loading-with experimental results, this research represents a new approach to refining mesoscopic compaction models. The authors gratefully acknowledge the ongoing support of Imperial College London, EPSRC, STFC and the Diamond Light Source, and AWE Plc.

  4. Single-crystal sapphire microstructure for high-resolution synchrotron X-ray monochromators

    DOE PAGES

    Asadchikov, Victor E.; Butashin, Andrey V.; Buzmakov, Alexey V.; Deryabin, Alexander N.; Kanevsky, Vladimir M.; Prokhorov, Igor A.; Roshchin, Boris S.; Volkov, Yuri O.; Zolotov, Dennis A.; Jafari, Atefeh; et al

    2016-03-22

    We report on the growth and characterization of several sapphire single crystals for the purpose of x-ray optics applications. Structural defects were studied by means of laboratory double-crystal X-ray diffractometry and white beam synchrotron-radiation topography. The investigations confirmed that the main defect types are dislocations. The best quality crystal was grown using the Kyropoulos technique with a dislocation density of 102-103 cm-2 and a small area with approximately 2*2 mm2 did not show dislocation contrast in many reflections and has suitable quality for application as a backscattering monochromator. As a result, a clear correlation between growth rate and dislocation densitymore » is observed, though growth rate is not the only parameter impacting the quality.« less

  5. Development of soft X-ray polarized light beamline on Indus-2 synchrotron radiation source

    SciTech Connect

    Phase, D. M. Gupta, Mukul Potdar, S. Behera, L. Sah, R. Gupta, Ajay

    2014-04-24

    This article describes the development of a soft x-ray beamline on a bending magnet source of Indus-2 storage ring (2.5 GeV) and some preliminary results of x-ray absorption spectroscopy (XAS) measurements using the same. The beamline layout is based on a spherical grating monochromator. The beamline is able to accept synchrotron radiation from the bending magnet port BL-1 of the Indus-2 ring with a wide solid angle. The large horizontal and vertical angular acceptance contributes to high photon flux and selective polarization respectively. The complete beamline is tested for ultrahigh vacuum (UHV) ∼ 10{sup −10} mbar. First absorption spectrum was obtained on HOPG graphite foil. Our performance test indicates that modest resolving power has been achieved with adequate photon flux to carry out various absorption experiments.

  6. Algorithms for three-dimensional chemical analysis via multi-energy synchrotron X-ray tomography

    NASA Astrophysics Data System (ADS)

    Ham, Kyungmin; Butler, Leslie G.

    2007-08-01

    The conversion of X-ray tomography images into three-dimensional chemical composition requires accurate mass absorption values, high-quality images, and a robust fitting algorithm. The least-squares fits of the images to a three-dimensional chemical composition can proceed with several different options such as minimal vs. over-determined and/or constrained parameters. This project has investigated the impact of XAFS features and a limited CCD dynamic range. These simulated results are compared to a recent experimental project in which synchrotron X-ray tomography was used to image a polymer blend, and from those images, calculated three-dimensional chemical composition maps of the two-component flame retardant, a brominated phthalimide dimer, Saytex ™ BT-93 and a synergist, antimony(III) oxide (Sb 2O 3).

  7. X-ray and synchrotron investigations of heterogeneous systems based on multiwalled carbon nanotubes

    NASA Astrophysics Data System (ADS)

    Sivkov, V. N.; Ob"edkov, A. M.; Petrova, O. V.; Nekipelov, S. V.; Kremlev, K. V.; Kaverin, B. S.; Semenov, N. M.; Gusev, S. A.

    2015-01-01

    This paper presents the results of a complex investigation of heterogeneous systems based on multiwalled carbon nanotubes with the outer surfaces covered by iron oxide (Fe3O4) nanocoatings deposited using iron pentacarbonyl as a precursor. Investigations were performed by the methods of electron microscopy, X-ray diffractometry, and ultrasoft X-ray spectroscopy with synchrotron radiation. It was established that the formed thin coatings are continuous and nonuniform in thickness. It was shown that good adhesion of iron oxide on the multiwalled carbon nanotube surface is provided by the formation of epoxy and double carbon-oxygen bonds; in this case, the outer graphene layer of nanotubes is not destroyed and retains the hexagonal structure.

  8. Small-angle scattering studies of meso-scopic structures with synchrotron X-rays

    NASA Astrophysics Data System (ADS)

    Dore, J. C.; North, A. N.; Rigden, J. S.

    1995-03-01

    The use of small-angle X-ray scattering techniques for the study of spatial inhomogeneities over the range 20 Å to 2 μm is reviewed. The basic formalism for scattering by an inhomogeneous medium is developed with particular reference to liquid suspensions, porous solids and solid aggregates. The instrumentation available on the Synchrotron Radiation Source at the Daresbury Laboratory is briefly presented and the use of the Bonse-Hart method for studies at ultra-low scattering angles described. The extraction of structural information for a range of natural and synthetic materials is presented with particular reference to microemulsions, porous silicas, clays and composites. The complementarity of X-ray and neutron techniques is critically reviewed and prospects for future developments, particularly for the study of anisotropic systems, are discussed.

  9. Residual strain gradient determination in metal matrix composites by synchrotron X-ray energy dispersive diffraction

    NASA Technical Reports Server (NTRS)

    Kuntz, Todd A.; Wadley, Haydn N. G.; Black, David R.

    1993-01-01

    An X-ray technique for the measurement of internal residual strain gradients near the continuous reinforcements of metal matrix composites has been investigated. The technique utilizes high intensity white X-ray radiation from a synchrotron radiation source to obtain energy spectra from small (0.001 cu mm) volumes deep within composite samples. The viability of the technique was tested using a model system with 800 micron Al203 fibers and a commercial purity titanium matrix. Good agreement was observed between the measured residual radial and hoop strain gradients and those estimated from a simple elastic concentric cylinders model. The technique was then used to assess the strains near (SCS-6) silicon carbide fibers in a Ti-14Al-21Nb matrix after consolidation processing. Reasonable agreement between measured and calculated strains was seen provided the probe volume was located 50 microns or more from the fiber/matrix interface.

  10. High-Speed Synchrotron X-ray Imaging Studies of the Ultrasound Shockwave and Enhanced Flow during Metal Solidification Processes

    NASA Astrophysics Data System (ADS)

    Tan, Dongyue; Lee, Tung Lik; Khong, Jia Chuan; Connolley, Thomas; Fezzaa, Kamel; Mi, Jiawei

    2015-07-01

    The highly dynamic behavior of ultrasonic bubble implosion in liquid metal, the multiphase liquid metal flow containing bubbles and particles, and the interaction between ultrasonic waves and semisolid phases during solidification of metal were studied in situ using the complementary ultrafast and high-speed synchrotron X-ray imaging facilities housed, respectively, at the Advanced Photon Source, Argonne National Laboratory, US, and Diamond Light Source, UK. Real-time ultrafast X-ray imaging of 135,780 frames per second revealed that ultrasonic bubble implosion in a liquid Bi-8 wt pctZn alloy can occur in a single wave period (30 kHz), and the effective region affected by the shockwave at implosion was 3.5 times the original bubble diameter. Furthermore, ultrasound bubbles in liquid metal move faster than the primary particles, and the velocity of bubbles is 70 ~ 100 pct higher than that of the primary particles present in the same locations close to the sonotrode. Ultrasound waves can very effectively create a strong swirling flow in a semisolid melt in less than one second. The energetic flow can detach solid particles from the liquid-solid interface and redistribute them back into the bulk liquid very effectively.

  11. Simultaneous X-ray fluorescence and scanning X-ray diffraction microscopy at the Australian Synchrotron XFM beamline.

    PubMed

    Jones, Michael W M; Phillips, Nicholas W; van Riessen, Grant A; Abbey, Brian; Vine, David J; Nashed, Youssef S G; Mudie, Stephen T; Afshar, Nader; Kirkham, Robin; Chen, Bo; Balaur, Eugeniu; de Jonge, Martin D

    2016-09-01

    Owing to its extreme sensitivity, quantitative mapping of elemental distributions via X-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. PMID:27577770

  12. Synchrotron-based small-angle X-ray scattering (SAXS) of proteins in solution

    PubMed Central

    Skou, Soren; Gillilan, Richard E

    2015-01-01

    Summary With recent advances in data analysis algorithms, X-ray detectors, and synchrotron sources, small-angle X-ray scattering (SAXS) has become much more accessible to the structural biology community than ever before. Although limited to ~10 Å resolution, SAXS can provide a wealth of structural information on biomolecules in solution and is compatible with a wide range of experimental conditions. SAXS is thus an attractive alternative when crystallography is not possible. Moreover, advanced usage of SAXS can provide unique insight into biomolecular behavior that can only be observed in solution, such as large conformational changes and transient protein-protein interactions. Unlike crystal diffraction data, however, solution scattering data are subtle in appearance, highly sensitive to sample quality and experimental errors, and easily misinterpreted. In addition, synchrotron beamlines that are dedicated to SAXS are often unfamiliar to the non-specialist. Here, we present a series of procedures that can be used for SAXS data collection and basic cross-checks designed to detect and avoid aggregation, concentration effects, radiation damage, buffer mismatch, and other common problems. The protein, human serum albumin (HSA), serves as a convenient and easily replicated example of just how subtle these problems can sometimes be, but also of how proper technique can yield pristine data even in problematic cases. Because typical data collection times at a synchrotron are only one to several days, we recommend that the sample purity, homogeneity, and solubility be extensively optimized prior to the experiment. PMID:24967622

  13. Experimental comparison between speckle and grating-based imaging technique using synchrotron radiation X-rays.

    PubMed

    Kashyap, Yogesh; Wang, Hongchang; Sawhney, Kawal

    2016-08-01

    X-ray phase contrast and dark-field imaging techniques provide important and complementary information that is inaccessible to the conventional absorption contrast imaging. Both grating-based imaging (GBI) and speckle-based imaging (SBI) are able to retrieve multi-modal images using synchrotron as well as lab-based sources. However, no systematic comparison has been made between the two techniques so far. We present an experimental comparison between GBI and SBI techniques with synchrotron radiation X-ray source. Apart from the simple experimental setup, we find SBI does not suffer from the issue of phase unwrapping, which can often be problematic for GBI. In addition, SBI is also superior to GBI since two orthogonal differential phase gradients can be simultaneously extracted by one dimensional scan. The GBI has less stringent requirements for detector pixel size and transverse coherence length when a second or third grating can be used. This study provides the reference for choosing the most suitable technique for diverse imaging applications at synchrotron facility.

  14. Investigation of artefact sources in synchrotron microtomography via virtual X-ray imaging

    NASA Astrophysics Data System (ADS)

    Vidal, F. P.; Létang, J. M.; Peix, G.; Cloetens, P.

    2005-06-01

    Qualitative and quantitative use of volumes reconstructed by computed tomography (CT) can be compromised due to artefacts which corrupt the data. This article illustrates a method based on virtual X-ray imaging to investigate sources of artefacts which occur in microtomography using synchrotron radiation. In this phenomenological study, different computer simulation methods based on physical X-ray properties, eventually coupled with experimental data, are used in order to compare artefacts obtained theoretically to those present in a volume acquired experimentally, or to predict them for a particular experimental setup. The article begins with the presentation of a synchrotron microtomographic slice of a reinforced fibre composite acquired at the European Synchrotron Radiation Facility (ESRF) containing streak artefacts. This experimental context is used as the motive throughout the paper to illustrate the investigation of some artefact sources. First, the contribution of direct radiation is compared to the contribution of secondary radiations. Then, the effect of some methodological aspects are detailed, including under-sampling, sample and camera misalignment, sample extending outside of the field of view and photonic noise. The effect of harmonic components present in the experimental spectrum are also simulated. Afterwards, detector properties, such as its impulse response or defective pixels, are taken into account. Finally, the importance of phase contrast effects is evaluated. In the last section, this investigation is discussed by putting emphasis on the experimental context which is used throughout this paper.

  15. Calibration of a compact XUV soft X-ray monochromator with a digital autocollimator in situ.

    PubMed

    Yuh, Jih Young; Lin, Shang Wei; Huang, Liang Jen; Lee, Long Life

    2016-09-01

    A digital autocollimator of resolution 0.1 µrad (0.02 arcsec) serves as a handy correction tool for calibrating the angular uncertainty during angular and lateral movements of gratings inside a monochromator chamber under ultra-high vacuum. The photon energy dispersed from the extreme ultraviolet (XUV) to the soft X-ray region of the synchrotron beamline at the Taiwan Light Source was monitored using molecular ionization spectra at high resolution as energy references that correlate with the fine angular steps during grating rotation. The angular resolution of the scanning mechanism was <0.3 µrad, which results in an energy shift of 80 meV at 867 eV. The angular uncertainties caused by the lateral movement during a grating exchange were decreased from 2.2 µrad to 0.1 µrad after correction. The proposed method provides a simple solution for on-site beamline diagnostics of highly precise multi-axis optical manipulating instruments at synchrotron facilities and in-house laboratories. PMID:27577780

  16. Calibration of a compact XUV soft X-ray monochromator with a digital autocollimator in situ.

    PubMed

    Yuh, Jih Young; Lin, Shang Wei; Huang, Liang Jen; Lee, Long Life

    2016-09-01

    A digital autocollimator of resolution 0.1 µrad (0.02 arcsec) serves as a handy correction tool for calibrating the angular uncertainty during angular and lateral movements of gratings inside a monochromator chamber under ultra-high vacuum. The photon energy dispersed from the extreme ultraviolet (XUV) to the soft X-ray region of the synchrotron beamline at the Taiwan Light Source was monitored using molecular ionization spectra at high resolution as energy references that correlate with the fine angular steps during grating rotation. The angular resolution of the scanning mechanism was <0.3 µrad, which results in an energy shift of 80 meV at 867 eV. The angular uncertainties caused by the lateral movement during a grating exchange were decreased from 2.2 µrad to 0.1 µrad after correction. The proposed method provides a simple solution for on-site beamline diagnostics of highly precise multi-axis optical manipulating instruments at synchrotron facilities and in-house laboratories.

  17. In Situ Density Measurement of Basaltic Melts at High Pressure by X-ray Absorption Method

    NASA Astrophysics Data System (ADS)

    Ando, R.; Ohtani, E.; Suzuki, A.; Urakawa, S.; Katayama, Y.

    2004-12-01

    Density of silicate melt at high pressure is one of the most important properties to understand magma migration in the planetary interior. However, because of experimental difficulties, the density of magma at high pressure is poorly known. Katayama et al. (1996) recently developed a new in situ density measurement method for metallic melts, based on the density dependency of X-ray absorption in the sample. In this study, we tried to measure the density of basaltic melt by this absorption method. When X-ray is transmitted to the sample, the intensity of the transmitted X-ray beam (I) is expressed as follows; I=I0exp(-μ ρ t), where I0 is the intensity of incident X-ray beam, μ is the mass absorption coefficient, ρ is the density of the sample, and t is the thickness of the sample. If t and μ are known, we can determine the density of the sample by measuring I and I0. This is the principle of the absorption method for density measurement. In this study, in order to determine t, we used a single crystalline diamond cylinder as a sample capsule, diamond is less compressive and less deformable so that even at high pressure t (thickness of the sample at the point x) is expressed as follows; t = 2*(R02-x2)1/2, R0 is the inner radius of cylinder at the ambient condition, and x is distance from a center of the capsule. And diamond also shows less absorption so that this make it possible to measure the density of silicate melt with smaller absorption coefficient than metallic melts. In order to know the μ of the sample, we measured both densities (ρ ) and absorptions (I/I0) for some glasses and crystals with same composition of the sample at the ambient condition, and calculated as fallows; μ =ln(I/I0)/ρ . Experiments were made at the beamline (BL22XU) of SPring-8. For generation of high pressure and high temperature, we used DIA-type cubic anvil apparatus (SMAP180) there. We used tungsten carbide anvils with the edge-length of 6 mm. The energy of monochromatic X-ray

  18. Defect characterization and stress analysis by white beam synchrotron X-ray topography in single crystal semiconducting materials

    NASA Astrophysics Data System (ADS)

    Sarkar, Vishwanath

    as a function of depth in a single crystal material. This novel technique, an extension of SMART technique is developed to determine stress tensor components at various depths within the crystal. In reflection geometry penetration depth is controlled by manipulating the geometrical parameters such as incident angle. Data is obtained from various penetration depth, which represents exponentially decaying weighted average of actual stress value or in other words this stress profile is Laplace transform of real stress profile. Mathematical procedure is described to determine real stress profile from Laplace profile. To demonstrate this method, a packaged semiconducting Silicon die is used and its complete stress tensor profile is generated. This method has demonstrated the capability of determining all six components of stress as a function of depth in the crystal. Experimental procedure, theoretical basis and mathematical methods along with its application, capability and limitations are discussed. Wafer dicing process results in edge and surface damage. Various characterization tools were used to detect these defects. Surface reflection topographs were taken to probe surface and subsurface defects, primarily scratches and micro cracks. Optical microscopy and SEM were used as a complementary tool for surface characterization. TEM is used for detecting sub-surface nano-cracks and dislocations. X-ray transmission topography is used to detect half loop dislocations resulting from dicing process. In order to study dynamic behavior of defects (dislocations) during thermal processing and operation an environmental chamber (furnace) is designed and built to record in-situ X-ray diffraction topographs during thermal cycling and at high temperature.

