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Sample records for in-situ synchrotron x-ray

  1. 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.

  2. 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.

  3. 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

  4. 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

  5. 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.

  6. 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.

  7. 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.

  8. In situ synchrotron x-ray studies of LiMn{sub 2}O{sub 4} cathodes

    SciTech Connect

    McBreen, J.; Mukerjee, S.; Yang, X.Q.

    1997-05-01

    LiCoO{sub 2} cathodes are now used in most commercial lithium ion batteries. LiMn{sub 2}O{sub 4} is an attractive low cost alternative. However, it is difficult to make reproducibly. At Brookhaven National Laboratory two in situ synchrotron x-ray techniques, that are available at the National Synchrotron Light Source (NSLS), have been used to investigate LiMn{sub 2}O{sub 4}. The techniques are x-ray absorption and high resolution x-ray diffraction. With x-ray absorption it is possible to follow the changes in the Mn oxidation state and the changes in the Mn-O and Mn-Mn bond lengths on cycling. Also it is possible to detect amorphous phases. The high energy x-rays at the diffraction Beam Lines at the NSLS (up to 24 KeV) permit in situ x-ray diffraction, in the transmission mode, in thin lithium and lithium ion cells. The evolution of the structural chances that occur on cycling can be followed. These in situ measurements were done on Li/LiMn{sub 2}O{sub 4} cells with a liquid electrolyte (1 M LiPF{sub 6} in a 1:1:3 PC:EC:DMC solvent).

  9. In Situ Synchrotron X-Ray Techniques for the Study of Lithium Battery Materials

    SciTech Connect

    McBreen, J.; Mukerjee, S.; Yang, X. Q.; Sun, X., Ein-Eli, Y.

    1998-11-01

    The combination of in situ X-ray diffraction (XRD) and x-ray absorption spectroscopy (XAS) is a very powerful technique in the study of lithium battery cathode materials. XRD identifies the phase changes that occur during cycling and XAS gives information on the redox charge compensation processes that occur on the transition metal oxides. Because of its element specific nature XAS can identify the occurrence of redox processes on the various cations in doped oxide cathode materials. Since XAS probes short range order and is particularly useful in the study of amorphous tin based composite oxide anode materials.

  10. 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.

  11. 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

  12. Recent progress on synchrotron-based in-situ soft X-ray spectroscopy for energy materials.

    PubMed

    Liu, Xiaosong; Yang, Wanli; Liu, Zhi

    2014-12-10

    Soft X-ray spectroscopy (SXS) techniques such as photoelectron spectroscopy, soft X-ray absorption spectroscopy and X-ray emission spectroscopy are efficient and direct tools to probe electronic structures of materials. Traditionally, these surface sensitive soft X-ray techniques that detect electrons or photons require high vacuum to operate. Many recent in situ instrument developments of these techniques have overcome this vacuum barrier. One can now study many materials and model devices under near ambient, semi-realistic, and operando conditions. Further developments of integrating the realistic sample environments with efficient and high resolution detection methods, particularly at the high brightness synchrotron light sources, are making SXS an important tool for the energy research community. In this progress report, we briefly describe the basic concept of several SXS techniques and discuss recent development of SXS instruments. We then present several recent studies, mostly in situ SXS experiments, on energy materials and devices. Using these studies, we would like to highlight that the integration of SXS and in situ environments can provide in-depth insight of material's functionality and help researchers in new energy material developments. The remaining challenges and critical research directions are discussed at the end. PMID:24799004

  13. 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.

  14. 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.

  15. 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.

  16. 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

  17. A flow cell for in situ synchrotron x-ray diffraction studies of scale formation under Bayer processing conditions.

    PubMed

    Webster, Nathan A S; Madsen, Ian C; Loan, Melissa J; Scarlett, Nicola V Y; Wallwork, Kia S

    2009-08-01

    The design, construction, and commissioning of a stainless steel flow cell for in situ synchrotron x-ray diffraction studies of scale formation under Bayer processing conditions is described. The use of the cell is demonstrated by a study of Al(OH)(3) scale formation on a mild steel substrate from synthetic Bayer liquor at 70 degrees C. The cell design allows for interchangeable parts and substrates and would be suitable for the study of scale formation in other industrial processes. PMID:19725670

  18. In-situ Synchrotron X-ray Microdiffraction Study of Lattice Rotation in Polycrystalline Materials during Uniaxial Deformations

    SciTech Connect

    Joo, H.D.; Bark, C.W.; Koo, Y.M.; Kim, K.H.; Tamura, N.

    2004-05-12

    Recent experiments have shown that formation of dislocation cell structures and rotation of structural elements at the macroscopic level are fundamental to the development of plastic deformation. However, attention should also be focused on micro-volumes because local stress and strain can significantly differ from their averaged values at the macroscale. In-situ orientation measurements in copper polycrystals during uniaxial deformation were performed using synchrotron x-ray microdiffraction at the Advanced Light Source. We observed heterogeneities in deformation-induced microstructure within individual grains. Different slip systems in particular can be simultaneously activated among neighboring volume elements of individual grains.

  19. In-situ synchrotron X-ray microdiffraction study of lattice rotation in polycrystalline materials during uniaxial deformations

    SciTech Connect

    Joo, H.D.; Kim, K.H.; Bark, C.W.; Koo, Y.M.; Tamura, N.

    2004-07-19

    Recent experiments have shown that formation of dislocation cell structures and rotation of structural elements at the macroscopic level are fundamental to the development of plastic deformation. However, attention should also be focused on micro-volumes because local stress and strain can significantly differ from their averaged values at the macroscale. In-situ orientation measurements in copper polycrystals during uniaxial deformation were performed using synchrotron x-ray microdiffraction at the Advanced Light Source. We observed heterogeneities in deformation-induced microstructure within individual grains. Different slip systems in particular can be simultaneously activated among neighboring volume elements of individual grains.

  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. PMID:23206092

  2. Neighborite Under High Pressure: In Situ Angle Dispersive X-ray Diffraction Study Using Synchrotron Radiation

    NASA Astrophysics Data System (ADS)

    Liu, H.; Chen, J.; Weidner, D.; Hu, J.; Meng, Y.; Mao, H.

    2003-12-01

    The neighborite (NaMgF3) is an ideal analogue model for silicate perovskite (MgSiO3) due to the similarities between their crystal and electronic structures. The advantage of the analogue study is that the weaker bonding feature of neighborite grants us the opportunity to simulate behavior of silicate perovskite at lower mantlei. e.high pressure and high temperature condition, at relatively lower P-T conditions. The previous high pressure studies for neighborite were reported by Zhao et al [1, 2]. Energy dispersive x-ray diffraction data were achieved within 10GPa and 1000oC, while angle dispersive x-ray diffraction data were obtained only at 4.9GPa and room temperature.More information of atomic position change is required to reveal the role of MgF6 octahedral framework tilting during its phase transition process responding to heating andcompressing. Thus the high-resolution monochromatic x-ray powder diffraction studies on NaMgF3 perovskite at high pressure were carried out using diamond anvil cell at X17C of National Synchrotron Light Source (Brookhaven) and HPCAT of Advance Photon Source (Argonne). The orthorhombic structure keeps stable under pressure up to 30 GPa, and the crystal structure is refined using Rietveld method. The result indicates that tilting angle of the MgF6 octahedral framework increases continually while the octahedral Mg-F bond length decreases slightly with increasing pressure.Difference between the tilting angles derived from macro-structure (lattice parameters) and from micro-structure (atomic positions), as well as the trend of change in the tilting angle with temperature and pressureare discussed. [1]. Zhao YS, Weidner DJ, Ko JD, Leinenweber K, Liu X, Li BS, Meng Y,Pacalo REG, Vaughan MT, Wang YB, Yeganehhaeri A,J.Geophys. Res. Solid Earth, 99 (1994) 2871. [2]. Zhao YS, Parise JB, Wang YB, Kusaba K, Vaughan MT, Weidner DJ, Kikegawa T, Chen J, Shimomura O,Am.Miner., 79 (1994) 615.

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

    SciTech Connect

    Yang, X. Q.; Sun, X.; Lee, S. J.; McBreen, J.; Mukerjee, S.; Daroux, M. L.; Xing, X. K.

    1998-11-01

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

  5. 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.

  6. Analysis of heat-affected zone phase transformations using in situ spatially resolved x-ray diffraction with synchrotron radiation

    SciTech Connect

    Elmer, J.W.; Wong, J.; Froeba, M.; Waide, P.A.; Larson, E.M.

    1996-03-01

    Spatially resolved X-ray diffraction (SRXRD) consists of producing a submillimeter size X-ray beam from an intense synchrotron radiation source to perform real-time diffraction measurements on solid materials. This technique was used int his study to investigate the crystal phases surrounding a liquid weld pool in commercial purity titanium and to determine the location of the phase boundary separating the high-temperature body-centered-cubic (bcc) {beta} phase from the low-temperature hexagonal-close-packed (hcp) {alpha} phase. The experiments were carried out at the Stanford Synchrotron Radiation Laboratory (SSRL) using a 0.25 x 0.50 mm X-ray probe that could be positioned with 10-{micro}m precision on the surface of a quasistationary gas tungsten arc weld (GTAW). The SRXRD results showed characteristic hcp, bcc, and liquid diffraction patterns at various points along the sample, starting from the base metal through the heat-affected zone (HAZ) and into the weld pool, respectively. Analyses of the SRXRD data show the coexistence of bcc and hcp phases in the partially transformed (outer) region of the HAZ and single-phase bcc in the fully transformed (inner) region of the HAZ. Postweld metallographic examinations of the HAZ, combined with a conduction-based thermal model of the weld, were correlated with the SRXRD results. Finally, analysis of the diffraction intensities of the hcp and bcc phases was performed on the SRXRD data to provide additional information about the microstructural conditions that may exist in the HAZ at temperature during welding. This work represents the first direct in situ mapping of phase boundaries in fusion welds.