  19. New insights into globoids of protein storage vacuoles in wheat aleurone using synchrotron soft X-ray microscopy

    PubMed Central

    Regvar, Marjana; Eichert, Diane; Kaulich, Burkhard; Gianoncelli, Alessandra; Pongrac, Paula; Vogel-Mikuš, Katarina; Kreft, Ivan

    2011-01-01

    Mature developed seeds are physiologically and biochemically committed to store nutrients, principally as starch, protein, oils, and minerals. The composition and distribution of elements inside the aleurone cell layer reflect their biogenesis, structural characteristics, and physiological functions. It is therefore of primary importance to understand the mechanisms underlying metal ion accumulation, distribution, storage, and bioavailability in aleurone subcellular organelles for seed fortification purposes. Synchrotron radiation soft X-ray full-field imaging mode (FFIM) and low-energy X-ray fluorescence (LEXRF) spectromicroscopy were applied to characterize major structural features and the subcellular distribution of physiologically important elements (Zn, Fe, Na, Mg, Al, Si, and P). These direct imaging methods reveal the accumulation patterns between the apoplast and symplast, and highlight the importance of globoids with phytic acid mineral salts and walls as preferential storage structures. C, N, and O chemical topographies are directly linked to the structural backbone of plant substructures. Zn, Fe, Na, Mg, Al, and P were linked to globoid structures within protein storage vacuoles with variable levels of co-localization. Si distribution was atypical, being contained in the aleurone apoplast and symplast, supporting a physiological role for Si in addition to its structural function. These results reveal that the immobilization of metals within the observed endomembrane structures presents a structural and functional barrier and affects bioavailability. The combination of high spatial and chemical X-ray microscopy techniques highlights how in situ analysis can yield new insights into the complexity of the wheat aleurone layer, whose precise biochemical composition, morphology, and structural characteristics are still not unequivocally resolved. PMID:21447756

  20. New insights into globoids of protein storage vacuoles in wheat aleurone using synchrotron soft X-ray microscopy.

    PubMed

    Regvar, Marjana; Eichert, Diane; Kaulich, Burkhard; Gianoncelli, Alessandra; Pongrac, Paula; Vogel-Mikus, Katarina; Kreft, Ivan

    2011-07-01

    Mature developed seeds are physiologically and biochemically committed to store nutrients, principally as starch, protein, oils, and minerals. The composition and distribution of elements inside the aleurone cell layer reflect their biogenesis, structural characteristics, and physiological functions. It is therefore of primary importance to understand the mechanisms underlying metal ion accumulation, distribution, storage, and bioavailability in aleurone subcellular organelles for seed fortification purposes. Synchrotron radiation soft X-ray full-field imaging mode (FFIM) and low-energy X-ray fluorescence (LEXRF) spectromicroscopy were applied to characterize major structural features and the subcellular distribution of physiologically important elements (Zn, Fe, Na, Mg, Al, Si, and P). These direct imaging methods reveal the accumulation patterns between the apoplast and symplast, and highlight the importance of globoids with phytic acid mineral salts and walls as preferential storage structures. C, N, and O chemical topographies are directly linked to the structural backbone of plant substructures. Zn, Fe, Na, Mg, Al, and P were linked to globoid structures within protein storage vacuoles with variable levels of co-localization. Si distribution was atypical, being contained in the aleurone apoplast and symplast, supporting a physiological role for Si in addition to its structural function. These results reveal that the immobilization of metals within the observed endomembrane structures presents a structural and functional barrier and affects bioavailability. The combination of high spatial and chemical X-ray microscopy techniques highlights how in situ analysis can yield new insights into the complexity of the wheat aleurone layer, whose precise biochemical composition, morphology, and structural characteristics are still not unequivocally resolved.

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

    PubMed

    Bein, Benjamin; Hsing, Hsiang-Chun; Callori, Sara J; Sinsheimer, John; Chinta, Priya V; Headrick, Randall L; Dawber, Matthew

    2015-12-04

    In 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 BaTiO3/SrTiO3 superlattices on SrTiO3 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. Effects of electric boundary conditions are investigated by growing the same superlattice alternatively on SrTiO3 substrates and 20 nm SrRuO3 thin films on SrTiO3 substrates. These experiments provide important insights into the formation and evolution of ferroelectric domains when the sample is ferroelectric during the growth process.

  2. 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.; Sinsheimer, John; Chinta, Priya V.; Headrick, Randall L.; Dawber, Matthew

    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 BaTiO3/SrTiO3 superlattices on SrTiO3 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. Effects of electric boundarymore » conditions are investigated by growing the same superlattice alternatively on SrTiO3 substrates and 20 nm SrRuO3 thin films on SrTiO3 substrates. Our experiments provide important insights into the formation and evolution of ferroelectric domains when the sample is ferroelectric during the growth process.« less

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

    SciTech Connect

    Bein, Benjamin; Hsing, Hsiang-Chun; Callori, Sara J.; Sinsheimer, John; Chinta, Priya V.; Headrick, Randall L.; Dawber, Matthew

    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 BaTiO3/SrTiO3 superlattices on SrTiO3 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. Effects of electric boundary conditions are investigated by growing the same superlattice alternatively on SrTiO3 substrates and 20 nm SrRuO3 thin films on SrTiO3 substrates. Our experiments provide important insights into the formation and evolution of ferroelectric domains when the sample is ferroelectric during the growth process.

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

    PubMed Central

    Bein, Benjamin; Hsing, Hsiang-Chun; Callori, Sara J.; Sinsheimer, John; Chinta, Priya V.; Headrick, Randall L.; Dawber, Matthew

    2015-01-01

    In 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 BaTiO3/SrTiO3 superlattices on SrTiO3 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. Effects of electric boundary conditions are investigated by growing the same superlattice alternatively on SrTiO3 substrates and 20 nm SrRuO3 thin films on SrTiO3 substrates. These experiments provide important insights into the formation and evolution of ferroelectric domains when the sample is ferroelectric during the growth process. PMID:26634894

  5. Versatile plug flow catalytic cell for in situ transmission/fluorescence x-ray absorption fine structure measurements

    SciTech Connect

    Centomo, P.; Zecca, M.; Meneghini, C.

    2013-05-15

    A novel flow-through catalytic cell has been developed for in situ x-ray absorption spectroscopy (XAS) experiments on heterogeneous catalysts under working conditions and in the presence of a liquid and a gas phase. The apparatus allows to carry out XAS measurements in both the transmission and fluorescence modes, at moderate temperature (from RT to 50-80 Degree-Sign C) and low-medium gas pressure (up to 7-8 bars). The materials employed are compatible with several chemicals such as those involved in the direct synthesis of hydrogen peroxide (O{sub 2}, H{sub 2}, H{sub 2}O{sub 2}, methanol). The versatile design of the cell allows to fit it to different experimental setups in synchrotron radiation beamlines. It was used successfully for the first time to test nanostructured Pd catalysts during the direct synthesis of hydrogen peroxide (H{sub 2}O{sub 2}) in methanol solution from dihydrogen and dioxygen.

  6. Dissolution dynamics of the calcite-water interface observed in situ by glancing-incidence X-ray scattering

    SciTech Connect

    Sturchio, N.C.; Chiarello, R.P.

    1995-06-02

    Glancing-incidence X-ray scattering measurements made at the National Synchrotron Light Source were used to investigate dissolution dynamics in situ at the calcite-water interface. The relation between calcite saturation state and roughness of the calcite (1014) cleavage surface as a function of time was examined during pH titrations of an initially calcite-saturated solution. Systematic variations in roughness were observed as a function of saturation state as pH was titrated to values below that of calcite saturation. Different steady-state values of roughness were evident at fixed values of {Delta}G{sub r}, and these were correlated with the extent of undersaturation. A significant increase in roughness begins to occur with increasing undersaturation at a {Delta}G{sub r} value of approximately {minus}2.0 kcal/mol. The dissolution rate corresponding to this increase is about 1.5 x 10{sup 7} mmol/cm {center_dot} sec. This increase in roughness is attributed to a transition in the principal rate-determining dissolution mechanism, and is consistent with both powder-reaction studies of dissolution kinetics and single-crystal dissolution studies by atomic force microscopy. These data indicate some important potential applications of GIXS in the study of mineral-water interface geochemistry.

  7. Biological X-ray spectroscopy on 3rd generation synchrotron radiation sources

    NASA Astrophysics Data System (ADS)

    Ralston, Corie Y.; Chen, Jie; Peng, Gang; George, Simon J.; van Elp, Jan; Cramer, Stephen P.

    1995-02-01

    Third generation synchrotron radiation sources such as the Advanced Light Source (ALS) at Lawrence Berkeley Laboratory deliver 1-2 orders of magnitude more monochromatic flux (and many orders of magnitude higher brightness) than previously available. This paper describes the ring and existing beamlines of the advanced light source, and plans for crystallography and elliptical wiggler stations are discussed. Using nickel metalloprotein spectra recorded at NSLS and SSRL as examples, this paper describes how the higher monochromatic flux available from the ALS will be used for biological soft X-ray spectroscopy.

  8. Synchrotron X-ray Optics Testing at Beamline 1-BM at the Advanced Photon Source

    NASA Astrophysics Data System (ADS)

    Macrander, Albert; Kujala, Naresh

    2014-03-01

    Beamline 1-BM at the Advanced Photon Source has been reconfigured, in part for testing of synchrotron optics with both monochromatic and white beams. Monochromatic energies between 6 and 30 keV are available. Primary agendas include both white beam and monochromatic beam topography, Talbot grating interferometry for measurement of coherence lengths and wavefronts, and micro-focusing. Recent examples will include topography of sapphire , tests of Kirkpatrick-Baez mirrors, and tests of multilayer Laue lenses. Analyzers for Inelastic X-ray Scattering has also been characterized by two user groups. Supported from U.S. DOE, Office of Science, Contract No. DE-AC-02-06CH11357.

  9. Microscopy and elemental analysis in tissue samples using computed microtomography with synchrotron x-rays

    SciTech Connect

    Spanne, P.; Rivers, M.L.

    1988-01-01

    The initial development shows that CMT using synchrotron x-rays can be developed to ..mu..m spatial resolution and perhaps even better. This creates a new microscopy technique which is of special interest in morphological studies of tissues, since no chemical preparation or slicing of the sample is necessary. The combination of CMT with spatial resolution in the ..mu..m range and elemental mapping with sensitivity in the ppM range results in a new tool for elemental mapping at the cellular level. 7 refs., 1 fig.

  10. A magnetizing system for dichroism measurements in soft x-ray emission excited by synchrotron radiation

    SciTech Connect

    Dallera, C.; Ghiringhelli, G.; Braicovich, L.

    1996-02-01

    We present the design and performance of a magnetic circuit suitable for magnetizing solid samples in the measurements of soft x-ray emission dichroism excited by synchrotron radiation. The system allows a variety of samples to be magnetized and satisfies the rather stringent geometrical constraints due to the need for minimizing the effect of photon self-absorption by the sample. The magnetic circuit is ultrahigh vacuum compatible, can reach about 2800 G, and allows fine adjustment of sample position. {copyright} {ital 1996 American Institute of Physics.}

  11. Load transfer in bovine plexiform bone determined by synchrotron x-ray diffraction.

    SciTech Connect

    Akhtar, R.; Daymond, M.; Almer, J.; Mummery, P.; The Univ. of Manchester; Queen's Univ.

    2008-02-01

    High-energy synchrotron x-ray diffraction (XRD) has been used to quantify load transfer in bovine plexiform bone. By using both wide-angle and small-angle XRD, strains in the mineral as well as the collagen phase of bone were measured as a function of applied compressive stress. We suggest that a greater proportion of the load is borne by the more mineralized woven bone than the lamellar bone as the applied stress increases. With a further increase in stress, load is shed back to the lamellar regions until macroscopic failure occurs. The reported data fit well with reported mechanisms of microdamage accumulation in bovine plexiform bone.

  12. A Optical Synchrotron Nebula around the X-Ray Pulsar 0540-693

    NASA Astrophysics Data System (ADS)

    Chanan, G.; Helfand, D.; Reynolds, S.

    The authors report the discovery of extended optical continuum emission around the recently discovered 50 ms X-ray pulsar in the supernova remnant 0540-693. Exposures in blue and red broadband filters made with the CTIO 4 m telescope and prime focus CCD show a center-brightened but clearly extended nebula about 4arcsec in diameter (FWHM), while an image in an [O III] filter shows an 8arcsec diameter shell (as reported earlier) which encloses the continuum source. 0540-693 is a system very similar to the Crab nebula and represents the second detection of optical synchrotron radiation in a supernova remnant.

  13. An x-ray fluorescence study of lake sediments from ancient Turkey using synchrotron radiation.

    SciTech Connect

    Alatas, A.; Alp, E. E.; Friedman, E. S.; Jennings, G.; Johnson, C. E.; Lai, B.; Mini, S. M.; Sato, Y.; Wilkinson, T. J.; Yener, K. A.

    1999-03-10

    Sediments from relic Lake Golbasi were analyzed by X-ray fluorescence with synchrotrons radiation to determine changes in element concentrations over time with selected elements serving as proxies for environmental change. Increases in Ca and Sr suggest soil formation during a dry period, from ca. 4500 BC to ca. 200 AD at which point K, Rb, Zr, Ti, and Y increase, indicating the return of a wet environment. Soil erosion, represented by Cr and Ni, increases ca. 7000 BC, probably as a consequence of environmental change, prior to suggested exploitation of natural resources by the newly urbanized society of the third millennium BC.

  14. Synchrotron total reflection X-ray fluorescence at BL-16 microfocus beamline of Indus-2

    SciTech Connect

    Tiwari, M. K. Singh, A. K. Das, Gangadhar Chowdhury, Anupam Lodha, G. S.

    2014-04-24

    Determination of ultra trace elements is important in many disciplines both in basic and applied sciences. Numerous applications show their importance in medical science, environmental science, materials science, food processing and semiconductor industries and in maintaining the quality control of ultra pure chemicals and reagents. We report commissioning of a synchrotron based total reflection x-ray fluorescence (TXRF) facility on the BL-16 microfocus beamline of Indus-2. This paper describes the performance of the BL-16 TXRF spectrometer and the detailed description of its capabilities through examples of measured results.

  15. Compressible cake filtration: monitoring cake formation and shrinkage using synchrotron X-rays

    SciTech Connect

    Bierck, B.R.; Wells, S.A.; Dick, R.I.

    1988-05-01

    High energy, highly collimated X-rays produced at the Cornell High Energy Synchrotron Sources (CHESS) enabled real-time suspended solids concentration measurements each second with 0.5 mm vertical separation in a kaolin filter cake. Suspended solids concentration profiles reflected expected effects of cumulative fluid drag forces. Shrinkage caused a significant increase in average cake suspended solids concentration after expiration of the slurry, and the saturated cake ultimately formed was virtually homogeneous. Shrinkage is consolidation under compressive forces created when capillary menisci form at air/liquid interfaces, and has a significant effect on cake structure in latter stages of compressible cake filtration.

  16. Synchrotron X-ray imaging of nanomagnetism in meteoritic metal (Invited)

    NASA Astrophysics Data System (ADS)

    Bryson, J. F.; Herrero Albillos, J.; Kronast, F.; Tyliszczak, T.; Redfern, S. A.; van der Laan, G.; Harrison, R. J.

    2013-12-01

    It is becoming increasingly apparent that a wealth of paleomagnetic information is stored at the nanoscale within natural samples. To date, this nanopaleomagetism has been investigated using high resolution magnetic microscopies, such as electron holography. Although unparalleled in its spatial resolution, electron holography produces images that are indirectly related to the magnetisation state of the sample, introducing ambiguity when interpreting magnetisation information. Holography also requires extensive off-line processing, making it unsuitable for studying dynamic processes, and the sample preparation negates the study of natural remanences. Here we demonstrate the capabilities of a new generation of nanomagnetic imaging methods using synchrotron X-ray radiation. X-rays tuned to an elemental absorption edge can display differing excitation probabilities depending on the orientation of an electron's magnetic moment relative to that of the X-ray beam. This is achieved by introducing an angular momentum to the photon through circular polarisation, resulting in an absorption signal that is proportional to the projection of the magnetic moment on to the X-ray beam direction. We introduce and compare two experimental set-ups capable of spatially resolving these signals to form a high-resolution magnetisation map: photoemission electron microscopy and scanning transmission electron microscopy. Both techniques provide measurements of magnetisation with 30-50nm resolution and elemental specificity. Photoemission electron microscopy can be used also to create maps of all three of the spatial components of magnetisation and investigate dynamic magnetic switching processes. The full capabilities of X-ray imaging are demonstrated through the application of both of these techniques to meteoritic metal. We show that the 'cloudy zone' within iron meteorites contains nanoscale islands of tetrataenite (FeNi) that are populated equally by all three possible magnetic easy axes

  17. In situ characterization of aluminum-containing mineral-microorganism aqueous suspensions using scanning transmission X-ray microscopy.

    PubMed

    Yoon, Tae Hyun; Johnson, Stephen B; Benzerara, Karim; Doyle, Colin S; Tyliszczak, Tolek; Shuh, David K; Brown, Gordon E

    2004-11-23

    In situ characterization of colloidal particles under hydrous conditions is one of the key requirements for understanding their state of aggregation and impact on the transport of pollutants in aqueous environments. Scanning transmission X-ray microscopy (STXM) is one of the few techniques that can satisfy this need by providing element- and chemical-state-specific 2-D maps at a spatial resolution better than 50 nm using soft X-rays from synchrotron radiation wiggler or undulator sources tuned to the absorption edges of different elements. X-ray absorption near-edge structure (XANES) spectra can also be collected simultaneously at a similar spatial resolution and can provide phase identification in many cases. In this study, we report STXM images and XANES spectroscopy measurements at or above the Al K-edge (E = 1559.6 eV) of various Al-containing minerals and synthetic oxides [alpha-Al2O3 (corundum), gamma-Al2O3, gamma-AlOOH (boehmite), alpha-Al(OH)3 (bayerite), KAl2(AlSi3O10)(OH)2 (muscovite), (Al,Mg)8(Si4O10)4(OH)8.nH2O (montmorillonite), and Mg6Al2(OH)16CO3.4H2O (hydrotalcite)] and demonstrate the capability of this spectromicroscopic tool to identify different Al-containing mineral colloids in multiphase mixtures in aqueous solution. We also demonstrate that STXM imaging at or above the C K-edge (E = 284.2 eV) and Al K-edge can provide unique information on the interactions between bacteria and Al-containing nanoparticles in aqueous suspensions. STXM images of a mixture of Caulobacter crescentus and montmorillonite and corundum particles just above the C and Al K-edges show that the mineral particles and bacteria are closely associated in aggregates, which is likely due to the binding of bacteria to clay and corundum particles by extracellular polysaccharides.

  18. New Insights into Chain Order Dynamics and Structural Development in Sulfur-Vulcanized Natural Rubber Latex using Multiple Quantum NMR and Synchrotron X-Ray Diffraction

    NASA Astrophysics Data System (ADS)

    Che, Justin; Toki, Shigeyuki; Valentin, Juan; Brasero, Justo; Rong, Lixia; Hsiao, Benjamin S.

    2012-02-01

    Network structure, chain dynamics, and structural development in sulfur-vulcanized natural rubber latex were studied by Multiple-Quantum (MQ) NMR and synchrotron x-ray scattering. Three important processes that can influence rubber network structure and its overall mechanical properties were the main focus and analyzed by both of these techniques: pre-vulcanization, drying, and post-vulcanization. MQ NMR experiments can provide quantitative information regarding networks at very small length scales, including network defects, number of cross-links, and spatial distribution of cross-links. Structural development in natural rubber was studied under uniaxial deformation by in-situ synchrotron x-ray diffraction, which can provide information on network structures at much larger length scales. Molecular orientation and strain-induced crystallization was analyzed by both stress-strain relations and wide-angle x-ray diffraction (WAXD). The morphology of the latex rubber particle during deformation was analyzed by small-angle x-ray scattering (SAXS). The combination of these techniques can provide a considerable amount of information regarding rubber network structure.

  19. In Situ Ambient Pressure X-ray Photoelectron Spectroscopy Studies of Lithium-Oxygen Redox Reactions

    PubMed Central

    Lu, Yi-Chun; Crumlin, Ethan J.; Veith, Gabriel M.; Harding, Jonathon R.; Mutoro, Eva; Baggetto, Loïc; Dudney, Nancy J.; Liu, Zhi; Shao-Horn, Yang

    2012-01-01

    The lack of fundamental understanding of the oxygen reduction and oxygen evolution in nonaqueous electrolytes significantly hinders the development of rechargeable lithium-air batteries. Here we employ a solid-state Li4+xTi5O12/LiPON/LixV2O5 cell and examine in situ the chemistry of Li-O2 reaction products on LixV2O5 as a function of applied voltage under ultra high vacuum (UHV) and at 500 mtorr of oxygen pressure using ambient pressure X-ray photoelectron spectroscopy (APXPS). Under UHV, lithium intercalated into LixV2O5 while molecular oxygen was reduced to form lithium peroxide on LixV2O5 in the presence of oxygen upon discharge. Interestingly, the oxidation of Li2O2 began at much lower overpotentials (~240 mV) than the charge overpotentials of conventional Li-O2 cells with aprotic electrolytes (~1000 mV). Our study provides the first evidence of reversible lithium peroxide formation and decomposition in situ on an oxide surface using a solid-state cell, and new insights into the reaction mechanism of Li-O2 chemistry. PMID:23056907

  20. A feasibility study of dynamic stress analysis inside a running internal combustion engine using synchrotron X-ray beams.

    PubMed

    Baimpas, Nikolaos; Drakopoulos, Michael; Connolley, Thomas; Song, Xu; Pandazaras, Costas; Korsunsky, Alexander M

    2013-03-01

    The present investigation establishes the feasibility of using synchrotron-generated X-ray beams for time-resolved in situ imaging and diffraction of the interior components of an internal combustion engine during its operation. The demonstration experiment was carried out on beamline I12 (JEEP) at Diamond Light Source, UK. The external hutch of the JEEP instrument is a large-scale engineering test bed for complex in situ processing and simulation experiments. The hutch incorporates a large capacity translation and rotation table and a selection of detectors for monochromatic and white-beam diffraction and imaging. These capabilities were used to record X-ray movies of a motorcycle internal combustion engine running at 1850 r.p.m. and to measure strain inside the connecting rod via stroboscopic X-ray diffraction measurement. The high penetrating ability and high flux of the X-ray beam at JEEP allowed the observation of inlet and outlet valve motion, as well as that of the piston, connecting rod and the timing chain within the engine. Finally, the dynamic internal strain within the moving connecting rod was evaluated with an accuracy of ~50 × 10(-6). PMID:23412489

  1. A feasibility study of dynamic stress analysis inside a running internal combustion engine using synchrotron X-ray beams.

    PubMed

    Baimpas, Nikolaos; Drakopoulos, Michael; Connolley, Thomas; Song, Xu; Pandazaras, Costas; Korsunsky, Alexander M

    2013-03-01

    The present investigation establishes the feasibility of using synchrotron-generated X-ray beams for time-resolved in situ imaging and diffraction of the interior components of an internal combustion engine during its operation. The demonstration experiment was carried out on beamline I12 (JEEP) at Diamond Light Source, UK. The external hutch of the JEEP instrument is a large-scale engineering test bed for complex in situ processing and simulation experiments. The hutch incorporates a large capacity translation and rotation table and a selection of detectors for monochromatic and white-beam diffraction and imaging. These capabilities were used to record X-ray movies of a motorcycle internal combustion engine running at 1850 r.p.m. and to measure strain inside the connecting rod via stroboscopic X-ray diffraction measurement. The high penetrating ability and high flux of the X-ray beam at JEEP allowed the observation of inlet and outlet valve motion, as well as that of the piston, connecting rod and the timing chain within the engine. Finally, the dynamic internal strain within the moving connecting rod was evaluated with an accuracy of ~50 × 10(-6).

  2. First use of portable system coupling X-ray diffraction and X-ray fluorescence for in-situ analysis of prehistoric rock art.

    PubMed

    Beck, L; Rousselière, H; Castaing, J; Duran, A; Lebon, M; Moignard, B; Plassard, F

    2014-11-01

    Study of prehistoric art is playing a major role in the knowledge of human evolution. Many scientific methods are involved in this investigation including chemical analysis of pigments present on artefacts or applied to cave walls. In the past decades, the characterization of coloured materials was carried on by taking small samples. This procedure had two main disadvantages: slight but existing damage of the paintings and limitation of the number of samples. Thanks to the advanced development of portable systems, in-situ analysis of pigment in cave can be now undertaken without fear for this fragile Cultural Heritage. For the first time, a portable system combining XRD and XRF was used in an underground and archaeological environment for prehistoric rock art studies. In-situ non-destructive analysis of black prehistoric drawings and determination of their composition and crystalline structure were successfully carried out. Original results on pigments used 13,000 years ago in the cave of Rouffignac (France) were obtained showing the use of two main manganese oxides: pyrolusite and romanechite. The capabilities of the portable XRD-XRF system have been demonstrated for the characterization of pigments as well as for the analysis of rock in a cave environment. This first in-situ experiment combining X-ray diffraction and X-ray fluorescence open up new horizons and can fundamentally change our approach of rock art studies.

  3. Multilayer-based soft X-ray polarimeter at the Beijing Synchrotron Radiation Facility

    NASA Astrophysics Data System (ADS)

    Sun, Li-Juan; Cui, Ming-Qi; Zhu, Jie; Zhao, Yi-Dong; Zheng, Lei; Wang, Zhan-Shan; Zhu, Jing-Tao

    2013-07-01

    A compact high precision eight-axis automatism and two-axis manual soft-ray polarimeter with a multilayer has been designed, constructed, and installed in 3W1B at the Beijing Synchrotron Radiation Facility (BSRF). Four operational modes in the same device, which are double-reflection, double-transmission, front-reflection-behind-transmission and front-transmission-behind-reflection, have been realized. It can be used for the polarization analysis of synchrotron radiation. It also can be used to characterize the polarization properties of the optical elements in the soft X-ray energy range. Some experiments with Mo/Si and Cr/C multilayers have been performed by using this polarimeter with good results obtained.

  4. Synchrotron X-ray CT characterization of titanium parts fabricated by additive manufacturing. Part II. Defects.

    PubMed

    Scarlett, Nicola Vivienne Yorke; Tyson, Peter; Fraser, Darren; Mayo, Sheridan; Maksimenko, Anton

    2016-07-01

    Synchrotron X-ray tomography (SXRT) has been applied to the study of defects within three-dimensional printed titanium parts. These parts were made using the Arcam EBM(®) (electron beam melting) process which uses powdered titanium alloy, Ti64 (Ti alloy with approximately 6%Al and 4%V) as the feed and an electron beam for the sintering/welding. The experiment was conducted on the Imaging and Medical Beamline of the Australian Synchrotron. The samples represent a selection of complex shapes with a variety of internal morphologies. Inspection via SXRT has revealed a number of defects which may not otherwise have been seen. The location and nature of such defects combined with detailed knowledge of the process conditions can contribute to understanding the interplay between design and manufacturing strategy. This fundamental understanding may subsequently be incorporated into process modelling, prediction of properties and the development of robust methodologies for the production of defect-free parts.

  5. High Resolution X-Ray Microangiography of 4T1 Tumor in Mouse Using Synchrotron Radiation

    SciTech Connect

    Sun Jianqi; Liu Ping; Gu Xiang; Liu Xiaoxia; Zhao Jun; Xiao Tiqiao; Xu, Lisa X.

    2010-07-23

    Angiogenesis is very important in tumor growth and metastasis. But in clinic, only vessels lager than 200 {mu}m in diameter, can be observed using conventional medical imaging. Synchrotron radiation (SR) phase contrast imaging, whose spatial resolution can reach as high as 1 {mu}m, has great advantages in imaging soft tissue structures, such as blood vessels and tumor tissues. In this paper, the morphology of newly formed micro-vessels in the mouse 4T1 tumor samples was firstly studied with contrast agent. Then, the angiogenesis in nude mice tumor window model was observed without contrast agent using the SR phase contrast imaging at the beamline for X-ray imaging and biomedical applications, Shanghai Synchrotron Radiation Facility (SSRF). The images of tumors showed dense, irregular and tortuous tumor micro-vessels with the smallest size of 20-30 {mu}m in diameter.

  6. Synchrotron X-ray CT characterization of titanium parts fabricated by additive manufacturing. Part II. Defects.

    PubMed

    Scarlett, Nicola Vivienne Yorke; Tyson, Peter; Fraser, Darren; Mayo, Sheridan; Maksimenko, Anton

    2016-07-01

    Synchrotron X-ray tomography (SXRT) has been applied to the study of defects within three-dimensional printed titanium parts. These parts were made using the Arcam EBM(®) (electron beam melting) process which uses powdered titanium alloy, Ti64 (Ti alloy with approximately 6%Al and 4%V) as the feed and an electron beam for the sintering/welding. The experiment was conducted on the Imaging and Medical Beamline of the Australian Synchrotron. The samples represent a selection of complex shapes with a variety of internal morphologies. Inspection via SXRT has revealed a number of defects which may not otherwise have been seen. The location and nature of such defects combined with detailed knowledge of the process conditions can contribute to understanding the interplay between design and manufacturing strategy. This fundamental understanding may subsequently be incorporated into process modelling, prediction of properties and the development of robust methodologies for the production of defect-free parts. PMID:27359151

  7. In situ X-ray diffraction study of post-spinel transformation in peridotite mantle: Implication to 660 km discontinuity

    NASA Astrophysics Data System (ADS)

    Litasov, K.; Ohtani, E.; Suzuki, A.; Funakoshi, K.

    2004-12-01

    The 660-km seismic discontinuity in the Earth's mantle is identified with the transformation of ringwoodite (spinel (Mg,Fe)2SiO4-phase) to (Mg,Fe)SiO3-perovskite and (Mg,Fe)O-ferropericlase. It was suggested using quench experiments that the transformation boundary has significant negative Clapeyron slope (-3 MPa/K, Ito and Takahashi, 1989) responsible for depressions and elevations of the 660-km discontinuity in subduction zones and hot spots of mantle plumes. Recent in situ x-ray diffraction studies in Mg2SiO4 system indicate that negative slope of the boundary is much gentler (-1.3 MPa/K) (Fei et al., 2004). Therefore there must be another factors resulting in significant depth variations of the 660-km discontinuity. In this study, we present the phase relations in anhydrous pyrolite by in situ X-ray diffraction measurements to examine the influence of additional components and Mg/Si-ratio on post-spinel phase transformation. Experiments were carried out using Speed-1500 multianvil apparatus installed at BL04B1 at synchrotron radiation facility `Spring-8' (Hyogo, Japan). Starting materials were synthetic glass representing SiO2-Al2O3-FeO-MgO-CaO-pyrolite. Graphite capsule were used as a sample container. Co-doped MgO was used as the pressure medium and a cylindrical LaCrO3 heater was used as the heating element. Temperature was measured with a WRe thermocouple. Different equation of states for Au and MgO was used for pressure calibration. The phase relations were determined at 20-25 GPa and temperature up to 2300 K. We observed easy nucleation of Mg-perovskite and ferropericlase from ringwoodite-bearing assembly in the temperature range of 1600-2200 K. The obtained post-spinel phase boundary can be expressed as P (GPa) = - 0.0004 T (K) + 22.26 using pressures calibrated by Au scale (Anderson et al., 1989). The choice of pressure scale does not have significant influence on the slope of phase transformation. Our experiments demonstrated that variations of

  8. Synchrotron-based Imaging and tomography with hard X-rays.

    SciTech Connect

    Rau, C.; Crecea, V.; Liu, W.; Richter, C. P.; Peterson, K. M.; Jemian, P. R.; Neuhausler, U.; Schneider, G.; Yu, X.; Braun, P. V.; Chiang, T. C.; Robinson, I. K.; X-Ray Science Division; Univ. of Illinois; Purdue Univ.; Northwestern Univ.; Univ. Bielefeld; Univ. Coll. London; Bessy GmbH; NIST

    2007-03-28

    Hard X-ray imaging with synchrotron radiation is a powerful tool to study opaque materials on the micro- and nano-lengthscales. Different imaging methods are available with an instrument recently built at Sector 34 of the Advanced Photon Source. In-line phase contrast imaging is performed with micrometer resolution. Increased spatial resolution is achieved using cone-beam geometry. The almost parallel beam is focused with a Kirkpatrick-Baez mirror system. The focal spot serves as a diverging secondary source. An X-ray magnified image of the sample is projected on the detector. For imaging and tomography with sub-100 nm resolution, an X-ray full-field microscope has been built. It uses a Kirkpatrick-Baez mirror (KB) as a condenser optic, followed by a micro-Fresnel zone plate (FZP) as an objective lens. The zone plates presently provide 50-85 nm spatial resolution when operating the microscope with photon energy between 6 and 12 keV. Tomography experiments have been performed with this new device.

  9. Absorption and Phase Contrast X-Ray Imaging in Paleontology Using Laboratory and Synchrotron Sources.

    PubMed

    Bidola, Pidassa; Stockmar, Marco; Achterhold, Klaus; Pfeiffer, Franz; Pacheco, Mírian L A F; Soriano, Carmen; Beckmann, Felix; Herzen, Julia

    2015-10-01

    X-ray micro-computed tomography (μCT) is commonly used for imaging of samples in biomedical or materials science research. Owing to the ability to visualize a sample in a nondestructive way, X-ray μCT is perfectly suited to inspect fossilized specimens, which are mostly unique or rare. In certain regions of the world where important sedimentation events occurred in the Precambrian geological time, several fossilized animals are studied to understand questions related to their origin, environment, and life evolution. This article demonstrates the advantages of applying absorption and phase-contrast CT on the enigmatic fossil Corumbella werneri, one of the oldest known animals capable of building hard parts, originally discovered in Corumbá (Brazil). Different tomographic setups were tested to visualize the fossilized inner structures: a commercial laboratory-based μCT device, two synchrotron-based imaging setups using conventional absorption and propagation-based phase contrast, and a commercial X-ray microscope with a lens-coupled detector system, dedicated for radiography and tomography. Based on our results we discuss the strengths and weaknesses of the different imaging setups for paleontological studies.