  7. In Situ Synchrotron X-ray Diffraction Measurement of the Strain Distribution in Si Die for the Embedded Substrates

    NASA Astrophysics Data System (ADS)

    Hsu, Hsueh Hsien; Chen, Hao; Ouyang, Yao Tsung; Chiu, Tz Cheng; Chang, Tao Chih; Lee, Hsin Yi; Ku, Chin Shun; Wu, Albert T.

    2015-10-01

    Three-dimensional packaging provides an acceptable solution for miniaturized integrated circuits. Because of the technological flexibility required for combining various modules to form a functional system, miniaturization can be achieved by using embedded techniques that could enhance the reliability of assembled systems. Because the mismatch of the thermal expansion coefficient among the materials has been an emerging issue when embedded components are subjected to thermal cycles, this study adopted the in situ synchrotron x-ray method to measure the strain distribution of a Si die in embedded substrates at various temperatures ranging from 25°C to 150°C. The out-of-plane strain of the Si die became less compressive when the temperature was increased. The numerical simulation of the finite elements software ANSYS also indicated the similar consequence of the strain behavior.

  8. In-situ early stage electromigration study in Al line using synchrotron polychromatic X-ray microdiffraction

    SciTech Connect

    Chen, Kai; Tamura, Nobumichi; Tu, King-Ning

    2007-10-31

    Electromigration is a phenomenon that has attracted much attention in the semiconductor industry because of its deleterious effects on electronic devices (such as interconnects) as they become smaller and current density passing through them increases. However, the effect of the electric current on the microstructure of interconnect lines during the very early stage of electromigration is not well documented. In the present report, we used synchrotron radiation based polychromatic X-ray microdiffraction for the in-situ study of the electromigration induced plasticity effects on individual grains of an Al (Cu) interconnect test structure. Dislocation slips which are activated by the electric current stressing are analyzed by the shape change of the diffraction peaks. The study shows polygonization of the grains due to the rearrangement of geometrically necessary dislocations (GND) in the direction of the current. Consequences of these findings are discussed.

  9. In situ investigation of working battery electrodes using synchrotron x-ray diffraction

    SciTech Connect

    Jisrawi, N.M.; Thurston, T.R.; Yang, X.Q.

    1996-12-31

    The results of an in situ investigation of the structural changes that occur during the operation of working battery electrodes using synchrotron radiation are presented. Two types of electrodes were investigated: an AB{sub 2}-type Laves phase alloy anode with the composition Zr{sub x}Ti{sub 1-x}M{sub 2} and a proprietary cell based on a Li{sub x}Mn{sub 2}O{sub 4} spinel compound cathode made by Gould electronics. For the Laves phase alloy compositions with x=0.25 and 0.5 and M=V{sub 0.5}N{sub 1.1}Mn{sub 0.2}Fe{sub 0.2} were examined. Cells made from two different batches of Li{sub x}Mn{sub 2}O{sub 4} material were investigated. The relationships between battery performance and structural changes will be discussed. In the later case, we also discuss the role of over-discharging on the Li{sub x}Mn{sub 2}O{sub 4} structure and on battery operation.

  10. 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). PMID:23949378

  11. In situ Rheological Measurements at Extreme Pressure and Temperature using Synchrotron X-ray Diffraction and Radiography

    SciTech Connect

    Raterron, P.; Merkel, S

    2009-01-01

    Dramatic technical progress seen over the past decade now allows the plastic properties of materials to be investigated under extreme pressure and temperature conditions. Coupling of high-pressure apparatuses with synchrotron radiation significantly improves the quantification of differential stress and specimen textures from X-ray diffraction data, as well as specimen strains and strain rates by radiography. This contribution briefly reviews the recent developments in the field and describes state-of-the-art extreme-pressure deformation devices and analytical techniques available today. The focus here is on apparatuses promoting deformation at pressures largely in excess of 3 GPa, namely the diamond anvil cell, the deformation-DIA apparatus and the rotational Drickamer apparatus, as well as on the methods used to carry out controlled deformation experiments while quantifying X-ray data in terms of materials rheological parameters. It is shown that these new techniques open the new field of in situ investigation of materials rheology at extreme conditions, which already finds multiple fundamental applications in the understanding of the dynamics of Earth-like planet interior.

  12. Hydrothermal synthesis of nanocrystalline ZnSe: An in situ synchrotron radiation X-ray powder diffraction study

    SciTech Connect

    Jorgensen, J.-E. Jensen, T.R.; Hanson, J.C.

    2008-08-15

    The hydrothermal synthesis of nanocrystalline ZnSe has been studied by in situ X-ray powder diffraction using synchrotron radiation. The formation of ZnSe was studied using the following starting mixtures: Zn+Se+H{sub 2}O (route A) and ZnCl{sub 2}+Se+H{sub 2}O+Na{sub 2}SO{sub 3} (route B). The route A experiment showed that Zn powder starts reacting with water at 134 deg. C giving ZnO and H{sub 2} followed by the formation of ZnSe which takes place in temperature range from 167 to 195 deg. C. The route B experiment shows a considerably more complex reaction path with several intermediate phases and in this case the formation of ZnSe starts at 141 deg. C and ZnSe and Se were the only crystalline phases observed at the end of the experiment where the temperature was 195 deg. C. The sizes of the nanocrystalline particles were determined to 18 and 9 nm in the route A and B experiments, respectively. Nanocrystalline ZnSe was also synthesized ex situ using the route A and B methods and characterized by conventional X-ray powder diffraction and transmission electron microscopy. An average crystalline domain size of ca. 8 nm was determined by X-ray powder diffraction in fair agreement with TEM images, which showed larger aggregates of nanoparticles having approximate diameters of 10 nm. Furthermore, a method for purification of the ZnSe nanoparticles was developed and the prepared particles showed signs of anisotropic size broadening of the diffraction peaks. - Graphical abstract: Stack of powder diagrams showing the formation of nanocrystalline ZnSe under hydrothermal conditions.

  13. Hydrothermal Synthesis of Nanocrystalline ZnSe: An in situ Synchrotron Radiation X-ray Powder Diffraction Study

    SciTech Connect

    Joergensen,J.; Jensen, T.; Hanson, J.

    2008-01-01

    The hydrothermal synthesis of nanocrystalline ZnSe has been studied by in situ X-ray powder diffraction using synchrotron radiation. The formation of ZnSe was studied using the following starting mixtures: Zn+Se+H2O (route A) and ZnCl2+Se+H2O+Na2SO3 (route B). The route A experiment showed that Zn powder starts reacting with water at 134 C giving ZnO and H2 followed by the formation of ZnSe which takes place in temperature range from 167 to 195 C. The route B experiment shows a considerably more complex reaction path with several intermediate phases and in this case the formation of ZnSe starts at 141 C and ZnSe and Se were the only crystalline phases observed at the end of the experiment where the temperature was 195 C. The sizes of the nanocrystalline particles were determined to 18 and 9 nm in the route A and B experiments, respectively. Nanocrystalline ZnSe was also synthesized ex situ using the route A and B methods and characterized by conventional X-ray powder diffraction and transmission electron microscopy. An average crystalline domain size of ca. 8 nm was determined by X-ray powder diffraction in fair agreement with TEM images, which showed larger aggregates of nanoparticles having approximate diameters of 10 nm. Furthermore, a method for purification of the ZnSe nanoparticles was developed and the prepared particles showed signs of anisotropic size broadening of the diffraction peaks.

  14. 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.

  15. 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.

  16. 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

  17. 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).

  18. Synchrotron X-Ray Microprobe In-Situ Analysis of Extraterrestrial Particles Collected in Aerogel on the MIR Space Station

    NASA Technical Reports Server (NTRS)

    Flynn, G. J.; Sutton, S. R.; Horz, F.

    2000-01-01

    Using in-situ x-ray fluorescence, we determined the Cr/Fe, Mn/Fe and Ni/Fe of a particle captured in aerogel on MIR are approximately chondritic, indicating an extraterrestrial origin. Impurity of the aerogel precluded determining the Cu and Zn.

  19. 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

  20. 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.

  1. In-situ Monitoring the Inhibiting Effect of Polyphophinocarboxylic Acid on CaCO3 Scale Formation by Synchrotron X-ray Diffraction

    SciTech Connect

    Chen, T.; Neville, A; Sorbie, K; Zhong, Z

    2009-01-01

    The formation of calcium carbonate mineral scale is a persistent and expensive problem in oil and gas production. The aim of this paper is to further the understanding of scale formation and inhibition by in-situ probing of crystal growth by synchrotron radiation wide angle X-ray scattering (WAXS) in the absence and presence of polyphosphinocarboxylic acid (PPCA) scale inhibitor. This technique offers an exciting prospect for the study of scaling.

  2. 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.

  3. 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.

  4. 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.

  5. 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

  6. 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

  7. 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.

  8. Complementary Control by Additivies of the Kinetics of Amorphous CaCO3 Mineralization at an Organic Interface: In-Situ Synchrotron X-ray Observations

    SciTech Connect

    DiMasi,E.; Kwak, S.; Amos, F.; Olszta, M.; Lush, D.; Gower, L.