  10. Absorption and Phase Contrast X-Ray Imaging in Paleontology Using Laboratory and Synchrotron Sources

    SciTech Connect

    Bidola, Pidassa; Stockmar, Marco; Achterhold, Klaus; Pfeiffer, Franz; Pacheco, Mirian L.A.F.; Soriano, Carmen; Beckmann, Felix; Herzen, Julia

    2015-10-01

    X-ray micro-computed tomography (CT) is commonly used for imaging of samples in biomedical or materials science research. Owing to the ability to visualize a sample in a nondestructive way, X-ray CT is perfectly suited to inspect fossilized specimens, which are mostly unique or rare. In certain regions of the world where important sedimentation events occurred in the Precambrian geological time, several fossilized animals are studied to understand questions related to their origin, environment, and life evolution. This article demonstrates the advantages of applying absorption and phase-contrast CT on the enigmatic fossil Corumbella werneri, one of the oldest known animals capable of building hard parts, originally discovered in Corumba (Brazil). Different tomographic setups were tested to visualize the fossilized inner structures: a commercial laboratory-based CT device, two synchrotron-based imaging setups using conventional absorption and propagation-based phase contrast, and a commercial X-ray microscope with a lens-coupled detector system, dedicated for radiography and tomography. Based on our results we discuss the strengths and weaknesses of the different imaging setups for paleontological studies.

  11. XPAD3-S: A fast hybrid pixel readout chip for X-ray synchrotron facilities

    NASA Astrophysics Data System (ADS)

    Pangaud, Patrick; Basolo, Stephanie; Boudet, Nathalie; Berar, Jean-François; Chantepie, Benoît; Clemens, Jean-Claude; Delpierre, Pierre; Dinkespiler, Bernard; Medjoubi, Kadda; Hustache, Stephanie; Menouni, Mohsine; Morel, Christian

    2008-06-01

    At X-ray synchrotron facilities, scattering experiments require detectors with a large sensitive surface, an high count rate capability, a large counter dynamics, a fast readout system and an adjustable energy threshold. X-ray pixel chip with adaptable dynamics (XPAD3) is a new pixellized photon detector based on hybrid pixel technology, which provides low noise data readout at high speed. It is designed in 0.25 μm IBM technology and contains 9600 pixels (130 μm×130 μm) distributed into 80 columns of 120 elements each. Its features have been optimized to fulfill a count rate capability up to 10 +6 photons/pixel/s, an high dynamic range over 35 keV, a very low noise of 130e -, and a threshold adjustment well below 4 keV. Fast data readout below 2 ms/frame is expected. To meet these requirements, an innovative architecture has been designed that makes possible the readout the circuit during acquisition while preserving the precise setting of the thresholds all over the pixel array. The XPAD3 circuit can be bump-bonded with Si, CdTe, or GaAs sensors to optimize its detection efficiency at high X-ray energies. XPAD3 detector modules will be tiled together to form the XPIX detector with a 8 cm×12 cm sensitive area. We present first results obtained using a single-chip prototype of the XPAD3 detector.

  12. Absorption and Phase Contrast X-Ray Imaging in Paleontology Using Laboratory and Synchrotron Sources.

    PubMed

    Bidola, Pidassa; Stockmar, Marco; Achterhold, Klaus; Pfeiffer, Franz; Pacheco, Mírian L A F; Soriano, Carmen; Beckmann, Felix; Herzen, Julia

    2015-10-01

    X-ray micro-computed tomography (μCT) is commonly used for imaging of samples in biomedical or materials science research. Owing to the ability to visualize a sample in a nondestructive way, X-ray μCT is perfectly suited to inspect fossilized specimens, which are mostly unique or rare. In certain regions of the world where important sedimentation events occurred in the Precambrian geological time, several fossilized animals are studied to understand questions related to their origin, environment, and life evolution. This article demonstrates the advantages of applying absorption and phase-contrast CT on the enigmatic fossil Corumbella werneri, one of the oldest known animals capable of building hard parts, originally discovered in Corumbá (Brazil). Different tomographic setups were tested to visualize the fossilized inner structures: a commercial laboratory-based μCT device, two synchrotron-based imaging setups using conventional absorption and propagation-based phase contrast, and a commercial X-ray microscope with a lens-coupled detector system, dedicated for radiography and tomography. Based on our results we discuss the strengths and weaknesses of the different imaging setups for paleontological studies. PMID:26306692

  13. Spatially confined low-power optically pumped ultrafast synchrotron x-ray nanodiffraction

    SciTech Connect

    Park, Joonkyu; Zhang, Qingteng; Chen, Pice; Cosgriff, Margaret P.; Tilka, Jack A.; Evans, Paul G.; Adamo, Carolina; Schlom, Darrell G.; Wen, Haidan; Zhu, Yi

    2015-08-15

    The combination of ultrafast optical excitation and time-resolved synchrotron x-ray nanodiffraction provides unique insight into the photoinduced dynamics of materials, with the spatial resolution required to probe individual nanostructures or small volumes within heterogeneous materials. Optically excited x-ray nanobeam experiments are challenging because the high total optical power required for experimentally relevant optical fluences leads to mechanical instability due to heating. For a given fluence, tightly focusing the optical excitation reduces the average optical power by more than three orders of magnitude and thus ensures sufficient thermal stability for x-ray nanobeam studies. Delivering optical pulses via a scannable fiber-coupled optical objective provides a well-defined excitation geometry during rotation and translation of the sample and allows the selective excitation of isolated areas within the sample. Experimental studies of the photoinduced lattice dynamics of a 35 nm BiFeO{sub 3} thin film on a SrTiO{sub 3} substrate demonstrate the potential to excite and probe nanoscale volumes.

  14. Steady X-Ray Synchrotron Emission in the Northeastern Limb of SN 1006

    NASA Technical Reports Server (NTRS)

    Katsuda, Satoru; Petre, Robert; Mori, Koji; Reynolds, Stephen; Long, Knox; Winkler, P.; Tsunemi, Hiroshi

    2010-01-01

    We investigate time variations and detailed spatial structures of X-ray synchrotron emission in the northeastern limb of SN 1006, using two Chandra observations taken in 2000 and 2008. We extract spectra from a number of small ([approx]10'') regions. After taking account of proper motion and isolating the synchrotron from the thermal emission, we study time variations in the synchrotron emission in the small regions. We find that there are no regions showing strong flux variations. Our analysis shows an apparent flux decline in the overall synchrotron flux of [approx]4% at high energies, but we suspect that this is mostly a calibration effect, and that flux is actually constant to [approx]1%. This is much less than the variation found in other remnants where it was used to infer magnetic-field strengths up to 1 mG. We attribute the lack of variability to the smoothness of the synchrotron morphology, in contrast to the small-scale knots found to be variable in other remnants. The smoothness is to be expected for a Type Ia remnant encountering uniform material. Finally, we find a spatial correlation between the flux and the cutoff frequency in synchrotron emission. The simplest interpretation is that the cutoff frequency depends on the magnetic-field strength. This would require that the maximum energy of accelerated electrons is not limited by synchrotron losses, but by some other effect. Alternatively, the rate of particle injection and acceleration may vary due to some effect not yet accounted for, such as a dependence on shock obliquity.

  15. Synchrotron Vacuum Ultraviolet Light and Soft X-Ray Radiation Effects on Aluminized Teflon FEP Investigated

    NASA Technical Reports Server (NTRS)

    Dever, Joyce A.; Townsend, Jacqueline A.; Gaier, James R.; Jalics, Alice I.

    1999-01-01

    Since the Hubble Space Telescope (HST) was deployed in low Earth orbit in April 1990, two servicing missions have been conducted to upgrade its scientific capabilities. Minor cracking of second-surface metalized Teflon FEP (DuPont; fluorinated ethylene propylene) surfaces from multilayer insulation (MLI) was first observed upon close examination of samples with high solar exposure retrieved during the first servicing mission, which was conducted 3.6 years after deployment. During the second HST servicing mission, 6.8 years after deployment, astronaut observations and photographic documentation revealed significant cracks in the Teflon FEP layer of the MLI on both the solar- and anti-solar-facing surfaces of the telescope. NASA Goddard Space Flight Center directed the efforts of the Hubble Space Telescope MLI Failure Review Board, whose goals included identifying the low-Earth-orbit environmental constituent(s) responsible for the cracking and embrittling of Teflon FEP which was observed during the second servicing mission. The NASA Lewis Research Center provided significant support to this effort. Because soft x-ray radiation from solar flares had been considered as a possible cause for the degradation of the mechanical properties of Teflon FEP (ref. 1), the effects of soft xray radiation and vacuum ultraviolet light on Teflon FEP were investigated. In this Lewisled effort, samples of Teflon FEP with a 100-nm layer of vapor-deposited aluminum (VDA) on the backside were exposed to synchrotron radiation of various vacuum ultraviolet and soft x-ray wavelengths between 18 nm (69 eV) and 0.65 nm (1900 eV). Synchrotron radiation exposures were conducted using the National Synchrotron Light Source at Brookhaven National Laboratory. Samples of FEP/VDA were exposed with the FEP surface facing the synchrotron beam. Doses and fluences were compared with those estimated for the 20-yr Hubble Space Telescope mission.

  16. A study of the behavior of bromide in artificial pits using in situ X-ray microprobe analysis

    SciTech Connect

    Isaacs, H.S.; Kaneko, M.

    1997-12-31

    An in situ X-ray microprobe analysis of Type 316 stainless steel artificial pits has been carried out with a bromide/chloride solution. A high intensity 8 micron diameter polychromatic X-ray beam was scanned across the steel solution interface within the artificial pit. The resulting X-ray fluorescence was analyzed using an energy dispersive X-ray detector. In contrast to the light Cl atom, Br could be detected, making it possible to monitor the behavior of halides in the artificial pits and in the salt layer at the interface. It was found that Br was more active than Cl. At high potentials, elemental Br was produced as an oxidation product, whereas without added bromide, chloride only formed a salt layer. Br also concentrated at the salt steel interface at potentials below where it was oxidized.

  17. In situ X-ray measurements of MOVPE growth of InxGa1-xN single quantum wells

    NASA Astrophysics Data System (ADS)

    Ju, Guangxu; Fuchi, Shingo; Tabuchi, Masao; Takeda, Yoshikazu

    2013-05-01

    GaN/InxGa1-xN/GaN single quantum wells (SQWs) have been grown on c-plane GaN/sapphire substrates using MOVPE system. PL (photoluminescence) and AFM (atomic force microscope) measurements demonstrate good quality of after-growth thermal-annealed SQWs. In situ XRD (X-ray diffraction), XRR (X-ray reflectivity), and X-ray CTR (crystal truncation rod) scattering measurements were successfully conducted on the SQWs under the NH3+N2 ambient at 1103 K. The analysis results of the XRR and the X-ray CTR spectra at 1103 K and at 300 K on the same sample matched well. It demonstrated that In0.09Ga0.91N SQW structure with several ML (monolayer) InGaN thicknesses was successfully investigated using the XRR and CTR scattering measurements at 1103 K.

  18. Mapping Metal Elements of Shuangbai Dinosaur Fossil by Synchrotron X-ray Fluorescence Microprobe

    SciTech Connect

    Wang, Y.; Qun, Y; Ablett, J

    2008-01-01

    The metal elements mapping of Shuangbai dinosaur fossil, was obtained by synchrotron x-ray fluorescence (SXRF). Eight elements, Ca, Mn, Fe, Cu, Zn, As, Y and Sr were determined. Elements As and Y were detected for the first time in the dinosaur fossil. The data indicated that metal elements are asymmetrical on fossil section. This is different from common minerals. Mapping metals showed that metal element As is few. The dinosaur most likely belongs to natural death. This is different from Zigong dinosaurs which were found dead from poisoning. This method has been used to find that metals Fe and Mn are accrete, and the same is true for Sr and Y. This study indicated that colloid granule Fe and Mn, as well as Sr and Y had opposite electric charges in lithification process of fossils. By this analysis, compound forms can be ascertained. Synchrotron light source x-ray fluorescence is a complementary method that shows mapping of metal elements at the dinosaur fossil, and is rapid, exact and intuitionist. This study shows that dinosaur fossil mineral imaging has a potential in reconstructing the paleoenvironment and ancient geology.

  19. Synchrotron X-ray CT characterization of friction-welded joints in tial turbocharger components

    NASA Astrophysics Data System (ADS)

    Sun, J. G.; Kropf, A. J.; Vissers, D. R.; Sun, W. M.; Katsoudas, J.; Yang, N.; Fei, D.

    2012-05-01

    Titanium aluminide (TiAl) is an advanced intermetallic material and is being investigated for application in turbocharger components for diesel engines. A TiAl turbocharger rotor consists of a cast TiAl turbine wheel and a Ti-alloy shaft that are joined by friction welding. Although friction welding is an established industrial process, it is still challenging to join dissimilar materials especially for brittle intermetallics. These joints are therefore required to be inspected using a nondestructive evaluation (NDE) method. In this study, synchrotron X-ray computed tomography (CT) developed at the Advanced Photon Source at Argonne National Laboratory was used for NDE characterization of friction-welded joint in three TiAl turbocharger rotors. The filtered synchrotron X-ray source has high peak energies to penetrate thick metallic materials, and the detector (imager) has high spatial resolutions to resolve small flaws. The CT inspections revealed detailed 3D crack distributions within poorly welded joints. The crack detection sensitivity and resolution was calibrated and found to be correlated well with destructive examination.

  20. Solution Synchrotron X-ray Diffraction Reveals Structural Details of Lipid Domains in Ternary Mixtures

    SciTech Connect

    Yuan, J.; Kiss, A; Pramudya, Y; Nguyen, L; Hirst, L

    2009-01-01

    The influence of cholesterol on lipid bilayer structure is significant and the effect of cholesterol on lipid sorting and phase separation in lipid-raft-forming model membrane systems has been well investigated by microscopy methods on giant vesicles. An important consideration however is the influence of fluorescence illumination on the phase state of these lipids and this effect must be carefully minimized. In this paper, we show that synchrotron x-ray scattering on solution lipid mixtures is an effective alternative technique for the identification and characterization of the l o (liquid ordered) and l d (liquid disordered) phases. The high intensity of synchrotron x rays allows the observation of up to 5 orders of diffraction from the l o phase, whereas only two are clearly visible when the l d phase alone is present. This data can be collected in approximately 1 min/sample, allowing rapid generation of phase data. In this paper, we measure the lamellar spacing in both the liquid-ordered and liquid-disordered phases simultaneously, as a function of cholesterol concentration in two different ternary mixtures. We also observe evidence of a third gel-phaselike population at 10-12 mol % cholesterol and determine the thickness of the bilayer for this phase. Importantly we are able to look at phase coexistence in the membrane independent of photoeffects.

  1. Solution synchrotron x-ray diffraction reveals structural details of lipid domains in ternary mixtures

    NASA Astrophysics Data System (ADS)

    Yuan, Jing; Kiss, Alexander; Pramudya, Yohanes H.; Nguyen, Lam T.; Hirst, Linda S.

    2009-03-01

    The influence of cholesterol on lipid bilayer structure is significant and the effect of cholesterol on lipid sorting and phase separation in lipid-raft-forming model membrane systems has been well investigated by microscopy methods on giant vesicles. An important consideration however is the influence of fluorescence illumination on the phase state of these lipids and this effect must be carefully minimized. In this paper, we show that synchrotron x-ray scattering on solution lipid mixtures is an effective alternative technique for the identification and characterization of the lo (liquid ordered) and ld (liquid disordered) phases. The high intensity of synchrotron x rays allows the observation of up to 5 orders of diffraction from the lo phase, whereas only two are clearly visible when the ld phase alone is present. This data can be collected in ˜1min/sample , allowing rapid generation of phase data. In this paper, we measure the lamellar spacing in both the liquid-ordered and liquid-disordered phases simultaneously, as a function of cholesterol concentration in two different ternary mixtures. We also observe evidence of a third gel-phaselike population at 10-12mol% cholesterol and determine the thickness of the bilayer for this phase. Importantly we are able to look at phase coexistence in the membrane independent of photoeffects.

  2. Synchrotron X-ray and optical studies of the DNA-mediated growth of plasmonic nanostructures

    NASA Astrophysics Data System (ADS)

    Chen, Gang; Wang, Geng; Zhang, Xiaonan; Geng, Heping; Xu, Lifeng; Li, Wenqin; Liu, Xin

    2015-03-01

    Reproducible and controllable growth of nanostructures with well-defined physical and chemical properties is a longstanding problem in nanoscience. A key step to address this issue is to understand their underlying growth mechanism, which is often entangled in the complexity of growth environments and obscured by rapid reaction speeds. Synchrotron x-rays, because of their specific wavelengths (nanometers) and advantages of large flux, high penetration and adjustable photon energy, have a particularly important position in structural and electronic characterizations of nanomaterials. Herein, we demonstrate that the evolution of size, surface morphology, and the optical properties of plasmonic nanostructures could be quantitatively intercepted by dynamic and stoichiometric control of the DNA-mediated growth. By combining synchrotron-based small-angle X-ray scattering with transmission electron microscopy, we reliably obtained quantitative structural parameters for these fine nanostructures that correlate well with their optical properties as identified by UV/Vis absorption and dark-field scattering spectroscopy. We report growth mechanisms for SERS active plasmonic nanostructures, and the remarkable interplay between their morphology and plasmonic properties. Work supported by NNSF of China (11375256) and Sci. and Tech. Commission of Shanghai Municipality (14JC1493300).

  3. Synchrotron soft X-ray and field-emission electron sources: a comparison.

    PubMed

    Spence, J C H; Howells, M R

    2002-12-01

    The soft X-ray spectral region and the useful range of electron energy-loss spectroscopy are very similar, both including the energy range 100-1000 eV. Moreover, well-developed monochromators and parallel detection devices with comparable resolution exist for both. Despite the differing interactions of electrons and photons, many complementary experiments in imaging, spectroscopy and diffraction have been performed using both techniques. We therefore compare the brightness, degeneracy, monochromaticity, beam size, source size, spatial and temporal coherence of field-emission electron beams and soft X-ray synchrotron radiation from typical undulators. Recent brightness values for nanotip field emitters and undulators, both measured and calculated, are provided with examples from the Advanced Light Source synchrotron-radiation facility at Berkeley USA. The quantum mechanical upper limit on source brightness, as well as relationships among beam brightness, coherence parameters, and degeneracy, are discussed. Factors which limit these parameters and methods of measurement are reviewed, and the implications for diffraction, imaging and spectroscopic experiments as well as radiation damage are briefly commented on.

  4. Fast X-Ray Fluorescence Camera Combined with Wide Band Pass Monochromatic Synchrotron Beam

    NASA Astrophysics Data System (ADS)

    Sakurai, Kenji; Mizusawa, Mari

    2004-05-01

    A double W/B4C multilayer monochromator (2d=50.4Å) was commissioned for non-scanning X-ray fluorescence (XRF) imaging experiments. The combination of a brilliant multi-pole wiggler source and the present wide band pass monochromator permits 1.2 × 1013 photons/sec at the sample position for 8.04 keV X-rays. Energy resolution ΔE and ΔE/E are 300˜500 eV and ˜5%, respectively. The exit beam height is constant for X-ray energy ranging from 5.5 to 13.0 keV. Indirect cooling of the 1st multilayer works successfully. In addition, a new fast CCD camera was developed for quick readout and transfer of the image data. It was found that the typical exposure time for one XRF image with 1000 × 1000 pixels is 0.03˜1 sec. This permits in-situ movie recording for the distribution of elements.

  5. Real-time, high-resolution x-ray diffraction measurements on shocked crystals at a synchrotron facility.

    PubMed

    Gupta, Y M; Turneaure, Stefan J; Perkins, K; Zimmerman, K; Arganbright, N; Shen, G; Chow, P

    2012-12-01

    The Advanced Photon Source (APS) at Argonne National Laboratory was used to obtain real-time, high-resolution x-ray diffraction measurements to determine the microscopic response of shock-compressed single crystals. Disk shaped samples were subjected to plane shock wave compression by impacting them with half-inch diameter, flat-faced projectiles. The projectiles were accelerated to velocities ranging between 300 and 1200 m/s using a compact powder gun designed specifically for use at a synchrotron facility. The experiments were designed to keep the sample probed volume under uniaxial strain and constant stress for a duration longer than the 153.4 ns spacing between x-ray bunches. X-rays from a single pulse (<100 ps duration) out of the periodic x-ray pulses emitted by the synchrotron were used for the diffraction measurements. A synchronization and x-ray detection technique was developed to ensure that the measured signal was obtained unambiguously from the desired x-ray pulse incident on the sample while the sample was in a constant uniaxial strain state. The synchronization and x-ray detection techniques described can be used for a variety of x-ray measurements on shock compressed solids and liquids at the APS. Detailed procedures for applying the Bragg-Brentano parafocusing approach to single crystals at the APS are presented. Analytic developments to determine the effects of crystal substructure and non-ideal geometry on the diffraction pattern position and shape are presented. Representative real-time x-ray diffraction data, indicating shock-induced microstructural changes, are presented for a shock-compressed Al(111) sample. The experimental developments presented here provided, in part, the impetus for the Dynamic Compression Sector (DCS) currently under development at the APS. Both the synchronization∕x-ray detection methods and the analysis equations for high-resolution single crystal x-ray diffraction can be used at the DCS.

  6. Real-time, high-resolution x-ray diffraction measurements on shocked crystals at a synchrotron facility

    SciTech Connect

    Gupta, Y. M.; Turneaure, Stefan J.; Perkins, K.; Zimmerman, K.; Arganbright, N.; Shen, G.; Chow, P.

    2012-12-15

    The Advanced Photon Source (APS) at Argonne National Laboratory was used to obtain real-time, high-resolution x-ray diffraction measurements to determine the microscopic response of shock-compressed single crystals. Disk shaped samples were subjected to plane shock wave compression by impacting them with half-inch diameter, flat-faced projectiles. The projectiles were accelerated to velocities ranging between 300 and 1200 m/s using a compact powder gun designed specifically for use at a synchrotron facility. The experiments were designed to keep the sample probed volume under uniaxial strain and constant stress for a duration longer than the 153.4 ns spacing between x-ray bunches. X-rays from a single pulse (<100 ps duration) out of the periodic x-ray pulses emitted by the synchrotron were used for the diffraction measurements. A synchronization and x-ray detection technique was developed to ensure that the measured signal was obtained unambiguously from the desired x-ray pulse incident on the sample while the sample was in a constant uniaxial strain state. The synchronization and x-ray detection techniques described can be used for a variety of x-ray measurements on shock compressed solids and liquids at the APS. Detailed procedures for applying the Bragg-Brentano parafocusing approach to single crystals at the APS are presented. Analytic developments to determine the effects of crystal substructure and non-ideal geometry on the diffraction pattern position and shape are presented. Representative real-time x-ray diffraction data, indicating shock-induced microstructural changes, are presented for a shock-compressed Al(111) sample. The experimental developments presented here provided, in part, the impetus for the Dynamic Compression Sector (DCS) currently under development at the APS. Both the synchronization/x-ray detection methods and the analysis equations for high-resolution single crystal x-ray diffraction can be used at the DCS.

  7. Characterization of phase transitions during freeze-drying by in situ X-ray powder diffractometry.

    PubMed

    Cavatur, R K; Suryanarayanan, R

    1998-11-01

    The purpose of this research was to develop the technique of in situ freeze-drying in the sample chamber of an X-ray powder diffractometer (XRD) and to monitor the phase transitions during the freeze-drying of aqueous solutions of sodium nafcillin (I) and mannitol (II). Aqueous solutions of I and II were frozen under controlled conditions in the sample chamber of an XRD. This variable temperature XRD was modified so that the sample chamber could be evacuated and the samples dried under reduced pressures. Thus the entire freeze-drying cycle was carried out in the XRD holder and the solid-state was monitored during the various stages of the process. Frozen solutions of I when annealed at -4 degrees C, resulted in crystallization of the solute as 'sodium nafcillin hydrate' (unknown stoichiometry). Primary drying at -10 degrees C, resulted in partial dehydration to a poorly crystalline sodium nafcillin hemihydrate. There was no crystallization of mannitol when solutions of II were cooled and subjected to primary drying at -50 degrees C. During the drying, the intensities of the characteristic X-ray lines of ice (d-spacings of 3.94, 3.70 and 3.48 A) were quantified. This enabled real time monitoring of the complete sublimation of crystalline ice. When the secondary drying was carried out at -25 degrees C, mannitol crystallized as an anhydrous mixture of the delta- and beta-polymorphs. In a second set of experiments, the frozen solutions were warmed to -25 degrees C and subjected to primary drying. Mannitol crystallized and its XRD pattern matched that of mannitol hydrate reported recently (Yu et al., Pharm. Res., 14S (1997) S-445). When the secondary drying was carried out at -10 degrees C, there was no change in the XRD pattern suggesting the formation of a dehydrated hydrate. This in situ XRD technique enabled us to characterize the phase transitions during freeze-drying. It would be useful in developing a mechanistic understanding of the alterations in the solid

  8. Non-destructive in situ study of "Mad Meg" by Pieter Bruegel the Elder using mobile X-ray fluorescence, X-ray diffraction and Raman spectrometers

    NASA Astrophysics Data System (ADS)

    Van de Voorde, Lien; Van Pevenage, Jolien; De Langhe, Kaat; De Wolf, Robin; Vekemans, Bart; Vincze, Laszlo; Vandenabeele, Peter; Martens, Maximiliaan P. J.

    2014-07-01

    "Mad Meg", a figure of Flemish folklore, is the subject of a famous oil-on-panel painting by the Flemish renaissance artist Pieter Bruegel the Elder, exhibited in the Museum Mayer van den Bergh (Antwerp, Belgium). This article reports on the in situ chemical characterization of this masterpiece by using currently available state-of-the-art portable analytical instruments. The applied non-destructive analytical approach involved the use of a) handheld X-ray fluorescence instrumentation for retrieving elemental information and b) portable X-ray fluorescence/X-ray diffraction instrumentation and laser-based Raman spectrometers for obtaining structural/molecular information. Next to material characterization of the used pigments and of the different preparation layers of the painting, also the verification of two important historical iconographic hypotheses is performed concerning the economic way of painting by Brueghel, and whether or not he used blue smalt pigment for painting the boat that appears towards the top of the painting. The pigments identified are smalt pigment (65% SiO2 + 15% K2O + 10% CoO + 5% Al2O3) for the blue color present in all blue areas of the painting, probably copper resinate for the green colors, vermillion (HgS) as red pigment and lead white is used to form different colors. The comparison of blue pigments used on different areas of the painting gives no differences in the elemental fingerprint which confirms the existing hypothesis concerning the economic painting method by Bruegel.

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

    PubMed

    Maddox, B R; Akin, M C; Teruya, A; Hunt, D; Hahn, D; Cradick, J; Morgan, D V

    2016-08-01

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

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

    PubMed

    Maddox, B R; Akin, M C; Teruya, A; Hunt, D; Hahn, D; Cradick, J; Morgan, D V

    2016-08-01

    Diagnostic use of single-pulse x-ray diffraction (XRD) at pulsed power facilities can be challenging due to factors such as the high flux and brightness requirements for diffraction and the geometric constraints of experimental platforms. By necessity, the x-ray source is usually positioned very close, within a few inches of the sample. On dynamic compression platforms, this puts the x-ray source in the debris field. We coupled x-ray polycapillary optics to a single-shot needle-and-washer x-ray diode source using a laser-based alignment scheme to obtain high-quality x-ray diffraction using a single 16 ns x-ray pulse with the source >1 m from the sample. The system was tested on a Mo sample in reflection geometry using 17 keV x-rays from a Mo anode. We also identified an anode conditioning effect that increased the x-ray intensity by 180%. Quantitative measurements of the x-ray focal spot produced by the polycapillary yielded a total x-ray flux on the sample of 3.3 ± 0.5 × 10(7) molybdenum Kα photons. PMID:27587130

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

    NASA Astrophysics Data System (ADS)

    Maddox, B. R.; Akin, M. C.; Teruya, A.; Hunt, D.; Hahn, D.; Cradick, J.; Morgan, D. V.

    2016-08-01

    Diagnostic use of single-pulse x-ray diffraction (XRD) at pulsed power facilities can be challenging due to factors such as the high flux and brightness requirements for diffraction and the geometric constraints of experimental platforms. By necessity, the x-ray source is usually positioned very close, within a few inches of the sample. On dynamic compression platforms, this puts the x-ray source in the debris field. We coupled x-ray polycapillary optics to a single-shot needle-and-washer x-ray diode source using a laser-based alignment scheme to obtain high-quality x-ray diffraction using a single 16 ns x-ray pulse with the source >1 m from the sample. The system was tested on a Mo sample in reflection geometry using 17 keV x-rays from a Mo anode. We also identified an anode conditioning effect that increased the x-ray intensity by 180%. Quantitative measurements of the x-ray focal spot produced by the polycapillary yielded a total x-ray flux on the sample of 3.3 ± 0.5 × 107 molybdenum Kα photons.

  12. In Situ X-ray Diffraction Studies of Cathode Materials in Lithium Batteries

    SciTech Connect

    Yang, X. Q.; Sun, X.; McBreen, J.; Mukerjee, S.; Gao, Yuan; Yakovleva, M. V.; Xing, X. K.; Daroux, M. L.

    1998-11-01

    system definitely requires an in situ XRD technique to study the detail structural changes of the system during charge and discharge. The in situ XRD technique was used by Reimers, Li,and Dahn to study the LiCoO{sub 2}, LiNiO{sub 2}, and LiMn{sub 2}O{sub 4} systems. Their results of these studies have demonstrated that in situ XRD can provide more detailed information about the cathode material structural changes during charge-discharge. Conventional x-ray sources were used in these studies and the beryllium windows were used in the in situ cells. Provisions were made to prevent corrosion of the beryllium windows during charge-discharge. For this reason, the in situ cells were often designed quite differently than a real battery. More seriously, the problem of beryllium corrosion restricted the voltage range of the cell below 4.5 V. This limited the use of this technique to study the effects of overcharge which is very important to the thermal stability of the cathodes. Using the plastic lithium battery technology, Amatucci, Tarascon, and Klein constructed an in situ XRD cell, which allows structural investigations at voltages greater than 5 V without any beryllium window corrosion. However, all of these in situ XRD studies using conventional x-ray sources probe the cell in reflection geometry. Therefore, the observed structural changes are predominantly from the top few microns of the electrode coating, which might not be representative for the whole coating during charge-discharge especially when the rate is high.

  13. Understanding Plasticity and Fracture in Aluminum Alloys and their Composites by 3D X-ray Synchrotron Tomography and Microdiffraction

    NASA Astrophysics Data System (ADS)

    Hruby, Peter

    Aluminum alloys and their composites are attractive materials for applications requiring high strength-to-weight ratios and reasonable cost. Many of these applications, such as those in the aerospace industry, undergo fatigue loading. An understanding of the microstructural damage that occurs in these materials is critical in assessing their fatigue resistance. Two distinct experimental studies were performed to further the understanding of fatigue damage mechanisms in aluminum alloys and their composites, specifically fracture and plasticity. Fatigue resistance of metal matrix composites (MMCs) depends on many aspects of composite microstructure. Fatigue crack growth behavior is particularly dependent on the reinforcement characteristics and matrix microstructure. The goal of this work was to obtain a fundamental understanding of fatigue crack growth behavior in SiC particle-reinforced 2080 Al alloy composites. In situ X-ray synchrotron tomography was performed on two samples at low (R=0.1) and at high (R=0.6) R-ratios. The resulting reconstructed images were used to obtain three-dimensional (3D) rendering of the particles and fatigue crack. Behaviors of the particles and crack, as well as their interaction, were analyzed and quantified. Four-dimensional (4D) visual representations were constructed to aid in the overall understanding of damage evolution. During fatigue crack growth in ductile materials, a plastic zone is created in the region surrounding the crack tip. Knowledge of the plastic zone is important for the understanding of fatigue crack formation as well as subsequent growth behavior. The goal of this work was to quantify the 3D size and shape of the plastic zone in 7075 Al alloys. X-ray synchrotron tomography and Laue microdiffraction were used to non-destructively characterize the volume surrounding a fatigue crack tip. The precise 3D crack profile was segmented from the reconstructed tomography data. Depth-resolved Laue patterns were obtained using

  14. Polarized synchrotron emission in quiescent black hole X-ray transients

    NASA Astrophysics Data System (ADS)

    Russell, David M.; Shahbaz, Tariq; Lewis, Fraser; Gallo, Elena

    2016-08-01

    We present near-infrared polarimetric observations of the black hole X-ray binaries Swift J1357.2-0933 and A0620-00. In both sources, recent studies have demonstrated the presence of variable infrared synchrotron emission in quiescence, most likely from weak compact jets. For Swift J1357.2-0933 we find that the synchrotron emission is polarized at a level of 8.0 ± 2.5 per cent (a 3.2 σ detection of intrinsic polarization). The mean magnitude and rms variability of the flux (fractional rms of 19-24 per cent in KS-band) agree with previous observations. These properties imply a continuously launched (stable on long timescales), highly variable (on short timescales) jet in the Swift J1357.2-0933 system in quiescence, which has a moderately tangled magnetic field close to the base of the jet. We find that for A0620-00, there are likely to be three components to the optical-infrared polarization; interstellar dust along the line of sight, scattering within the system, and an additional source that changes the polarization position angle in the reddest (H and KS) wave-bands. We interpret this as a stronger contribution of synchrotron emission, and by subtracting the line-of-sight polarization, we measure an excess of ˜1.25 ± 0.28 per cent polarization and a position angle of the magnetic field vector that is consistent with being parallel with the axis of the resolved radio jet. These results imply that weak jets in low luminosity accreting systems have magnetic fields which possess similarly tangled fields compared to the more luminous, hard state jets in X-ray binaries.