    2006-01-01

    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.

  9. 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.

  10. 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.

  11. Formation of Delta Ferrite in 9 Wt Pct Cr Steel Investigated by In-Situ X-Ray Diffraction Using Synchrotron Radiation

    NASA Astrophysics Data System (ADS)

    Mayr, P.; Palmer, T. A.; Elmer, J. W.; Specht, E. D.; Allen, S. M.

    2010-10-01

    In-situ X-ray diffraction (XRD) measurements using high energy synchrotron radiation were performed to monitor in real time the formation of delta ferrite in a martensitic 9 wt pct 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 K/s heating rate to 1573 K (1300 °C) and subsequent cooling. At the peak temperature, the delta ferrite concentration rose to 19 pct, of which 17 pct transformed back to austenite on subsequent cooling.

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

    DOE PAGESBeta

    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.

  13. 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.

  14. 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.

  15. 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.

  16. 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.

  17. 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

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

    NASA Astrophysics Data System (ADS)

    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.

    2016-03-01

    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.

  19. Large-scale orientation in a vulcanized stretched natural rubber network: proved by in situ synchrotron X-ray diffraction characterization.

    PubMed

    Weng, Gengsheng; Huang, Guangsu; Qu, Liangliang; Nie, Yijing; Wu, Jinrong

    2010-06-01

    In situ studies of strain-induced crystallization in unfilled and multiwalled carbon nanotube (MWCNT)-filled natural rubber (NR) were carried out by using synchrotron wide-angle X-ray diffraction (WAXD). Synchrotron WAXD results indicate that more nuclei appear in the MWCNT-filled NR sample, leading to higher crystallinity, lower onset strain of crystallization, and remarkable enhancement in tensile strength. During deformation, despite the amorphous chains remaining in isotropic orientation, the domains of larger scale (10-100 nm) with high network chain density in the NR matrix are oriented. The MWCNTs induce significant variation of this orientational process, and it is monitored by the stearic acid (SA) crystallites, which are effective nanoprobes of the amorphous phase. The results indicate that a small amount of MWCNTs and SA crystallites can be used as new tools to analyze the microstructural orientation of NR during deformation. The results also yield new insight into the strain-induced crystallization mechanism. PMID:20455577

  20. Pressure-induced amorphization of cubic Zr W2 O8 studied in situ and ex situ by synchrotron x-ray diffraction and absorption

    NASA Astrophysics Data System (ADS)

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

    2005-07-01

    The behavior of cubic ZrW2O8 on compression in a DAC to 7.6GPa 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 ZrW2O8 recovered from 7.5GPa in a multianvil apparatus. The in situ diffraction data show the complete formation of orthorhombic ZrW2O8 at low pressure (<0.5GPa) , and amorphization onset at >2.4GPa with completion at <7.6GPa . 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 LI 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.

  1. 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.

  2. 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.

  3. 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.

  4. Solubility of Minerals in HP-HT Aqueous Fluids: Results and Potentials of in situ Synchrotron X-Ray Fluorescence

    NASA Astrophysics Data System (ADS)

    Daniel, I.; Sanchez Valle, C.; Reynard, B.; Martinez, I.; Simionovici, A. S.

    2005-12-01

    CO2-rich saline aqueous fluids are liberated into the mantle when the altered oceanic crust is subducted, leading to the important geochemical phenomena of mantle wedge metasomatism and arc magmatism. To better understand these processes, knowledge of mineral-fluid equilibria and mineral solubility in high pressure-high temperature crustal fluids is thus required. We report here in situ measurements on the solubility of strontianite (SrCO3) and GeO2-rutile at P (up to 6.6 GPa) and T (up to 400°C) relevant for cold subducted slabs. The composition of the fluid surrounding the crystal, loaded in an externally heated diamond-anvil cell, was analysed in situ by monitoring the X-ray fluorescence of Sr2+ and Ge4+ cations, respectively, until chemical equilibrium was reached. Experiments were carried out at the ESRF (ID22 beamline) using a high-resolution monochromatic beam (2x5 μm2 and 18 keV), and a collection geometry at 30° from the transmitted beam. This results in quantitative analysis of the solution down to the 20 ppm level. In the case of strontianite, kinetic data of the dissolution reaction showed instantaneous equilibration times at 400°C. Measured dissolution rates are essentially compatible with a first-order reaction mechanism and allow to retrieve the activation energy (E_A) for the dissolution of SrCO3 at HP-HT conditions. Taking into account activity coefficients, measured Sr2+ concentrations are used to determine the solubility constant (K_s) of SrCO3 at HP-HT conditions, allowing further thermodynamic modelling of carbonate dissolution. In the case of GeO2-rutile, we observed a gradient of the Ge concentration in the fluid. Hence, on the top of solubility measurements, it also allows to calculate the diffusion coefficients of Ge in high P-T aqueous fluids. This experiment thus shows the suitability of the SXRF technique for the in situ study of elemental diffusion in aqueous systems under high P-T conditions. Such data are essential for the

  5. 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.

  6. 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.

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

    PubMed

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

    2014-08-01

    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. PMID:25173271

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

    NASA Astrophysics Data System (ADS)

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

    2014-08-01

    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.

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

    NASA Astrophysics Data System (ADS)

    Chen, Kai; Tamura, N.; Kunz, M.; Tu, K. N.; Lai, Yi-Shao

    2009-07-01

    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 β-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 builtup 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 β-Sn derived from the electromigration data is in good agreement with the calculated value.

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

    NASA Astrophysics Data System (ADS)

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

    2016-04-01

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

  11. 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.

  12. 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.

  13. 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

  14. A second-order phase-transformation of the dislocation structure during plastic deformation determined by in situ synchrotron X-ray diffraction

    SciTech Connect

    Schafler, E.; Simon, K.; Bernstorff, S.; Tichy, G.; Ungar, T. . E-mail: ungar@ludens.elte.hu; Zehetbauer, M.J.

    2005-01-10

    In situ X-ray diffraction peak profile analysis during plastic deformation in [0 0 1] oriented copper single crystals was carried out using synchrotron radiation. Characteristic changes of the hardening coefficient indicate that a transition occurs from stage III to stage IV which has been observed for the first time in a single crystal under low temperature deformation conditions. The long-range internal stresses, the dislocation arrangement parameters and the fluctuations of the dislocation density show non-monotonous changes at this transition suggesting that the dislocation structure, especially within the cell-wall regions, reveals a second-order phase transition. A microscopic dislocation model is introduced which not only illustrates the break of symmetry, but also describes well the development of new grains ('fragmentation') during plastic deformation.

  15. 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.

  16. 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.

  17. (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

  18. Oxygen storage properties of La1-xSrxFeO3- for chemical-looping reactions an in-situ neutron and synchrotron X-ray study

    SciTech Connect

    Taylor, Daniel; Schreiber, Nathaniel; Levitas, Benjamin; Xu, Wenqian; Rodriguez, Efrain E

    2016-01-01

    Oxygen storage materials (OSMs) provide lattice oxygen for a number of chemical-looping reactions including natural gas combustion and methane reforming. La1 xSrxFeO3 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 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 an envelope , or temperature range, of oxygen storage capacity (OSC), where oxygen can easily and reversibly be inserted and removed from the OSM. Our in situ X-ray and neutron diffraction results reveal that while samples with higher Sr contents had a higher OSC, those same samples suffered from slower reaction kinetics and some, such as the x = 1/2 and x = 2/3 compositions, had local variations in Sr content, which led to inhomogeneous regions with varying reaction rates. Therefore, we highlight the importance of in situ diffraction studies, and we propose that these measurements are required for the thorough evaluation of future candidate OSMs. We recommend La2/3Sr1/3FeO3 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.

  19. 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.

  20. Oxygen storage properties of La1-xSrxFeO3- for chemical-looping reactions an in-situ neutron and synchrotron X-ray study

    DOE PAGESBeta

    Taylor, Daniel; Schreiber, Nathaniel; Levitas, Benjamin; Xu, Wenqian; Rodriguez, Efrain E

    2016-01-01

    Oxygen storage materials (OSMs) provide lattice oxygen for a number of chemical-looping reactions including natural gas combustion and methane reforming. La1 xSrxFeO3 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 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, wemore » discover an envelope , or temperature range, of oxygen storage capacity (OSC), where oxygen can easily and reversibly be inserted and removed from the OSM. Our in situ X-ray and neutron diffraction results reveal that while samples with higher Sr contents had a higher OSC, those same samples suffered from slower reaction kinetics and some, such as the x = 1/2 and x = 2/3 compositions, had local variations in Sr content, which led to inhomogeneous regions with varying reaction rates. Therefore, we highlight the importance of in situ diffraction studies, and we propose that these measurements are required for the thorough evaluation of future candidate OSMs. We recommend La2/3Sr1/3FeO3 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

  1. In situ analysis of elemental depth distributions in thin films by combined evaluation of synchrotron x-ray fluorescence and diffraction

    SciTech Connect

    Mainz, R.; Klenk, R.