  15. Relativistic klystron driven compact high gradient accelerator as an injector to an X-ray synchrotron radiation ring

    DOEpatents

    Yu, David U. L.

    1990-01-01

    A compact high gradient accelerator driven by a relativistic klystron is utilized to inject high energy electrons into an X-ray synchrotron radiation ring. The high gradients provided by the relativistic klystron enables accelerator structure to be much shorter (typically 3 meters) than conventional injectors. This in turn enables manufacturers which utilize high energy, high intensity X-rays to produce various devices, such as computer chips, to do so on a cost effective basis.

  16. In situ alkali-silica reaction observed by x-ray microscopy

    SciTech Connect

    Kurtis, K.E.; Monteiro, P.J.M.; Brown, J.T.; Meyer-Ilse, W.

    1997-04-01

    In concrete, alkali metal ions and hydroxyl ions contributed by the cement and reactive silicates present in aggregate can participate in a destructive alkali-silica reaction (ASR). This reaction of the alkalis with the silicates produces a gel that tends to imbibe water found in the concrete pores, leading to swelling of the gel and eventual cracking of the affected concrete member. Over 104 cases of alkali-aggregate reaction in dams and spillways have been reported around the world. At present, no method exists to arrest the expansive chemical reaction which generates significant distress in the affected structures. Most existing techniques available for the examination of concrete microstructure, including ASR products, demand that samples be dried and exposed to high pressure during the observation period. These sample preparation requirements present a major disadvantage for the study of alkali-silica reaction. Given the nature of the reaction and the affect of water on its products, it is likely that the removal of water will affect the morphology, creating artifacts in the sample. The purpose of this research is to observe and characterize the alkali-silica reaction, including each of the specific reactions identified previously, in situ without introducing sample artifacts. For observation of unconditioned samples, x-ray microscopy offers an opportunity for such an examination of the alkali-silica reaction. Currently, this investigation is focusing on the effect of calcium ions on the alkali-silica reaction.

  17. Versatile in situ powder X-ray diffraction cells for solid–gas investigations

    PubMed Central

    Jensen, Torben R.; Nielsen, Thomas K.; Filinchuk, Yaroslav; Jørgensen, Jens-Erik; Cerenius, Yngve; Gray, Evan MacA.; Webb, Colin J.

    2010-01-01

    This paper describes new sample cells and techniques for in situ powder X-ray diffraction specifically designed for gas absorption studies up to ca 300 bar (1 bar = 100 000 Pa) gas pressure. The cells are for multipurpose use, in particular the study of solid–gas reactions in dosing or flow mode, but can also handle samples involved in solid–liquid–gas studies. The sample can be loaded into a single-crystal sapphire (Al2O3) capillary, or a quartz (SiO2) capillary closed at one end. The advantages of a sapphire single-crystal cell with regard to rapid pressure cycling are discussed, and burst pressures are calculated and measured to be ∼300 bar. An alternative and simpler cell based on a thin-walled silicate or quartz glass capillary, connected to a gas source via a VCR fitting, enables studies up to ∼100 bar. Advantages of the two cell types are compared and their applications are illustrated by case studies. PMID:22477780

  18. Boron phosphide under pressure: In situ study by Raman scattering and X-ray diffraction

    NASA Astrophysics Data System (ADS)

    Solozhenko, Vladimir L.; Kurakevych, Oleksandr O.; Le Godec, Yann; Kurnosov, Aleksandr V.; Oganov, Artem R.

    2014-07-01

    Cubic boron phosphide, BP, has been studied in situ by X-ray diffraction and Raman scattering up to 55 GPa at 300 K in a diamond anvil cell. The bulk modulus of B0 = 174(2) GPa has been established, which is in excellent agreement with our ab initio calculations. The data on Raman shift as a function of pressure, combined with equation-of-state (EOS) data, allowed us to estimate the Grüneisen parameters of the TO and LO modes of zinc-blende structure, γGTO= 1.26 and γGLO= 1.13, just like in the case of other AIIIBV diamond-like phases, for which γGTO> γGLO≅ 1. We also established that the pressure dependence of the effective electro-optical constant α is responsible for a strong change in relative intensities of the TO and LO modes from ITO/ILO ˜ 0.25 at 0.1 MPa to ITO/ILO ˜ 2.5 at 45 GPa, for which we also find excellent agreement between experiment and theory.

  19. Boron phosphide under pressure: In situ study by Raman scattering and X-ray diffraction

    SciTech Connect

    Solozhenko, Vladimir L.; Kurakevych, Oleksandr O.; Le Godec, Yann; Kurnosov, Aleksandr V.; Oganov, Artem R.

    2014-07-21

    Cubic boron phosphide, BP, has been studied in situ by X-ray diffraction and Raman scattering up to 55 GPa at 300 K in a diamond anvil cell. The bulk modulus of B{sub 0} = 174(2) GPa has been established, which is in excellent agreement with our ab initio calculations. The data on Raman shift as a function of pressure, combined with equation-of-state (EOS) data, allowed us to estimate the Grüneisen parameters of the TO and LO modes of zinc-blende structure, γ{sub G}{sup TO }= 1.26 and γ{sub G}{sup LO }= 1.13, just like in the case of other A{sup III}B{sup V} diamond-like phases, for which γ{sub G}{sup TO }> γ{sub G}{sup LO }≅ 1. We also established that the pressure dependence of the effective electro-optical constant α is responsible for a strong change in relative intensities of the TO and LO modes from I{sub TO}/I{sub LO} ∼ 0.25 at 0.1 MPa to I{sub TO}/I{sub LO} ∼ 2.5 at 45 GPa, for which we also find excellent agreement between experiment and theory.

  20. Scanning of Adsorption Hysteresis In Situ with Small Angle X-Ray Scattering

    PubMed Central

    Mitropoulos, Athanasios Ch.; Favvas, Evangelos P.; Stefanopoulos, Konstantinos L.; Vansant, Etienne F.

    2016-01-01

    Everett’s theorem-6 of the domain theory was examined by conducting adsorption in situ with small angle x-ray scattering (SAXS) supplemented by the contrast matching technique. The study focuses on the spectrum differences of a point to which the system arrives from different scanning paths. It is noted that according to this theorem at a common point the system has similar macroscopic properties. Furthermore it was examined the memory string of the system. We concluded that opposite to theorem-6: a) at a common point the system can reach in a finite (not an infinite) number of ways, b) a correction for the thickness of the adsorbed film prior to capillary condensation is necessary, and c) the scattering curves although at high-Q values coincide, at low-Q values are different indicating different microscopic states. That is, at a common point the system holds different metastable states sustained by hysteresis effects. These metastable states are the ones which highlight the way of a system back to a return point memory (RPM). Entering the hysteresis loop from different RPMs different histories are implanted to the paths toward the common point. Although in general the memory points refer to relaxation phenomena, they also constitute a characteristic feature of capillary condensation. Analogies of the no-passing rule and the adiabaticity assumption in the frame of adsorption hysteresis are discussed. PMID:27741263

  1. Shock Melting of Forsterite by In-Situ X-Ray Diffraction

    NASA Astrophysics Data System (ADS)

    Newman, M.; Kraus, R. G.; Wicks, J. K.; Coppari, F.; Smith, R.; Duffy, T. S.

    2015-12-01

    The equation of state of magnesium silicates at pressures and temperatures near the solid-liquid coexistence curve is important for understanding the thermal evolution and interior structure of rocky planets. Here, we present a series of laser driven shock-melt experiments on single crystal Mg_2SiO_4 forsterite, conducted at the Omega EP laser facility. Particle velocities in the Mg_2SiO_4 samples were measured using a line VISAR and used to infer the thermodynamic state of the shocked samples. In situ X-ray diffraction measurements are used to probe the melting transition and investigate the potential decomposition of Mg_2SiO_4 in to MgO and MgSiO_3 upon melt. This work examines potential kinetic effects of decomposition due to the short time scale of laser-shock experiments. In addition, the thermodynamic data collected in these experiments adds to a limited body of information regarding the equation of state of Mg_2SiO_4, which is the dominant end member composition in Earth's upper mantle. This work was performed under the auspices of the U.S. Department of Energy by Lawrence Livermore National Laboratory under Contract DE-AC52-07NA27344.

  2. Implementation of ultrafast X-ray diffraction at the 1W2B wiggler beamline of Beijing Synchrotron Radiation Facility.

    PubMed

    Sun, Da Rui; Xu, Guang Lei; Zhang, Bing Bing; Du, Xue Yan; Wang, Hao; Li, Qiu Ju; Zhou, Yang Fan; Li, Zhen Jie; Zhang, Yan; He, Jun; Yue, Jun Hui; Lei, Ge; Tao, Ye

    2016-05-01

    The implementation of a laser pump/X-ray probe scheme for performing picosecond-resolution X-ray diffraction at the 1W2B wiggler beamline at Beijing Synchrotron Radiation Facility is reported. With the hybrid fill pattern in top-up mode, a pixel array X-ray detector was optimized to gate out the signal from the singlet bunch with interval 85 ns from the bunch train. The singlet pulse intensity is ∼2.5 × 10(6) photons pulse(-1) at 10 keV. The laser pulse is synchronized to this singlet bunch at a 1 kHz repetition rate. A polycapillary X-ray lens was used for secondary focusing to obtain a 72 µm (FWHM) X-ray spot. Transient photo-induced strain in BiFeO3 film was observed at a ∼150 ps time resolution for demonstration.

  3. Soft x-ray emission spectroscopy using monochromatized synchrotron radiation (invited)

    NASA Astrophysics Data System (ADS)

    Nordgren, J.; Bray, G.; Cramm, S.; Nyholm, R.; Rubensson, J.-E.; Wassdahl, N.

    1989-07-01

    Soft x-ray emission spectroscopy is a common tool for the study of the electronic structure of molecules and solids. However, the interpretation of spectra is sometimes made difficult by overlaying lines due to satellite transitions or close-lying core holes. Also, irrelevant inner core transitions may accidentally fall in the wavelength region under study. These problems, which often arise for spectra excited with electrons or broadband photon sources can be removed by using monochromatized synchrotron radiation. In addition, one achieves other advantages as well, such as the ability to study resonant behavior. Another important aspect is the softness of this excitation agent, which allows chemically fragile compounds to be investigated. In this work we demonstrate the feasibility of using monochromatized synchrotron radiation to excite soft x-ray spectra. We also show new results which have been accomplished as a result of the selectivity of the excitation. The work has been carried out using the Flipper I wiggler beamline at HASYLAB in Hamburg using a new grazing incidence instrument designed specifically for this experiment. The photon flux at the Flipper I station (typically 5×1012 photons per second on the sample with a 1% bandpass) is enough to allow soft x-ray fluorescence spectra to be recorded at relatively high resolution and within reasonable accumulation times (typically, the spectra presented in this work were recorded in 30 min). The spectrometer is based on a new concept which allows the instrument to be quite small, still covering a large wavelength range (10-250 Å). The basic idea involves the use of several fixed mounted gratings and a large two-dimensional detector. The grating arrangement provides simple mounting within a limited space and, in particular, large spectral range. The detector can be moved in a three-axis coordinate system in order to cover the different Rowland curves defined by the different gratings. The arrangement permits

  4. Structural evolution of regenerated silk fibroin under shear: Combined wide- and small-angle x-ray scattering experiments using synchrotron radiation

    SciTech Connect

    Rossle, Manfred; Panine, Pierre; Urban, Volker S; Riekel, Christine

    2004-04-01

    The structural evolution of regenerated Bombyx mori silk fibroin during shearing with a Couette cell has been studied in situ by synchrotron radiation small- and wide-angle x-ray scattering techniques. An elongation of fibroin molecules was observed with increasing shear rate, followed by an aggregation phase. The aggregates were found to be amorphous with {beta}-conformation according to infrared spectroscopy. Scanning x-ray microdiffraction with a 5 {micro}m beam on aggregated material, which had solidified in air, showed silk II reflections and a material with equatorial reflections close to the silk I structure reflections, but with strong differences in reflection intensities. This silk I type material shows up to two low-angle peaks suggesting the presence of water molecules that might be intercalated between hydrogen-bonded sheets.

  5. First Observation of a Wooden Foreign Body in Soft Palate by Means of Synchrotron X-Ray Refraction Contrast

    NASA Astrophysics Data System (ADS)

    Mori, Koichi; Sekine, Norio; Sato, Hitoshi; Shikano, Naoto; Shimao, Daisuke; Shiwaku, Hideaki; Hyodo, Kazuyuki; Ohashi, Kenjirou

    2002-08-01

    A clear image of a wooden chopstick penetrating the soft palate of a pig-head was obtained using highly coherent synchrotron X-ray. The image was recorded on a mammography film with an intensifying screen at an X-ray energy of 35 keV. The tubular tissues as sieve tubes or ducts in the chopsticks appeared as white-black line images by means of X-ray refraction contrast. This method may enable development of an accurate diagnostic method in the field of penetrating trauma by wood.

  6. Synchrotron X-ray microfluorescence measurement of metal distributions in Phragmites australis root system in the Yangtze River intertidal zone.

    PubMed

    Feng, Huan; Zhang, Weiguo; Qian, Yu; Liu, Wenliang; Yu, Lizhong; Yoo, Shinjae; Wang, Jun; Wang, Jia Jun; Eng, Christopher; Liu, Chang Jun; Tappero, Ryan

    2016-07-01

    This study investigates the distributions of Br, Ca, Cl, Cr, Cu, K, Fe, Mn, Pb, Ti, V and Zn in Phragmites australis root system and the function of Fe nanoparticles in scavenging metals in the root epidermis using synchrotron X-ray microfluorescence, synchrotron transmission X-ray microscope measurement and synchrotron X-ray absorption near-edge structure techniques. The purpose of this study is to understand the mobility of metals in wetland plant root systems after their uptake from rhizosphere soils. Phragmites australis samples were collected in the Yangtze River intertidal zone in July 2013. The results indicate that Fe nanoparticles are present in the root epidermis and that other metals correlate significantly with Fe, suggesting that Fe nanoparticles play an important role in metal scavenging in the epidermis.

  7. Synchrotron X-ray microfluorescence measurement of metal distributions in Phragmites australis root system in the Yangtze River intertidal zone

    DOE PAGES

    Feng, Huan; Zhang, Weiguo; Qian, Yu; Liu, Wenliang; Yu, Lizhong; Yoo, Shinjae; Wang, Jun; Wang, Jia -Jun; Eng, Christopher; Liu, Chang -Jun; et al

    2016-06-15

    This paper investigates the distributions of Br, Ca, Cl, Cr, Cu, K, Fe, Mn, Pb, Ti, V and Zn in Phragmites australis root system and the function of Fe nanoparticles in scavenging metals in the root epidermis using synchrotron X-ray microfluorescence, synchrotron transmission X-ray microscope measurement and synchrotron X-ray absorption near-edge structure techniques. The purpose of this study is to understand the mobility of metals in wetland plant root systems after their uptake from rhizosphere soils. Phragmites australis samples were collected in the Yangtze River intertidal zone in July 2013. The results indicate that Fe nanoparticles are present in themore » root epidermis and that other metals correlate significantly with Fe, suggesting that Fe nanoparticles play an important role in metal scavenging in the epidermis.« less

  8. Extracting material parameters from x-ray attenuation: a CT feasibility study using kilovoltage synchrotron x-rays incident upon low atomic number absorbers.

    PubMed

    Kirby, B J; Davis, J R; Grant, J A; Morgan, M J

    2003-10-21

    The work reported here is a feasibility study of the extraction of material parameters from measurements of the linear x-ray attenuation coefficient of low atomic number absorbers. Computed tomography (CT) scans of small samples containing several liquids and solids were carried out with synchrotron radiation at the Australian National Beamline Facility (BL 20B) in Japan. Average values of the x-ray linear attenuation coefficient were extracted for each material for x-ray energies ranging from 11 keV to 20.5 keV. The electron density was estimated by applying results derived from a parametrization of the x-ray linear attenuation coefficient first developed by Jackson and Hawkes and extended for this work. Average estimates for the electron density of triethanolamine and acetic acid were made to within +5.3% of the actual value. Other materials examined included furfuraldehyde, perspex and teflon, for which average estimates of the electron density were less than 10% in excess of the calculated value. PMID:14620065

  9. 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

    2014-01-01

    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.

  10. 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

    2014-01-01

    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. PMID:24786694

  11. Distinct charge dynamics in battery electrodes revealed by in situ and operando soft X-ray spectroscopy

    PubMed Central

    Liu, Xiaosong; Wang, Dongdong; Liu, Gao; Srinivasan, Venkat; Liu, Zhi; Hussain, Zahid; Yang, Wanli

    2013-01-01

    Developing high-performance batteries relies on material breakthroughs. During the past few years, various in situ characterization tools have been developed and have become indispensible in studying and the eventual optimization of battery materials. However, soft X-ray spectroscopy, one of the most sensitive probes of electronic states, has been mainly limited to ex situ experiments for battery research. Here we achieve in situ and operando soft X-ray absorption spectroscopy of lithium-ion battery cathodes. Taking advantage of the elemental, chemical and surface sensitivities of soft X-rays, we discover distinct lithium-ion and electron dynamics in Li(Co1/3Ni1/3Mn1/3)O2 and LiFePO4 cathodes in polymer electrolytes. The contrast between the two systems and the relaxation effect in LiFePO4 is attributed to a phase transformation mechanism, and the mesoscale morphology and charge conductivity of the electrodes. These discoveries demonstrate feasibility and power of in situ soft X-ray spectroscopy for studying integrated and dynamic effects in batteries. PMID:24100759

  12. Absolute x-ray dosimetry on a synchrotron medical beam line with a graphite calorimeter

    SciTech Connect

    Harty, P. D. Ramanathan, G.; Butler, D. J.; Johnston, P. N.; Lye, J. E.; Hall, C. J.; Stevenson, A. W.