    2011-06-15

    In this work we present a method for the in situ analysis of elemental depth distributions in thin films using a combined evaluation of synchrotron x-ray fluorescence and energy-dispersive x-ray diffraction signals. We recorded diffraction and fluorescence signals simultaneously during the reactive annealing of thin films. By means of the observed diffraction signals, the time evolution of phases in the thin films during the annealing processes can be determined. We utilized this phase information to parameterize the depth distributions of the elements in the films. The time-dependent fluorescence signals were then taken to determine the parameters representing the parameterized depth distributions. For this latter step, we numerically calculated the fluorescence intensities for a given set of depth distributions. These calculations handle polychromatic excitation and arbitrary functions of depth distributions and take into account primary and secondary fluorescence. Influences of lateral non-uniformities of the films, as well as the accuracy limits of the method, are investigated. We apply the introduced method to analyze the evolution of elemental depth distributions and to quantify the kinetic parameters during a synthesis process of CuInS{sub 2} thin films via the reactive annealing of Cu-In precursors in a sulfur atmosphere.

  2. 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.

  3. 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.

  4. Evolution of Crack-Tip Transformation Zones in Superelastic Nitinol Subjected to in Situ Fatigue. a Fracture Mechanics And Synchrotron X-Ray Microdiffraction Analysis

    SciTech Connect

    Robertson, S.W.; Mehta, A.; Pelton, A.R.; Ritchie, R.O.; /UC, Berkeley /SLAC, SSRL

    2009-04-29

    The ultrahigh spatial resolution ({approx}1 {micro}m{sup 2}) of synchrotron X-ray microdiffraction is combined with fracture mechanics techniques to directly measure in situ three-dimensional strains, phases and crystallographic alignment ahead of a growing fatigue crack (100 cycles in situ) in superelastic Nitinol. The results provide some surprising insights into the growth of cracks in phase-transforming material at the microscale. Specifically, despite a macroscopic superelastic strain recovery of 6-8% associated with the phase transformation, individual austenite grains experience local strains of less than 1.5%. This observation indicates that it is the localized process of the accommodation of the transformation and subsequent loading of the martensite that provide the main source of the large recoverable strains. Furthermore, the plastic region ahead of the crack is composed of deformed martensite. This micromechanical transformation process is dependent upon the material texture, and directly influences the transformation zone size/shape as well as the crack path.

  5. 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.

  6. 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.

  7. 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

  8. 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

  9. 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.

  10. 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

  11. Temperature Dependence of the Structural Parameters in the Transformation of Aragonite to Calcite, as Determined from In Situ Synchrotron Powder X-ray-Diffratction Data

    SciTech Connect

    Antao, Sytle M.; Hassan, Ishmael

    2011-09-06

    The temperature dependency of the crystal structure and the polymorphic transition of CaCO{sub 3} from aragonite to calcite were studied using Rietveld structure refinement and high-temperature in situ synchrotron powder X-ray-diffraction data at ambient pressure, P. The orthorhombic metastable aragonite at room P, space group Pmcn, transforms to trigonal calcite, space group R{bar 3}c, at about T{sub c} = 468 C. This transformation occurs rapidly; it starts at about 420 C and is completed by 500 C, an 80 C interval that took about 10 minutes using a heating rate of 8 C/min. Structurally, from aragonite to calcite, the distribution of the Ca atom changes from approximately hexagonal to cubic close-packing. A 5.76% discontinuous increase in volume accompanies the reconstructive first-order transition. Besides the change in coordination of the Ca atom from nine to six from aragonite to calcite, the CO{sub 3} groups change by a 30{sup o} rotation across the transition.

  12. 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.

  13. In situ synchrotron wide-angle X-ray diffraction investigation of fatigue cracks in natural rubber.

    PubMed

    Rublon, Pierre; Huneau, Bertrand; Saintier, Nicolas; Beurrot, Stéphanie; Leygue, Adrien; Verron, Erwan; Mocuta, Cristian; Thiaudière, Dominique; Berghezan, Daniel

    2013-01-01

    Natural rubber exhibits remarkable mechanical fatigue properties usually attributed to strain-induced crystallization. To investigate this phenomenon, an original experimental set-up that couples synchrotron radiation with a homemade fatigue machine has been developed. Diffraction-pattern recording is synchronized with cyclic loading in order to obtain spatial distributions of crystallinity in the sample at prescribed times of the mechanical cycles. Then, real-time measurement of crystallinity is permitted during uninterrupted fatigue experiments. First results demonstrate the relevance of the method: the set-up is successfully used to measure the crystallinity distribution around a fatigue crack tip in a carbon black filled natural rubber for different loading conditions. PMID:23254662

  14. 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.

  15. 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.

  16. 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.

  17. 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

  18. In-situ synchrotron radiation x-ray diffraction and visual imaging study of magnesite + quartz + water at mid-crustal temperatures and pressures

    NASA Astrophysics Data System (ADS)

    Kerrigan, R. J.; Candela, P. A.; Piccoli, P. M.

    2009-12-01

    The system MgO-SiO2-H2O-CO2 (MSHC) has been investigated to observe the decarbonation of magnesite and the kinetics of mineral dissolution/precipitation in the presence of a silica-rich fluid. Hydrothermal experiments containing magnesite + quartz + water under greenschist to amphibolite facies temperatures and pressures (up to 765°C and 1 GPa) were conducted in a Bassett-type hydrothermal diamond anvil cell (HDAC). Two sets of experiments were conducted: (1) experiments monitored by using visible light microscopy, digitally recorded to track apparent dissolution and precipitation changes, and (2) experiments monitored over time by synchrotron radiation x-ray diffraction (SR-XRD). Our experiments have produced minerals of a fibrous habit, a morphology sometimes linked to respiratory illnesses. Understanding the conditions that promote the growth of fibrous minerals will allow us to better identify geological environments wherein they may form. The starting materials consist of two equidimensional grains of magnesite and quartz (~0.05 mm in diameter) in deionized H2O. The sample chamber is confined by the two diamonds (1mm culet) and a rhenium gasket (0.3 mm diameter, 0.15 mm thick). Experimental temperatures and pressures were progressively increased, step-wise through 450-765°C and 0.1-1GPa, with several isothermal steps of 30-90 minutes duration. Experiments were returned to 465°C before quench. The final equilibrium assemblage was dependent on the molar ratio of starting materials. Images of digitally recorded experiments were analyzed to track apparent changes of mineral proportions over time. In-situ SR-XRD, provides phase identification information and data on reaction progress through the relative abundance of reactants and products. Changes in characteristic x-ray peak intensity, morphology and cross-sectional area, allows for the determination of important physical properties and kinetic parameters for the reactant and product phases. At temperatures

  19. 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.

  20. 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

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

    DOE PAGESBeta

    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

  2. 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.

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

    NASA Astrophysics Data System (ADS)

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

    2016-02-01

    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.

  4. 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

  5. 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.

  6. 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. PMID:26429486

  7. 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.

  8. Synchrotron beamlines for x-ray lithography

    NASA Astrophysics Data System (ADS)

    Trippe, Anthony P.; Pearce, W. J.

    1994-02-01

    Louisiana State University established the J. Bennett Johnston, Sr., Center for Advanced Microstructures and Devices (CAMD). Designed and constructed by the Brobeck Division of Maxwell Laboratories, the CAMD synchrotron light source is the first electron storage ring to be built by a commercial company in the United States. The synchrotron x-ray radiation generated at CAMD is an extremely useful exposure source for both thin and thick film lithography. Passing through a beamline containing two plane mirrors, the synchrotron light is used to expose thin resists for lithography of patterns with feature sizes of 0.25 micron and smaller. Two thick-resist beamlines, one using a single aspheric (collimating) mirror and one using a plane mirror, provide the higher flux photons required for miniaturization in silicon to produce microscopic mechanical devices including gears, motors, filters, and valves.

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

    PubMed

    Shen, Ya-Ting

    2014-03-01

    In order to investigate plant reacting mechanism with heavy metal stress in organ and tissue level, synchrotron radiation micro X-ray fluorescence (micro-SRXRF) was used to determine element distribution characteristics of K, Ca, Mn, Fe, Cu, Zn, Pb in an Arabidopsis thaliana seedling grown in tailing dam soil taken from a lead-zinc mine exploration area. The results showed a regular distribution characters of K, Ca, Fe, Cu and Zn, while Pb appeared not only in root, but also in a leaf bud which was beyond previously understanding that Pb mainly appeared in plant root. Pb competed with Mn in the distribution of the whole seedling. Pb may cause the increase of oxidative stress in root and leaf bud, and restrict Mn absorption and utilization which explained the phenomenon of seedling death in this tailing damp soil. Speciation of Pb in Arabidopsis thaliana and tailing damp rhizosphere soil were also presented after using PbL3 micro X-ray absorption near edge structure (micro-XANES). By comparison of PbL3 XANES peak shape and peak position between standard samples and rhizosphere soil sample, it was demonstrated that the tailing damp soil was mainly formed by amorphous forms like PbO (64.2%), Pb (OH)2 (28.8%) and Pb3O4 (6.3%) rather than mineral or organic Pb speciations. The low plant bioavailability of Pb demonstrated a further research focusing on Pb absorption and speciation conversion is needed, especially the role of dissolve organic matter in soil which may enhance Pb bioavailability. PMID:25208420

  10. 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.

  11. In situ high-pressure synchrotron X-ray diffraction study of the structural stability in NdVO{sub 4} and LaVO{sub 4}

    SciTech Connect

    Errandonea, D.; Achary, S.N.; Tyagi, A.K.; Bettinelli, M.

    2014-02-01

    Highlights: • NdVO{sub 4} and LaVO{sub 4} were studied under high pressure using synchrotron powder XRD. • Both compounds exhibit first-order phase transitions. • In NdVO{sub 4} the transition involves a symmetry breaking and in LaVO{sub 4} is isomorphic. • The crystal structures of the high-pressure phases are assigned. • Axial and bulk compressibilities are determined. - Abstract: Room-temperature angle-dispersive X-ray diffraction measurements on zircon-type NdVO{sub 4} and monazite-type LaVO{sub 4} were performed in a diamond-anvil cell up to 12 GPa. In NdVO{sub 4}, we found evidence for a non-reversible pressure-induced structural phase transition from zircon to a monazite-type structure at 6.5 GPa. Monazite-type LaVO{sub 4} also exhibits a phase transition but at 8.6 GPa. In this case the transition is reversible and isomorphic. In both compounds the pressure induced transitions involve a large volume collapse. Finally, the equations of state and axial compressibilities for the low-pressure phases are also determined.

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

    PubMed

    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

  13. 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

  14. 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.

  15. 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.

  16. Measuring Cavitation with Synchrotron X-Rays

    NASA Astrophysics Data System (ADS)

    Duke, Daniel; Kastengren, Alan; Powell, Chris; X-Ray Fuel Spray Group, Energy Systems Division Team

    2012-11-01

    Cavitation plays an important role in the formation of sprays from small nozzles such as those found in fuel injection systems. A sharp-edged inlet from the sac into the nozzle of a diesel fuel injector is shown to inititate a strong sheet-like cavitation along the boundary layer of the nozzle throat, which is difficult to measure and can lead to acoustic damage. To investigate this phenomenon, a diagnostic technique capable of mapping the density field of the nozzle through regions of intense cavitation is required. Available visible-light techniques are limited to qualitative observations of the outer extent of cavitation zones. However, brilliant X-rays from a synchrotron source have negligible refraction and are capable of penetrating the full extent of cavitation zones. We present the early results of a novel application of line-of-sight, time-resolved X-ray radiography on a cavitating model nozzle. Experiments were conducted at Sector 7-BM of the Advanced Photon Source. Density and vapor distribution are measured from the quantitative absorption of monochromatic X-rays. The density field can then be tomographically reconstructed from the projections. The density is then validated against a range of compressible and incompressible numerical simulations. This research was performed at the 7-BM beamline of the Advanced Photon Source. We acknowledge the support of the U.S. Department of Energy under Contract No. DE-AC02-06CH11357 and the DOE Vehicle Technologies Program (DOE-EERE).

  17. 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

  18. 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.

  19. New Findings on the Phase Transitions in Li(sub 1-x)CoO(sub 2) and Li(sub 1-x)NiO(sub 2) Cathode Materials During Cycling: In Situ Synchrotron X-Ray Diffraction Studies

    SciTech Connect

    Yang, X. Q.; Sun, X.; McBreen, J.

    1999-10-17

    The authors have utilized synchrotron x-ray radiation to perform ''in situ'' x-ray diffraction studies on Li{sub 1-x}CoO{sub 2} and Li{sub 1-x}NiO{sub 2} cathodes. A C/10 charging rate was used for a Li/Li{sub 1-x}CoO{sub 2} cell. For the Li/Li{sub 1-x}NiO{sub 2} cells, C/13 and C/84 rates were applied. The in situ XRD data were collected during the first charge from 3.5 to 5.2 V. For the Li{sub 1-x}CoO{sub 2} cathode, in the composition range of x = 0 to x = 0.5, a new intermediate phase H2a was observed in addition to the two expected hexagonal phases H1 and H2. In the region very close to x = 0.5, some spectral signatures for the formation of a monoclinic phase M1 were also observed. Further, in the x = 0.8 to x = 1 region, the formation of a CdI{sub 2} type hexagonal phase has been confirmed. However, this new phase is transformed from a CdCl{sub 2} type hexagonal phase, rather than from a monoclinic phase M2 as previously reported in the literature. For the Li{sub 1-x}NiO{sub 2} system, by taking the advantage of the high resolution in 2{theta} angles through the synchrotron based XRD technique, they were able to identify a two-phase coexistence region of hexagonal phase H1 and H2, which has been mistakenly indexed as a single phase region for monoclinic phase M1. Interesting similarities and differences between these two systems are also discussed.

  20. Perovskite at high P-T conditions: An in situ synchrotron X ray diffraction study of NaMgF3 perovskite

    NASA Astrophysics Data System (ADS)

    Zhao, Yusheng; Weidner, Donald J.; Ko, Jiadong; Leinenweber, Kurt; Liu, Xing; Li, Baosheng; Meng, Yue; Pacalo, Rosemary E. G.; Vaughan, Michael T.; Wang, Yanbin

    1994-02-01

    The lattice distortion and structural phase transition of NaMgF3 perovskite (Neighborite) have been studied using synchrotron X ray powder diffraction at high pressure and temperature. Changes in the unit cell dimensions of the perovskite are determined by conventional peak indexing and least squares routines. The stress field within the high-pressure cell assembly is analyzed, and the yield strength of the NaMgF3 perovskite is determined at high P and T. The pressure- and temperature-induced dimensional changes of the NaMgF3 perovskite structure are expressed empirically as a combination of compression/expansion of the (Mg-F) bond length and tilting of the MgF6 octahedral framework. The linear thermal expansions of the NaMgF3 perovskite observed at different pressures show significant anisotropy with alpha(sub a) is greater than alpha(sub c) is greater than alpha(sub b), which reflects the decrease of structural distortion and the development of a phase transition in the perovskite with increasing temperature. The tilting angle of the MgF6 octahedral framework is observed to decrease rapidly toward zero, in a manner expected for a ferroelastic phase transition, as the temperature approaches the transition point T(sub c). The apparent (Mg-F) bond lengths of the MgF6 octahedra experience drastic shrinkage with increasing temperature just prior to the transition. Despite a 12% change in volume due to compression, the experimental results on NaMgF3 perovskite show that the thermal expansivity is independent of pressure, i.e., d(alpha)/dP is approximately equal to 0, and, compatibly, that the compressibility is independent of temperature, i.e., d(beta)/dT is approximately equal to 0. However, the dominant compression mechanism is the compression of the octahedral bond length, whereas the dominant mechanism for thermal expansion is the diminishing of octahedral tilting. The Earth's mantle may be isochemical if the thermal expansion of MgSiO3 perovskite at high pressure

  1. 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

  2. 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.

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

    DOE PAGESBeta

    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

  4. Two kinds of in-plane resistivity anisotropy in Fe1 +δTe (δ =0.09 ) as seen via synchrotron radiation x-ray diffraction and in situ resistivity measurements

    NASA Astrophysics Data System (ADS)

    Nakajima, Taro; Machida, Tadashi; Kariya, Hironori; Morohoshi, Daiki; Yamasaki, Yuichi; Nakao, Hironori; Hirata, Kazuto; Mochiku, Takashi; Takeya, Hiroyuki; Mitsuda, Setsuo; Sakata, Hideaki

    2015-05-01

    We have investigated correlation between structural and electronic anisotropies in a parent compound of Fe-chalcogenide superconductor Fe1 +δTe with δ =0.09 by means of synchrotron x-ray diffraction and in situ in-plane resistivity anisotropy measurements with uniaxial stress applied along a tetragonal a axis. This system is known to exhibit a tetragonal-to-monoclinic structural transition at TS˜60 K. We have confirmed that the in-plane resistivity anisotropy in the low-temperature monoclinic phase is attributed to the asymmetry in volume fractions of the monoclinic domains, as was suggested in a previous study [Jiang et al., Phys. Rev. B 88 115130 (2013), 10.1103/PhysRevB.88.115130]. On the other hand, we found another in-plane resistivity anisotropy above TS. The present x-ray diffraction and resistivity anisotropy measurements have revealed that this anisotropy is not due to an onset of the low-temperature monoclinic phase but to the lattice softening enhanced toward TS. As one of the possibilities, we suggest that the orbital fluctuation contributes to the lattice softening and the resistivity anisotropy above TS.

  5. 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...

  6. Scanning force microscope for in situ nanofocused X-ray diffraction studies

    PubMed Central

    Ren, Zhe; Mastropietro, Francesca; Davydok, Anton; Langlais, Simon; Richard, Marie-Ingrid; Furter, Jean-Jacques; Thomas, Olivier; Dupraz, Maxime; Verdier, Marc; Beutier, Guillaume; Boesecke, Peter; Cornelius, Thomas W.

    2014-01-01

    A compact scanning force microscope has been developed for in situ combination with nanofocused X-ray diffraction techniques at third-generation synchrotron beamlines. Its capabilities are demonstrated on Au nano-islands grown on a sapphire substrate. The new in situ device allows for in situ imaging the sample topography and the crystallinity by recording simultaneously an atomic force microscope (AFM) image and a scanning X-ray diffraction map of the same area. Moreover, a selected Au island can be mechanically deformed using the AFM tip while monitoring the deformation of the atomic lattice by nanofocused X-ray diffraction. This in situ approach gives access to the mechanical behavior of nanomaterials. PMID:25178002

  7. 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.

  8. In situ synchrotron x-ray studies of dense thin-film strontium-doped lanthanum manganite solid oxide fuel cell cathodes.

    SciTech Connect

    Chang, K. C.; Ingram, B.; Kavaipatti, B.; Yildiz, B.; Hennessy, D.; Salvador, P.; Leyarovski, N.; You, H.; Carnegie Mellon Univ.; Massachusetts Inst. of Tech.