    2014-05-15

    Purpose: The absolute dose rate of the Imaging and Medical Beamline (IMBL) on the Australian Synchrotron was measured with a graphite calorimeter. The calorimetry results were compared to measurements from the existing free-air chamber, to provide a robust determination of the absolute dose in the synchrotron beam and provide confidence in the first implementation of a graphite calorimeter on a synchrotron medical beam line. Methods: The graphite calorimeter has a core which rises in temperature when irradiated by the beam. A collimated x-ray beam from the synchrotron with well-defined edges was used to partially irradiate the core. Two filtration sets were used, one corresponding to an average beam energy of about 80 keV, with dose rate about 50 Gy/s, and the second filtration set corresponding to average beam energy of 90 keV, with dose rate about 20 Gy/s. The temperature rise from this beam was measured by a calibrated thermistor embedded in the core which was then converted to absorbed dose to graphite by multiplying the rise in temperature by the specific heat capacity for graphite and the ratio of cross-sectional areas of the core and beam. Conversion of the measured absorbed dose to graphite to absorbed dose to water was achieved using Monte Carlo calculations with the EGSnrc code. The air kerma measurements from the free-air chamber were converted to absorbed dose to water using the AAPM TG-61 protocol. Results: Absolute measurements of the IMBL dose rate were made using the graphite calorimeter and compared to measurements with the free-air chamber. The measurements were at three different depths in graphite and two different filtrations. The calorimetry measurements at depths in graphite show agreement within 1% with free-air chamber measurements, when converted to absorbed dose to water. The calorimetry at the surface and free-air chamber results show agreement of order 3% when converted to absorbed dose to water. The combined standard uncertainty is 3

  13. Design and Operation of an In Situ High Pressure Reaction Cell for X-Ray Absorption Spectroscopy

    SciTech Connect

    Bare, Simon R.; Mickelson, G. E.; Modica, F. S.; Yang, N.; Kelly, S. D.

    2007-02-02

    The design and initial operation of an in situ catalysis reaction cell for x-ray absorption spectroscopy measurements at high pressure is described. The design is based on an x-ray transparent tube fabricated from beryllium. This forms a true plug flow reactor for catalysis studies. The reactor is coupled to a portable microprocessor-controlled versatile feed system, and incorporates on-line analysis of reaction products. XAFS data recorded during the reduction of a NiRe/carbon catalyst at 4 bar are used to illustrate the performance of the reactor.

  14. Design and operation of an in situ high pressure reaction cell for x-ray absorption spectroscopy.

    SciTech Connect

    Bare, S. R.; Yang, N.; Kelly, S. D.; Mickelson, G. E.; Modica, F. S.; UOP LLC; EXAFS Analysis

    2007-01-01

    The design and initial operation of an in situ catalysis reaction cell for x-ray absorption spectroscopy measurements at high pressure is described. The design is based on an x-ray transparent tube fabricated from beryllium. This forms a true plug flow reactor for catalysis studies. The reactor is coupled to a portable microprocessor-controlled versatile feed system, and incorporates on-line analysis of reaction products. XAFS data recorded during the reduction of a NiRe/carbon catalyst at 4 bar are used to illustrate the performance of the reactor.

  15. Accounting for low-frequency synchrotron X-ray beam position fluctuations for dynamic visualizations.

    PubMed

    Hinebaugh, J; Challa, P R; Bazylak, A

    2012-11-01

    Synchrotron X-ray radiography on beamline 05B1-1 at the Canadian Light Source Inc. was employed to study dynamic liquid water transport in the porous electrode materials of polymer electrolyte membrane fuel cells. Dynamic liquid water distributions were quantified for each radiograph in a sequence, and non-physical liquid water measurements were obtained. It was determined that the position of the beam oscillated vertically with an amplitude of ~25 µm at the sample and a frequency of ~50 mHz. In addition, the mean beam position moved linearly in the vertical direction at a rate of 0.74 µm s(-1). No evidence of horizontal oscillations was detected. In this work a technique is presented to account for the temporal and spatial dependence of synchrotron beam intensity, which resulted in a significant reduction in false water thickness. This work provides valuable insight into the treatment of radiographic time-series for capturing dynamic processes from synchrotron radiation.

  16. Study of liquid gallium as a function of pressure and temperature using synchrotron x-ray microtomography and x-ray diffraction

    SciTech Connect

    Li, Renfeng; Li, Liangliang; Chen, Jiaxuan; Yu, Tony; Wang, Yanbin; Rivers, Mark L.; Wang, Luhong E-mail: haozhe@hit.edu.cn; Cai, Zhonghou; Chen, Jiuhua; Liu, Haozhe E-mail: haozhe@hit.edu.cn

    2014-07-28

    The volume change of liquid and solid gallium has been studied as a function of pressure and temperature up to 3.02 GPa at 300 K and up to 3.63 GPa at 330 K using synchrotron x-ray microtomography combined with energy dispersive x-ray diffraction techniques. Two sets of directly measured P-V data at 300 K and 330 K were obtained from 3D tomography reconstruction data, and the corresponding isothermal bulk moduli were determined as 23.6 (0.5) GPa and 24.6 (0.4) GPa, respectively. The existence of a liquid-liquid phase transition region is proposed based on the abnormal compressibility of Ga melt at about 2.44 GPa and 330 K conditions.

  17. Synchrotron X-ray diffraction study of 112-type Ca1-xLaxFeAs2

    NASA Astrophysics Data System (ADS)

    Katayama, N.; Sugawara, K.; Nakano, A.; Kitou, S.; Sugiyama, Y.; Kawaguchi, N.; Ito, H.; Higuchi, T.; Fujii, T.; Sawa, H.

    2015-11-01

    Synchrotron X-ray diffraction studies of Ca1-xLaxFeAs2 with monovalent arsenic zigzag chain layers are presented. While the crystal twins appear in all samples for the nominal composition of x = 0.25, we successfully obtained the samples without crystal twins for the nominal composition of x = 0.17. We present the structural parameters obtained using the synchrotron X-ray diffraction data and physical properties for the samples with x = 0.17. We further discuss the tactics for exploring novel 112-type iron arsenides without arsenic zigzag chains.

  18. Comparison between x-ray tube-based and synchrotron radiation-based μCT

    NASA Astrophysics Data System (ADS)

    Brunke, Oliver; Brockdorf, Kathleen; Drews, Susanne; Müller, Bert; Donath, Tilman; Herzen, Julia; Beckmann, Felix

    2008-08-01

    Nowadays, X-ray tube-based high-resolution CT systems are widely used in scientific research and industrial applications. But the potential, convenience and economy of these lab systems is often underestimated. The present paper shows the comparison of sophisticated conventional μCT with synchrotron radiation-based μCT (SRμCT). The different aspects and characteristics of both approaches like spatial and density resolution, penetration depth, scanning time or sample size is described in detail. The tube-based μCT measurements were performed with a granite-based nanotom®-CT system (phoenix|x-ray, Wunstorf, Germany) equipped with a 180 kV - 15 W high-power nanofocus® tube with tungsten or molybdenum targets. The tube offers a wide range of applications from scanning low absorbing samples in nanofocus® mode with voxel sizes below 500 nm and highly absorbing objects in the high power mode with focal spot and voxel sizes of a few microns. The SRμCT measurements were carried out with the absorption contrast set-up at the beamlines W 2 and BW 2 at HASYLAB/DESY, operated by the GKSS Research Center. The range of samples examined covers materials of very different absorption levels and related photon energies for the CT scans. Both quantitative and qualitative comparisons of CT scans using biomedical specimens with rather low X-ray absorption such as parts of the human spine as well as using composites from the field of materials science are shown.

  19. MOSFET dosimetry with high spatial resolution in intense synchrotron-generated x-ray microbeams

    SciTech Connect

    Siegbahn, E. A.; Braeuer-Krisch, E.; Bravin, A.; Nettelbeck, H.; Lerch, M. L. F.; Rosenfeld, A. B.

    2009-04-15

    Various dosimeters have been tested for assessing absorbed doses with microscopic spatial resolution in targets irradiated by high-flux, synchrotron-generated, low-energy ({approx}30-300 keV) x-ray microbeams. A MOSFET detector has been used for this study since its radio sensitive element, which is extraordinarily narrow ({approx}1 {mu}m), suits the main applications of interest, microbeam radiation biology and microbeam radiation therapy (MRT). In MRT, micrometer-wide, centimeter-high, and vertically oriented swaths of tissue are irradiated by arrays of rectangular x-ray microbeams produced by a multislit collimator (MSC). We used MOSFETs to measure the dose distribution, produced by arrays of x-ray microbeams shaped by two different MSCs, in a tissue-equivalent phantom. Doses were measured near the center of the arrays and maximum/minimum (peak/valley) dose ratios (PVDRs) were calculated to determine how variations in heights and in widths of the microbeams influenced this for the therapy, potentially important parameter. Monte Carlo (MC) simulations of the absorbed dose distribution in the phantom were also performed. The results show that when the heights of the irradiated swaths were below those applicable to clinical therapy (<1 mm) the MC simulations produce estimates of PVDRs that are up to a factor of 3 higher than the measured values. For arrays of higher microbeams (i.e., 25 {mu}mx1 cm instead of 25x500 {mu}m{sup 2}), this difference between measured and simulated PVDRs becomes less than 50%. Closer agreement was observed between the measured and simulated PVDRs for the Tecomet MSC (current collimator design) than for the Archer MSC. Sources of discrepancies between measured and simulated doses are discussed, of which the energy dependent response of the MOSFET was shown to be among the most important.

  20. Protein folding and protein metallocluster studies using synchrotron small angler X-ray scattering

    SciTech Connect

    Eliezer, D.

    1994-06-01

    Proteins, biological macromolecules composed of amino-acid building blocks, possess unique three dimensional shapes or conformations which are intimately related to their biological function. All of the information necessary to determine this conformation is stored in a protein`s amino acid sequence. The problem of understanding the process by which nature maps protein amino-acid sequences to three-dimensional conformations is known as the protein folding problem, and is one of the central unsolved problems in biophysics today. The possible applications of a solution are broad, ranging from the elucidation of thousands of protein structures to the rational modification and design of protein-based drugs. The scattering of X-rays by matter has long been useful as a tool for the characterization of physical properties of materials, including biological samples. The high photon flux available at synchrotron X-ray sources allows for the measurement of scattering cross-sections of dilute and/or disordered samples. Such measurements do not yield the detailed geometrical information available from crystalline samples, but do allow for lower resolution studies of dynamical processes not observable in the crystalline state. The main focus of the work described here has been the study of the protein folding process using time-resolved small-angle x-ray scattering measurements. The original intention was to observe the decrease in overall size which must accompany the folding of a protein from an extended conformation to its compact native state. Although this process proved too fast for the current time-resolution of the technique, upper bounds were set on the probable compaction times of several small proteins. In addition, an interesting and unexpected process was detected, in which the folding protein passes through an intermediate state which shows a tendency to associate. This state is proposed to be a kinetic molten globule folding intermediate.

  1. Synchrotron Radiation {mu}-X Ray Fluorescence on Multicellular Tumor Spheroids

    SciTech Connect

    Burattini, E.; Cinque, G.; Bellisola, G.; Fracasso, G.; Colombatti, M.; Monti, F.

    2003-01-24

    Synchrotron Radiation micro X-Ray Fluorescence (SR {mu}-XRF) was applied for the first time to map the trace element content on Multicellular Tumor Spheroids (MTS), i.e. human cell clusters used as an in vitro model for testing micrometastases responses to antitumoral drugs. In particular, immunotoxin molecules composed of a carrier protein (Transferrin) bound to a powerful cytotoxin (Ricin A), were here considered as representatives of a class of therapheutic macromolecules used in cancer theraphy. Spheroids included in polyacrylamide gel and placed inside quartz capillaries were studied at the ESRF ID22 beamline using a 15 keV monochromatic photon microbeam. Elemental maps (of Fe, Cu, Zn and Pb) on four groups of spheroids grown under different conditions were studied: untreated, treated only with the carrier molecule or with the toxin alone, and with the complete immunotoxin molecule (carrier+toxin). The results indicate that the distribution of Zn and, to some extent, Cu in the spheroid cells is homogeneous and independent of the treatment type. Total Reflection X-Ray Fluorescence (TR-XRF) was also applied to quantify the average trace element content in the spheroids. Future developments of the technique are finally outlined on the basis of these preliminary results.

  2. 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.

  3. Synchrotron X-ray Scattering Studies of Poly(lactide) Electrospun Fibers Containing Carbon Nanotubes

    NASA Astrophysics Data System (ADS)

    Zhu, Yazhe; Cebe, Peggy

    2014-03-01

    Carbon nanotubes(CNTs) often serve as an effective nucleating agent that facilitates the crystallization of semicrystalline polymers. Here we study the influence of CNTs on thermal and structural properties of Poly-lactide (PLA), which is well-known as a biodegradable and biocompatible thermoplastic polymer. The effect of CNTs on the crystallization and melting behavior of electrospun fibers of poly (L-lactide) (PLLA, with 100% L-isomer) and poly (D-lactide) (PDLA, containing 4% D-isomer) was systemically studied by scanning electron microscopy (SEM), differential scanning calorimetry (DSC), Fourier transform spectroscopy(FT-IR) and real time synchrotron wide-angle X-ray scattering (WAXS) . Multi-walled CNTs were co-electrospun with the poly(lactides) in weight ratios ranging from 0.1 to 4.0 wt% MW-CNT. PLA/carbon nanotubes composite electrospun fibers were successfully produced by appropriate choice of processing conditions and solution concentration. The morphologies of neat and CNT-filled electrospun nanofibers were observed by scanning electron microscopy. WAXS and DSC results show that lower content of CNTs contributes to higher speed of crystallization. However the results also showed that at the highest concentration of CNTs the ultimate crystallinity was reduced. FTIR and X-ray results show that PLA fibers have different crystal forms at high and low crystallization temperature. DSC results also show that D-lactide has reduced crystallinity compared to L-lactide.

  4. Synchronizing femtosecond laser with x-ray synchrotron operating at arbitrarily different frequencies

    SciTech Connect

    Jo, Wonhyuk; Lee, Sooheyong; Eom, Intae; Landahl, Eric C.

    2014-12-15

    The ability to synchronize a femtosecond laser to x-ray pulses is crucial for performing ultrafast time-resolved x-ray scattering experiments at synchrotrons. Conventionally, the task has been achieved by locking a harmonic frequency of the laser oscillator to the storage ring master radio-frequency (RF). However, when the frequency mismatch between the two sources cannot be compensated by small adjustments to the laser cavity length, synchronization to a harmonic frequency requires modifying the optical components of the laser system. We demonstrate a novel synchronization scheme, which is a flexible alternative for synchronizing these two sources operating at arbitrarily different frequencies. First, we find the greatest common divisor (GCD) of the two frequencies that is still within the limited tuning range of the laser cavity length. The GCD is generated by dividing down from the storage ring RF, and is separately multiplied up to provide a feedback signal for synchronizing the laser cavity. Unique to our scheme, the GCD also serves as a harmonic RF source for the laser amplifier such that only laser oscillator pulses at fixed integer multiples of the storage ring RF are selected for amplification and delivery to experiments. Our method is implemented at the Photon Test Facility beamline of Pohang Light Source where timing-jitter less than 4 ps (r.m.s.) is measured using a new shot-to-shot method.

  5. Study of liquid gallium at high pressure using synchrotron x-ray

    SciTech Connect

    Yu, Tony; Guo Quanzhong; Parise, John; Chen Jiuhua; Ehm, Lars; Huang Shu; Luo Shengnian

    2012-06-01

    Liquid gallium has been studied at high pressure up to 2 GPa and ambient temperature in a diamond anvil cell using high energy synchrotron x-ray beam. The total x-ray scattering data of liquid gallium were collected up to Q = 12 A{sup -1} and analyzed using pair distribution functions (PDF). The results indicate that the first nearest neighbor peak and second nearest neighbor (shoulder) peak of PDF in liquid gallium does not change with pressure, whereas the higher order (i.e., third and fourth) nearest neighbor peaks shift towards shorter distance with increasing pressure. Reverse Monte Carlo modeling based on the observed data shows that the coordination number in the liquid gallium increases with pressure from 10.5 at 0.3 GPa to 11.6 at 2 GPa. An atomic arrangement similar to the crystalline phase of Ga(II) with coordination number of 12 is proposed for the locally dense-packed rigid unit in liquid gallium. The volume compression data derived from the structure modeling yield a bulk modulus of 12.1(6) GPa for liquid gallium.