    2009-01-01

    Using a model cathode-electrolyte system composed of epitaxial thin-films of La{sub 1-x}Sr{sub x}MnO{sub 3-{delta}} (LSM) on single crystal yttria-stabilized zirconia (YSZ), we investigated changes in the cation concentration profile in the LSM during heating and under applied potential using grazing incidence x-rays. Pulsed laser deposition (PLD) was used to grow epitaxial LSM(011) on YSZ(111). At room temperature, we find that Sr segregates to form Sr enriched nanoparticles and upon heating the sample to 700 C, Sr is slowly reincorporated into the film. We also find different amounts of Sr segregation as the X-ray beam is moved across the sample. The variation in the amount of Sr segregation is greater on the sample that has been subject to 72 hours of applied potential, suggesting that the electrochemistry plays a role in the Sr segregation.

  9. In Situ Lipolysis and Synchrotron Small-Angle X-ray Scattering for the Direct Determination of the Precipitation and Solid-State Form of a Poorly Water-Soluble Drug During Digestion of a Lipid-Based Formulation.

    PubMed

    Khan, Jamal; Hawley, Adrian; Rades, Thomas; Boyd, Ben J

    2016-09-01

    In situ lipolysis and synchrotron small-angle X-ray scattering (SAXS) were used to directly detect and elucidate the solid-state form of precipitated fenofibrate from the digestion of a model lipid-based formulation (LBF). This method was developed in light of recent findings that indicate variability in solid-state form upon the precipitation of some drugs during the digestion of LBFs, addressing the need to establish a real-time technique that enables solid-state analysis during in vitro digestion. In addition, an ex situ method was also used to analyse the pellet phase formed during an in vitro lipolysis experiment at various time points for the presence of crystalline drug. Fenofibrate was shown to precipitate in its thermodynamically stable crystalline form upon digestion of the medium-chain LBF, and an increase in scattering intensity over time corresponded well to an increase in concentration of precipitated fenofibrate quantified from the pellet phase using high-performance liquid chromatography. Crossed polarized light microscopy served as a secondary technique confirming the crystallinity of the precipitated fenofibrate. Future application of in situ lipolysis and SAXS may focus on drugs, and experimental conditions, which are anticipated to produce altered solid-state forms upon the precipitation of drug (i.e., polymorphs, amorphous forms, and salts). PMID:26359590

  10. Structural evolution of Li{sub x}Mn{sub 2}O{sub 4} in lithium-ion battery cells measured in situ using synchrotron X-ray diffraction techniques

    SciTech Connect

    Mukerjee, S.; Thurston, T.R.; Jisrawi, N.M.; Yang, X.Q.; McBreen, J.; Daroux, M.L.; Xing, X.K.

    1998-02-01

    The authors describe synchrotron based X-ray diffraction techniques and issues related to in situ studies of intercalation processes in battery electrodes. They then demonstrate the utility of this technique, through a study of two batches of Li{sub x}Mn{sub 2}O{sub 4} cathode materials. The structural evolution of these spinel materials was monitored in situ during the initial charge of these electrodes in actual battery cells. Significant differences were observed in the two batches, particularly in the intercalation range of x = 0.45 to 0.20. The first-order structural transitions in this region indicated coexistence of two cubic phases in the batch 2 material, whereas the batch 1 material showed suppressed two-phase coexistence. Batch 2 cells also indicated structural evolution in the low-potential region below 3.0 V in contrast to the batch 1 material. Differences in structural evolution between batches of Li{sub x}Mn{sub 2}O{sub 4} could have important ramifications in their cycle life and stability characteristics.

  11. In situ synchrotron x-ray studies of strain and composition evolution during metal-organic chemical vapor deposition of InGaN.

    SciTech Connect

    Richard, M.-I.; Highland, M. J.; Fister, T. T.; Munkholm, A.; Mei, J.; Streiffer, S. K.; Thompson, C.; Fuoss, P. H.; Stephenson, G. B.; Univ. Paul Cezanne; Philips Lumileds Lighting Co.; Northern Illinois Univ.; Faculte des Sciences de St. Jerome

    2010-01-01

    Composition and strain inhomogeneities strongly affect the optoelectronic properties of InGaN but their origin has been unclear. Here we report real-time x-ray reciprocal space mapping that reveals the development of strain and composition distributions during metal-organic chemical vapor deposition of In{sub x}Ga{sub 1-x}N on GaN. Strong, correlated inhomogeneities of the strain state and In fraction x arise during growth in a manner consistent with models for instabilities driven by strain relaxation.

  12. 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

  13. In situ high-pressure synchrotron x-ray diffraction study of CeVO[subscript 4] and TbVO[subscript 4] up to 50 GPa

    SciTech Connect

    Errandonea, D.; Kumar, R.S.; Achary, S.N.; Tyagi, A.K.

    2012-02-07

    Room-temperature angle-dispersive x-ray diffraction measurements on zircon-type TbVO{sub 4} and CeVO{sub 4} were performed in a diamond-anvil cell up to 50 GPa using neon as a pressure-transmitting medium. In TbVO{sub 4}, we found at 6.4 GPa evidence of a nonreversible pressure-induced structural phase transition from zircon to a scheelite-type structure. A second transition to an M-fergusonite-type structure was found at 33.9 GPa, which is reversible. Zircon-type CeVO{sub 4} exhibits two pressure-induced transitions: first, an irreversible transition to a monazite-type structure at 5.6 GPa and, second, at 14.7 GPa, a reversible transition to an orthorhombic structure. No additional phase transitions or evidences of chemical decomposition are found in the experiments. The equations of state and axial compressibility for the different phases are also determined. Finally, the sequence of structural transitions and the compressibilities are discussed in comparison with other orhtovanadates and the influence of nonhydrostaticity commented.

  14. 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.

  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. EVOLUTION OF SYNCHROTRON X-RAYS IN SUPERNOVA REMNANTS

    SciTech Connect

    Nakamura, Ryoko; Bamba, Aya; Dotani, Tadayasu; Ishida, Manabu; Kohri, Kazunori

    2012-02-20

    A systematic study of the synchrotron X-ray emission from supernova remnants (SNRs) has been conducted. We selected a total of 12 SNRs whose synchrotron X-ray spectral parameters are available in the literature with reasonable accuracy and studied how their luminosities change as a function of radius. It is found that the synchrotron X-ray luminosity tends to drop especially when the SNRs become larger than {approx}5 pc, despite large scatter. This may be explained by the change of spectral shape caused by the decrease of the synchrotron roll-off energy. A simple evolutionary model of the X-ray luminosity is proposed and is found to reproduce the observed data approximately, with reasonable model parameters. According to the model, the total energy of accelerated electrons is estimated to be 10{sup 47-48} erg, which is well below the supernova explosion energy. The maximum energies of accelerated electrons and protons are also discussed.

  17. 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.

  18. X-ray fluorescence imaging with synchrotron radiation

    SciTech Connect

    Rivers, M.L.

    1987-01-01

    The micro-distribution of trace elements is of great interest in fields such as geochemistry, biology and material science. The synchrotron x-ray fluorescence microprobe provides a technique to quantitatively measure trace element compositions at individual points and to construct semiquantitative two dimensional maps of trace element compositions. This paper describes an x-ray fluorescence system used at the National Synchrotron Light Source.

  19. Modelling Al-4wt.%Cu as-cast structure using equiaxed morphological parameters deduced from in-situ synchrotron X-ray radiography

    NASA Astrophysics Data System (ADS)

    Ahmadein, M.; Wu, M.; Reinhart, G.; Nguyen-Thi, H.; Ludwig, A.

    2016-03-01

    The as-cast structure of laboratory scale Al-4wt.%Cu was numerically calculated using assumed morphological parameters. Two parameters are identified: The shape factor which correlates the growth velocity of dendrite envelope to that of the tip; and the sphericity of the equiaxed envelope or the circularity of the columnar trunk envelope which is required to calculate the averaged species diffusion flux across the envelope. In the present work, the real-time radiographs of equiaxed solidification experiment carried out on Al-4wt.%Cu at the European Synchrotron Radiation Facility are used to track the development of crystal envelope with time. The growth rate of the equivalent circular envelope was correlated to dendrite tip growth velocity to deduce the shape factor. The sphericity of dendrite envelope is estimated over the time. The average of the deduced morphological parameters is applied to the model to predict the as-cast structure. The results were compared to those obtained by using morphological parameters from literature. The predicted phase quantities, columnar-to- equiaxed transition, and macrosegregation exhibited significant dependence on those parameters. The predicted macrosegregation using the experimentally deduced parameters fits better to the measurements.

  20. 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.

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

    SciTech Connect

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

    2013-06-15

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

  2. Synchrotron X-ray techniques for fluid dynamics

    NASA Astrophysics Data System (ADS)

    Kastengren, Alan; Powell, Christopher F.

    2014-03-01

    X-ray diagnostics have the potential for making quantitative measurements in many flowfields where optical diagnostics are challenging, especially multiphase flows. In the past, many such measurements have been taken with laboratory-scale X-ray sources. This review describes the measurements that are possible with synchrotron X-ray sources, which can provide high-flux, tunable, monochromatic X-ray beams that cannot be created with laboratory sources. The relevant properties of X-rays and their interactions with matter are described. The types and capabilities of various X-ray optics and sources are discussed. Finally, four major X-ray diagnostics are described in detail. X-ray radiography provides quantitative measurements of density in variable-density flows. X-ray phase-contrast imaging is used to visualize multiphase flows with high spatial and temporal resolution. X-ray fluorescence spectroscopy shows significant promise to study mixing in single-phase and multiphase flows. Small-angle X-ray scattering is a powerful technique to examine small-scale particles in flows.

  3. 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

  4. Setup for in situ X-ray diffraction studies of thin film growth by magnetron sputtering

    NASA Astrophysics Data System (ADS)

    Ellmer, K.; Mientus, R.; Weiß, V.; Rossner, H.

    2001-07-01

    A novel method is described for the in situ-investigation of nucleation and growth of thin films during magnetron sputtering. Energy dispersive X-ray diffraction with synchrotron light is used for the structural analysis during film growth. An in situ-magnetron sputtering chamber was constructed and installed at a synchrotron radiation beam line with a bending magnet. The white synchrotron light (1-70 keV) passes the sputtering chamber through Kapton windows and hits one of the substrates on a four-fold sample holder. The diffracted beam, observed under a fixed diffraction angle between 3° and 10°, is energy analyzed by a high purity Ge-detector. The in situ-EDXRD setup is demonstrated for the growth of tin-doped indium oxide (ITO) films prepared by reactive magnetron sputtering from a metallic target.

  5. 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.

  6. In situ x-ray investigation of freestanding nanoscale Cu-Nb multilayers under tensile load.

    SciTech Connect

    Aydiner, C. C.; Misra, A.; Brown, D. W.; Mara, N. A.; Almer, J. D

    2009-01-01

    The yield behavior in a freestanding sputter-deposited Cu/Nb multilayer with 30 nm nominal individual layer thickness has been investigated with in situ synchrotron x-ray diffraction during tensile loading. A pronounced elastic-plastic transition is observed with the fraction of plastically yielded grains increasing gradually with strain. Near synchronous yielding is observed in the Cu and Nb grains. The gradual progression in yield behavior is interpreted in terms of residual stresses, and elastic and plastic anisotropy.

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

    SciTech Connect

    Pereloma, E.; Zhang, L.; Liss, K.-D.; Garbe, U.; Almer, J.; Schambron, T.; Beladi, H.; Timokhina, I.

    2011-06-01

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

  8. Synchrotron x-ray modification of nanoparticle superlattice formation

    NASA Astrophysics Data System (ADS)

    Lu, Chenguang; Akey, Austin J.; Herman, Irving P.

    2012-09-01

    The synchrotron x-ray radiation used to perform small angle x-ray scattering (SAXS) during the formation of three-dimensional nanoparticle superlattices by drop casting nanoparticle solutions affects the structure and the local crystalline order of the resulting films. The domain size decreases due to the real-time SAXS analysis during drying and more macroscopic changes are visible to the eye.

  9. Phase-contrast x-ray tomography using synchrotron radiation

    NASA Astrophysics Data System (ADS)

    Bonse, Ulrich; Beckmann, Felix; Bartscher, Markus; Biermann, Theodor; Busch, Frank; Guennewig, Olaf

    1997-10-01

    The principle and experimental l realization of x-ray phase- contrast in compute assisted microtomography ((mu) CT) at the micrometer resolution level is described. The camera used is a modification of a setup previously developed by us for attenuation-contrast (mu) CT using synchrotron x-rays. Phase detection is accomplished by employing the x-ray interferometer. By using x-ray phase contrast it is possible to image structural details in low-z biological tissues much better than with absorption contrast. The advantage of phase over attenuation contrast is not limited to light element or to low x-ray energies. Examples of applying phase contrast (mu) CT to the structural investigation of rat trigeminal nerve are given.

  10. 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

  11. 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

  12. 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.

  13. Wavelength dispersive analysis with the synchrotron x ray fluorescence microprobe

    NASA Technical Reports Server (NTRS)

    Rivers, M. L.; Thorn, K. S.; Sutton, S. R.; Jones, K. W.; Bajt, S.

    1993-01-01

    A wavelength dispersive spectrometer (WDS) was tested on the synchrotron x ray fluorescence microprobe at Brookhaven National Laboratory. Compared to WDS spectra using an electron microprobe, the synchrotron WDS spectra have much better sensitivity and, due to the absence of bremsstrahlung radiation, lower backgrounds. The WDS spectrometer was successfully used to resolve REE L fluorescence spectra from standard glasses and transition metal K fluorescence spectra from kamacite.

  14. 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

  15. X-Ray Absorption Spectra of Uranium by Synchrotron Radiation

    NASA Astrophysics Data System (ADS)

    Adachi, Hirohiko; Fujima, Kazumi; Taniguchi, Kazuo; Miyake, Chie; Imoto, Shosuke

    1981-08-01

    The X-ray absorption spectra of U, UO2 and UCl4 near the U OIV and OV thresholds have been measured by use of synchrotron radiation. The absorption peaks at about 100 eV and 110 eV are observed for all of these materials. However, the detailed structure of the spectra depend on the chemical state.

  16. 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.

  17. 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

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

    NASA Astrophysics Data System (ADS)

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

    2012-07-01

    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.

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

    DOE PAGESBeta

    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.

  20. 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.

  1. 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.

  2. 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.

  3. 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. PMID:26827327

  4. TOPICAL REVIEW: Medical applications of synchrotron radiation x-rays

    NASA Astrophysics Data System (ADS)

    Lewis, R.

    1997-07-01

    The use of synchrotron radiation is not widespread in the field of medicine and in fact few health-care professionals have even heard of it. It is the purpose of this article to explain what it is and to give some examples of how it can contribute to medical science. X-rays have been used for diagnostic medical imaging for more than 100 years and, whilst new techniques such as computed tomography have been developed, the means of producing x-rays has altered little during that time. Synchrotron radiation sources provide multiple, extremely intense and tuneable beams of photons over a huge range of energies from infrared through to hard x-rays. Their advent has revolutionized many experimental techniques and synchrotron radiation is being applied across many fields from imaging to molecular dynamics. It has spawned several methods for studying live and wet tissue samples, yielding information on both structure and composition on all length scales down to atomic resolution. Such techniques have played a crucial role in the development of molecular biology and the solution of protein structures. The application of synchrotron radiation in the field of radiography is now expanding and it is clear that very substantial improvements in image quality and patient dose can be realized. Following an overview of the production and properties of synchrotron radiation, some of the ways in which this remarkable tool has already been exploited for medical research are reviewed and some potential clinical opportunities highlighted.

  5. Applications of synchrotron x-ray fluorescence to extraterrestrial materials

    SciTech Connect

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

    1986-01-01

    Synchrotron x-ray fluorescence (SXRF) is a valuable technique for trace element analyses of extraterrestrial materials permitting minimum detection limits less than 1 ppM for 20 micrometer spots. SXRF measurements have been performed on iron meteorites and micrometeorites using white synchrotron radiation and an energy dispersive x-ray detector at the National Synchrotron Light Source (X-26C), Brookhaven National Laboratory (NY). Partitioning of Cu between troilite (FeS) and metal in the nine iron meteorites studied suggests sub-solidus re-equilibration in these objects. A technique has been developed for determining self-absorption corrections for filtered, continuum excitation of small specimens, such as stratospheric particles and refractory inclusions in meteorites.

  6. Synchrotron X-ray imaging applied to solar photovoltaic silicon

    NASA Astrophysics Data System (ADS)

    Lafford, T. A.; Villanova, J.; Plassat, N.; Dubois, S.; Camel, D.

    2013-03-01

    Photovoltaic (PV) cell performance is dictated by the material of the cell, its quality and purity, the type, quantity, size and distribution of defects, as well as surface treatments, deposited layers and contacts. A synchrotron offers unique opportunities for a variety of complementary X-ray techniques, given the brilliance, spectrum, energy tunability and potential for (sub-) micron-sized beams. Material properties are revealed within in the bulk and at surfaces and interfaces. X-ray Diffraction Imaging (X-ray Topography), Rocking Curve Imaging and Section Topography reveal defects such as dislocations, inclusions, misorientations and strain in the bulk and at surfaces. Simultaneous measurement of micro-X-Ray Fluorescence (μ-XRF) and micro-X-ray Beam Induced Current (μ-XBIC) gives direct correlation between impurities and PV performance. Together with techniques such as microscopy and Light Beam Induced Current (LBIC) measurements, the correlation between structural properties and photovoltaic performance can be deduced, as well as the relative influence of parameters such as defect type, size, spatial distribution and density (e.g [1]). Measurements may be applied at different stages of solar cell processing in order to follow the evolution of the material and its properties through the manufacturing process. Various grades of silicon are under study, including electronic and metallurgical grades in mono-crystalline, multi-crystalline and mono-like forms. This paper aims to introduce synchrotron imaging to non-specialists, giving example results on selected solar photovoltaic silicon samples.

  7. X-ray multilayer optics for Indus synchrotrons application

    NASA Astrophysics Data System (ADS)

    Nayak, Maheswar; Pradhan, P. C.; Lodha, G. S.

    2015-06-01

    We present the state-of-the-art X-ray multilayer optics fabrication facilities at Indus synchrotrons complex. The facilities are regularly used for fabrication of high quality x-ray multilayer structures. The results on two representative materials combination of Mo/Si and W/B4C are presented. In Mo/Si multilayer system, we have achieved ˜70% of reflectivity (near normal incidence angle) at soft x-ray region. Large area (300mm×50mm) Mo/Si multilayers are also successively fabricated for monochromator application in hard x-ray region. Whereas in W/B4C system, we demonstrate the capability of these facilities to fabricate ultra short period multilayer (periodicity ˜15-20 Å) with large number of layer pairs in the range of 200-400 for transmission polarizer near Fe L-edge and for monochromator application in hard x-ray region. Hard x-ray reflectivity of ˜54% is achieved from W/B4C MLs with periodicity ˜20 Å and number of layer pairs 300.