  6. Synchrotron Radiation μ-X Ray Fluorescence on Multicellular Tumor Spheroids

    NASA Astrophysics Data System (ADS)

    Burattini, E.; Cinque, G.; Bellisola, G.; Fracasso, G.; Monti, F.; Colombatti, M.

    2003-01-01

    Synchrotron Radiation micro X-Ray Fluorescence (SR μ-XRF) was applied for the first time to map the trace element content on Multicellular Tumor Spheroids (MTS), i.e. human cell clusters used as an in vitro model for testing micrometastases responses to antitumoral drugs. In particular, immunotoxin molecules composed of a carrier protein (Transferrin) bound to a powerful cytotoxin (Ricin A), were here considered as representatives of a class of therapheutic macromolecules used in cancer theraphy. Spheroids included in polyacrylamide gel and placed inside quartz capillaries were studied at the ESRF ID22 beamline using a 15 keV monochromatic photon microbeam. Elemental maps (of Fe, Cu, Zn and Pb) on four groups of spheroids grown under different conditions were studied: untreated, treated only with the carrier molecule or with the toxin alone, and with the complete immunotoxin molecule (carrier+toxin). The results indicate that the distribution of Zn and, to some extent, Cu in the spheroid cells is homogeneous and independent of the treatment type. Total Reflection X-Ray Fluorescence (TR-XRF) was also applied to quantify the average trace element content in the spheroids. Future developments of the technique are finally outlined on the basis of these preliminary results.

  7. Investigation of GEM-Micromegas detector on X-ray beam of synchrotron radiation

    NASA Astrophysics Data System (ADS)

    Zhang, Yu-Lian; Qi, Hui-Rong; Hu, Bi-Tao; Fan, Sheng-Nan; Wang, Bo; Liu, Mei; Zhang, Jian; Liu, Rong-Guang; Chang, Guang-Cai; Liu, Peng; Ouyang, Qun; Chen, Yuan-Bo; Yi, Fu-Ting

    2014-04-01

    To reduce the discharge of the standard bulk Micromegas and GEM detectors, a GEM-Micromegas detector was developed at the Institute of High Energy Physics. Taking into account the advantages of the two detectors, one GEM foil was set as a preamplifier on the mesh of Micromegas in the structure and the GEM preamplification decreased the working voltage of Micromegas to significantly reduce the effect of the discharge. At the same gain, the spark probability of the GEM-Micromegas detector can be reduced to a factor 0.01 compared to the standard Micromegas detector, and an even higher gain could be obtained. This paper describes the performance of the X-ray beam detector that was studied at 1W2B Laboratory of Beijing Synchrotron Radiation Facility. Finally, the result of the energy resolution under various X-ray energies was given in different working gases. This indicates that the GEM-Micromegas detector has an energy response capability in an energy range from 6 keV to 20 keV and it could work better than the standard bulk-Micromegas.

  8. Synchronizing femtosecond laser with x-ray synchrotron operating at arbitrarily different frequencies

    NASA Astrophysics Data System (ADS)

    Jo, Wonhyuk; Lee, Sooheyong; Eom, Intae; Landahl, Eric C.

    2014-12-01

    The ability to synchronize a femtosecond laser to x-ray pulses is crucial for performing ultrafast time-resolved x-ray scattering experiments at synchrotrons. Conventionally, the task has been achieved by locking a harmonic frequency of the laser oscillator to the storage ring master radio-frequency (RF). However, when the frequency mismatch between the two sources cannot be compensated by small adjustments to the laser cavity length, synchronization to a harmonic frequency requires modifying the optical components of the laser system. We demonstrate a novel synchronization scheme, which is a flexible alternative for synchronizing these two sources operating at arbitrarily different frequencies. First, we find the greatest common divisor (GCD) of the two frequencies that is still within the limited tuning range of the laser cavity length. The GCD is generated by dividing down from the storage ring RF, and is separately multiplied up to provide a feedback signal for synchronizing the laser cavity. Unique to our scheme, the GCD also serves as a harmonic RF source for the laser amplifier such that only laser oscillator pulses at fixed integer multiples of the storage ring RF are selected for amplification and delivery to experiments. Our method is implemented at the Photon Test Facility beamline of Pohang Light Source where timing-jitter less than 4 ps (r.m.s.) is measured using a new shot-to-shot method.

  9. Synchronizing femtosecond laser with x-ray synchrotron operating at arbitrarily different frequencies.

    PubMed

    Jo, Wonhyuk; Lee, Sooheyong; Eom, Intae; Landahl, Eric C

    2014-12-01

    The ability to synchronize a femtosecond laser to x-ray pulses is crucial for performing ultrafast time-resolved x-ray scattering experiments at synchrotrons. Conventionally, the task has been achieved by locking a harmonic frequency of the laser oscillator to the storage ring master radio-frequency (RF). However, when the frequency mismatch between the two sources cannot be compensated by small adjustments to the laser cavity length, synchronization to a harmonic frequency requires modifying the optical components of the laser system. We demonstrate a novel synchronization scheme, which is a flexible alternative for synchronizing these two sources operating at arbitrarily different frequencies. First, we find the greatest common divisor (GCD) of the two frequencies that is still within the limited tuning range of the laser cavity length. The GCD is generated by dividing down from the storage ring RF, and is separately multiplied up to provide a feedback signal for synchronizing the laser cavity. Unique to our scheme, the GCD also serves as a harmonic RF source for the laser amplifier such that only laser oscillator pulses at fixed integer multiples of the storage ring RF are selected for amplification and delivery to experiments. Our method is implemented at the Photon Test Facility beamline of Pohang Light Source where timing-jitter less than 4 ps (r.m.s.) is measured using a new shot-to-shot method.

  10. In situ X-ray tomographic microscopy observations of vesiculation of bubble-free and bubble-bearing magmas

    NASA Astrophysics Data System (ADS)

    Pistone, Mattia; Caricchi, Luca; Fife, Julie L.; Mader, Kevin; Ulmer, Peter

    2015-12-01

    Magma degassing is thought to play a major role in magma fractionation, transport, storage, and volcanic eruption dynamics. However, the conditions that determine when and how magma degassing operates prior to and during an eruption remain poorly constrained. We performed experiments to explore if the initial presence of gas bubbles in magma influences the capability of gas to escape from the magma. Vesiculation of natural H2O-poor (<<1 wt.%) silicic obsidian glasses was investigated by in situ, high-temperature (above the glass transition) experiments using synchrotron-based X-ray tomographic microscopy with high spatial (3 μm/pixel) and temporal resolution (1 second per 3D dataset). As a validation, a second set of experiments was performed on identical starting materials using a Karl-Fisher titration setup to quantify the amount of extracted gas that escapes via volatile diffusion and/or bubble coalescence during vesiculation. In both sets of experiments, vesiculation was triggered by heating the samples at room pressure. Our results suggest that the presence of pre-existing gas bubbles during a nucleation event significantly decreases the tendency of bubbles to coalesce and inhibits magma outgassing. In contrast, in initially bubble-free samples, the nucleation and growth of bubbles is accompanied by significant coalescence and outgassing. We infer that volatile-undersaturated (i.e. bubble-free) magmas in the reservoirs are more likely to erupt effusively, while the presence of excess gas already at depth (i.e. bubble-bearing systems) increases the likelihood of explosive eruptions.

  11. Local structure in diatom biosilica probed by synchrotron x-ray diffraction

    NASA Astrophysics Data System (ADS)

    Dibiccari, Michael; Kwak, Seo-Young; Hind, Geoffrey; Dimasi, Elaine

    2006-03-01

    Diatoms are single-celled algae that form intricate outer shells, or frustrules, composed of biosilica. They have attracted attention in the context of nanotechnology, since the submicron architectures are genetically determined and thus potentially could be reproduced synthetically, by using organic additives that mimic the proteins responsible for controlling biological silicification. We have compared the local atomic structure of diatom biosilica to that of inorganic silica with synchrotron x-ray diffraction, analyzed as the Pair Distribution Function (PDF). Specimens of Thalassiosira weissflogii (Tw) were cleaned of organic matter using either hydrogen peroxide, commercial bleach, or sodium dodecyl sulfate treatments. Low resolution PDF measurements (qmax 13.6 å-1) were made of wet and dry Tw, pure silica microspheres, and diatomaceous earth containing 15% mineral impurities. All samples have similar PDFs, demonstrating that local structure in diatoms and synthetic silica are equivalent, and that the PDF method is insensitive to biological impurites.

  12. Organic-modified and biological silica studied by synchrotron x-ray pair distribution function measurements

    NASA Astrophysics Data System (ADS)

    Dimasi, Elaine; Jeffryes, Clayton; Rorrer, Gregory; Belton, David; Perry, Carole

    2007-03-01

    Biomineralization is a process by which living organisms create composite organic/mineral tissues which have hierarchical structures on micron and submicron scales. Fine control over mineral phase and morphology make biomineralization an important inspiration for materials science. It is often not appreciated that even amorphous minerals such as silica can exhibit hierarchical structure and special properties. One difficulty is that the molecular structures of amorphous phases can be hard to elucidate. We are exploring the use of pair distribution function measurements from synchrotron x-ray scattering to study silica structures, comparing both synthetic organic-modifed silicas and germanium-containing biosilica from diatoms. The raw scattering patterns show clear differences. We will discuss how these data can be scrutinized to determine what differences may be created at the molecular level by different silicification processes.

  13. Dynamic imaging of oil shale pyrolysis using synchrotron X-ray microtomography

    NASA Astrophysics Data System (ADS)

    Saif, Tarik; Lin, Qingyang; Singh, Kamaljit; Bijeljic, Branko; Blunt, Martin J.

    2016-07-01

    The structure and connectivity of the pore space during the pyrolysis of oil shales determines hydrocarbon flow behavior and ultimate recovery. We image the time evolution of the pore and microfracture networks during oil shale pyrolysis using synchrotron X-ray microtomography. Immature Green River (Mahogany Zone) shale samples were thermally matured under vacuum conditions at temperatures up to 500°C while being periodically imaged with a 2 µm voxel size. The structural transformation of both organic-rich and organic-lean layers within the shale was quantified. The images reveal a dramatic change in porosity accompanying pyrolysis between 390 and 400°C with the formation of micron-scale heterogeneous pores. With a further increase in temperature, the pores steadily expand resulting in connected microfracture networks that predominantly develop along the kerogen-rich laminations.

  14. Synchrotron X-ray microprobe and computed microtomography for characterization of nanocatalysts

    NASA Astrophysics Data System (ADS)

    Jones, K. W.; Feng, H.; Lanzirotti, A.; Mahajan, D.

    2005-12-01

    Gas-to-liquids (GTL) is a viable pathway for synthesis of clean fuels from natural gas. One of the attractive synthesis options is the Fischer-Tropsch (F-T) method using an iron catalyst to yield a broad range of hydrocarbons. We collected catalyst samples during three separate F-T runs that utilized nanophase (mean particle diameter (MPD): 3 nm and 20-80 nm) and micrometer-sized (32.5 μm) Fe2O3 that served as catalyst precursors. The collected samples were characterized with micro-X-ray fluorescence and computed microtomography at the National Synchrotron Light Source (NSLS). Results found with two different measurement techniques indicated that there was heterogeneity on a spatial scale corresponding to volumes of roughly 103 μm3.

  15. Synchrotron radiation x-ray beam profile monitor using chemical vapor deposition diamond film

    SciTech Connect

    Kudo, Togo; Takahashi, Sunao; Nariyama, Nobuteru; Hirono, Toko; Tachibana, Takeshi; Kitamura, Hideo

    2006-12-15

    Photoluminescence (PL) of a Si-doped polycrystalline diamond film fabricated using the chemical vapor deposition technique was employed to measure the profile of a synchrotron radiation pink x-ray beam emitted from an in-vacuum hybrid undulator at the SPring-8 facility. The spectrum of the section of the diamond film penetrated by the emitted visible red light exhibited a peak at 739 nm and a wideband structure extending from 550 to 700 nm. The PL intensity increased with the absorbed dose of the incident beam in the diamond within a dynamic range of 10{sup 3}. A two-dimensional distribution of the PL intensity revealed the undulator beam profile.

  16. Compressional residual stress in Bastogne boudins revealed by synchrotron X-ray microdiffraction

    NASA Astrophysics Data System (ADS)

    Chen, Kai; Kunz, Martin; Li, Yao; Zepeda-Alarcon, Eloisa; Sintubin, Manuel; Wenk, Hans-Rudolf

    2016-06-01

    Lattice distortions in crystals can be mapped at the micron scale using synchrotron X-ray Laue microdiffraction (μXRD). From lattice distortions the shape and orientation of the elastic strain tensor can be derived and interpreted in terms of residual stress. Here we apply the new method to vein quartz from the original boudinage locality at Bastogne, Belgium. A long-standing debate surrounds the kinematics of the Bastogne boudins. The μXRD measurements reveal a shortening residual elastic strain, perpendicular to the vein wall, corroborating the model that the Bastogne boudins formed by layer-parallel shortening and not by layer-parallel extension, as is in the geological community generally inferred by the process of boudinage.

  17. A novel crystal bender for x-ray synchrotron radiation monochromators

    NASA Astrophysics Data System (ADS)

    Zaeper, Ralf; Richwin, Matthias; Lützenkirchen-Hecht, Dirk; Frahm, Ronald

    2002-03-01

    A new bending mechanism for an indirectly water cooled monochromator crystal has been developed. The main design goals were a lightweight construction, ease of manufacture, and control. The construction consists of a U-shaped first Si(111) crystal, which can be bent by compressed air to compensate the bowing induced by the heat load from the impinging white synchrotron radiation. The performance of the system was tested at the x-ray undulator beamline BW1 at HASYLAB (Hamburg, Germany). For heat loads between ˜100 and 400 W, rebending of the crystal significantly increases the intensity of the monochromatic beam while the rocking curve is narrowed accordingly, typical widths obtained at 8.9 keV photon energy amount to about 10 arc sec.

  18. Issues of convection in insect respiration: Insights from synchrotron X-ray imaging and beyond

    SciTech Connect

    Socha, John J.; Förster, Thomas D.; Greenlee, Kendra J.

    2010-11-01

    While it has long been known that in small animals, such as insects, sufficient gas transport could be provided by diffusion, it is now recognized that animals generate and control convective flows to improve oxygen delivery across a range of body sizes and taxa. However, size-based methodological limitations have constrained our understanding of the mechanisms that underlie the production of these convective flows. Recently, new techniques have enabled the elucidation of the anatomical structures and physiological processes that contribute to creating and maintaining bulk flow in small animals. In particular, synchrotron X-ray imaging provides unprecedented spatial and temporal resolution of internal functional morphology and is changing the way we understand gas exchange in insects. This symposium highlights recent efforts towards understanding the relationship between form, function, and control in the insect respiratory system.

  19. Failure Analysis of Batteries Using Synchrotron-based Hard X-ray Microtomography.

    PubMed

    Harry, Katherine J; Parkinson, Dilworth Y; Balsara, Nitash P

    2015-08-26

    Imaging morphological changes that occur during the lifetime of rechargeable batteries is necessary to understand how these devices fail. Since the advent of lithium-ion batteries, researchers have known that the lithium metal anode has the highest theoretical energy density of any anode material. However, rechargeable batteries containing a lithium metal anode are not widely used in consumer products because the growth of lithium dendrites from the anode upon charging of the battery causes premature cell failure by short circuit. Lithium dendrites can also form in commercial lithium-ion batteries with graphite anodes if they are improperly charged. We demonstrate that lithium dendrite growth can be studied using synchrotron-based hard X-ray microtomography. This non-destructive imaging technique allows researchers to study the growth of lithium dendrites, in addition to other morphological changes inside batteries, and subsequently develop methods to extend battery life.

  20. Factors influencing real time internal structural visualization and dynamic process monitoring in plants using synchrotron-based phase contrast X-ray imaging

    NASA Astrophysics Data System (ADS)

    Karunakaran, Chithra; Lahlali, Rachid; Zhu, Ning; Webb, Adam M.; Schmidt, Marina; Fransishyn, Kyle; Belev, George; Wysokinski, Tomasz; Olson, Jeremy; Cooper, David M. L.; Hallin, Emil

    2015-07-01

    Minimally invasive investigation of plant parts (root, stem, leaves, and flower) has good potential to elucidate the dynamics of plant growth, morphology, physiology, and root-rhizosphere interactions. Laboratory based absorption X-ray imaging and computed tomography (CT) systems are extensively used for in situ feasibility studies of plants grown in natural and artificial soil. These techniques have challenges such as low contrast between soil pore space and roots, long X-ray imaging time, and low spatial resolution. In this study, the use of synchrotron (SR) based phase contrast X-ray imaging (PCI) has been demonstrated as a minimally invasive technique for imaging plants. Above ground plant parts and roots of 10 day old canola and wheat seedlings grown in sandy clay loam soil were successfully scanned and reconstructed. Results confirmed that SR-PCI can deliver good quality images to study dynamic and real time processes such as cavitation and water-refilling in plants. The advantages of SR-PCI, effect of X-ray energy, and effective pixel size to study plant samples have been demonstrated. The use of contrast agents to monitor physiological processes in plants was also investigated and discussed.