  8. SYNCHROTRON X-RAY BASED CHARACTERIZATION OF CDZNTE CRYSTALS

    SciTech Connect

    Duff, M

    2006-09-28

    Synthetic CdZnTe or 'CZT' crystals can be used for the room temperature-based detection of {gamma}-radiation. Structural/morphological heterogeneities within CZT, such as twinning, inclusions, and polycrystallinity can affect detector performance. We used a synchrotron-based X-ray technique, specifically extended X-ray absorption fine-structure (EXAFS) spectroscopy, to determine whether there are differences on a local structural level between intact CZT of high and low radiation detector performance. These studies were complemented by data on radiation detector performance and transmission IR imaging. The EXAFS studies revealed no detectable local structural differences between the two types of CZT materials.

  9. 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.

  10. Instrument for x-ray absorption spectroscopy with in situ electrical control characterizations

    SciTech Connect

    Huang, Chun-Chao; Chang, Shu-Jui; Yang, Chao-Yao; Tseng, Yuan-Chieh; Chou, Hsiung

    2013-12-15

    We report a synchrotron-based setup capable of performing x-ray absorption spectroscopy and x-ray magnetic circular dichroism with simultaneous electrical control characterizations. The setup can enable research concerning electrical transport, element- and orbital-selective magnetization with an in situ fashion. It is a unique approach to the real-time change of spin-polarized electronic state of a material/device exhibiting magneto-electric responses. The performance of the setup was tested by probing the spin-polarized states of cobalt and oxygen of Zn{sub 1-x}Co{sub x}O dilute magnetic semiconductor under applied voltages, both at low (∼20 K) and room temperatures, and signal variations upon the change of applied voltage were clearly detected.

  11. Rapid in situ X-ray position stabilization via extremum seeking feedback.

    PubMed

    Zohar, S; Venugopalan, N; Kissick, D; Becker, M; Xu, S; Makarov, O; Stepanov, S; Ogata, C; Sanishvili, R; Fischetti, R F

    2016-03-01

    X-ray beam stability is crucial for acquiring high-quality data at synchrotron beamline facilities. When the X-ray beam and defining apertures are of similar dimensions, small misalignments driven by position instabilities give rise to large intensity fluctuations. This problem is solved using extremum seeking feedback control (ESFC) for in situ vertical beam position stabilization. In this setup, the intensity spatial gradient required for ESFC is determined by phase comparison of intensity oscillations downstream from the sample with pre-existing vertical beam oscillations. This approach compensates for vertical position drift from all sources with position recovery times <6 s and intensity stability through a 5 µm aperture measured at 1.5% FWHM over a period of 8 hours. PMID:26917131

  12. 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.

  13. 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)

  14. 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.

  15. X-ray studies of multilayer semiconductors using synchrotron radiation

    NASA Astrophysics Data System (ADS)

    Huang, Shiwen

    X-ray scattering and absorption techniques utilizing synchrotron radiation have been used to study a variety of multilayer semiconductors. The angular-dependent x-ray scattering at grazing incidence angles (grazing incidence x-ray scattering, GIXS) provides structural information of interfaces in these materials, such as rms interfacial roughness, cross- and lateral-correlation lengths, etc. Long-range order structures in material are probed by large-angle scattering (x-ray diffraction), in which strain and lattice constant as well as crystallinity of the epilayers are measured. Local structural variations in materials including local bond length, coordination number, and local disorder are obtained quantitatively by examining the modulation in the x-ray absorption spectrum some 40 eV above the absorption edge (extended x-ray absorption fine structure, EXAFS). Materials studied in the present work are SiGe/Si heterostructures, MnAs/GaAs ferromagnetic-semiconductor films, solar cell films, ZnSe-based II-VI semiconductor thin films, InGaAs/GaAs and GaAs/AlAs superlattices. Results obtained have shown (i) evidence for strain-induced surface/interface morphology variations in SiGe/Si heterostructures, (ii) template-dependent microstructures in MnAs/GaAs, (iii) changes in interface structures for films of different formations in solar cell films, (iv) differences between samples prepared by different epitaxial growth methods in II-VI semiconductor films, (v) observation of lateral structural ordering in one of the InGaAs/GaAs superlattices, (vi) differences in interfacial microstructures between MBE-grown samples with different interrupts in GaAs/AlAs superlattices. Most of all, x- rays are found to be a very useful nondestructive tool for probing microscopic structures in various multilayer semiconductor materials.

  16. Ray tracing homogenizing mirrors for synchrotron x-ray lithography

    NASA Astrophysics Data System (ADS)

    Homer, Michael; Rosser, Roy J.; Speer, R. J.

    1991-12-01

    Saddle toroid array mirrors (STAMs) are novel grazing-incidence mirrors. They have been proposed as the optical component that most efficiently matches synchrotron orbital radiation (SOR) to the needs of proximity x-ray lithography. However, STAMs have yet to be accepted by the synchrotron lithography community because of the lack of detailed data on their expected performance, due primarily to the difficulty of raytracing such mirrors using existing optical raytrace programs. A raytracing package written especially to study the design and optimization of these unusually shaped mirrors and the very encouraging results obtained with the package to date are described. The optimum STAM designs turn out to be the most effective way of homogeneously illuminating a rectangular proximity x-ray lithography mask, improving on existing scanning mirror systems by at least a factor of four. They have the added advantage of being stationary, which should lead to greater reliability--a quality of considerable value in the production environment these mirrors are intended for, namely the ultra-high vacuum of a synchrotron beamline. Based on the results of the raytracing, a prototype STAM has been constructed, and preparations are being made for an x-ray test of the device.

  17. 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

  18. 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.

  19. 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.

  20. 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.

  1. Data of low-dose phase-based X-ray imaging for in situ soft tissue engineering assessments.

    PubMed

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

    2016-03-01

    This article presents the data of using three phase-based X-ray imaging techniques to characterize biomaterial scaffold and soft tissues in situ, as reported in our study "Low-dose phase-based X-ray imaging techniques for in situ soft tissue engineering assessments" [1]. The examined parameters include the radiation dose, scan time, and image quality, which are all critical to longitudinal in situ live animal assessments. The data presented were obtained from three dimensional imaging of scaffolds in situ cartilage by means of synchrotron-based computed tomography-diffraction enhanced imaging (CT-DEI), analyzer based imaging (CT-ABI), and in-line phase contrast imaging (CT-PCI) at standard and low dose imaging modalities. PMID:26909381

  2. Data of low-dose phase-based X-ray imaging for in situ soft tissue engineering assessments

    PubMed Central

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

    2016-01-01

    This article presents the data of using three phase-based X-ray imaging techniques to characterize biomaterial scaffold and soft tissues in situ, as reported in our study “Low-dose phase-based X-ray imaging techniques for in situ soft tissue engineering assessments” [1]. The examined parameters include the radiation dose, scan time, and image quality, which are all critical to longitudinal in situ live animal assessments. The data presented were obtained from three dimensional imaging of scaffolds in situ cartilage by means of synchrotron-based computed tomography-diffraction enhanced imaging (CT-DEI), analyzer based imaging (CT-ABI), and in-line phase contrast imaging (CT-PCI) at standard and low dose imaging modalities. PMID:26909381

  3. Miniature pulsed magnet system for synchrotron x-ray measurements

    SciTech Connect

    Linden, Peter J. E. M. van der; Mathon, Olivier; Strohm, Cornelius; Sikora, Marcin

    2008-07-15

    We have developed a versatile experimental apparatus for synchrotron x-ray measurements in pulsed high magnetic fields. The apparatus consists of a double cryostat incorporating a liquid nitrogen bath to cool the miniature pulsed coil and an independent helium flow cryostat allowing sample temperatures from 4 up to 250 K. The high duty cycle miniature pulsed coils can generate up to 38 T. During experiments at 30 T a repetition rate of 6 pulses/min was routinely reached. Using a 4 kJ power supply, the pulse duration was between 500 {mu}s and 1 ms. The setup was used for nuclear forward scattering measurements on {sup 57}Fe up to 25 T on the ESRF beamline ID18. In another experiment, x-ray magnetic circular dichroism was measured up to 30 T on the ESRF energy dispersive beamline ID24.

  4. An in situ XAFS study--the formation mechanism of gold nanoparticles from X-ray-irradiated ionic liquid.

    PubMed

    Ma, Jingyuan; Zou, Yang; Jiang, Zheng; Huang, Wei; Li, Jiong; Wu, Guozhong; Huang, Yuying; Xu, Hongjie

    2013-07-28

    An in situ X-ray absorption fine structure (XAFS) experiment has been performed to observe the evolution of gold nanoparticles in the ionic liquid [BMIM][AuCl4], by hard X-ray irradiation. The ionic liquid acts as both a reducing agent and a protective ligand. A synchrotron-based X-ray plays the role of the irradiation source, which induces the reduction of the gold species, as well as being a real time probe for XAFS measurements. From the extended X-ray absorption fine structure (EXAFS) fitting results for a series of spectra of gold L3-edge, it can be seen clearly that there is a single Au-Cl bond breaking process before the formation of Au-Au bonds, which is different from previous reports on the formation of Au nanoparticles by several chemical methods. PMID:23765109

  5. Contrasting of biological samples for X-ray synchrotron microtomography.

    PubMed

    Efimova, O I; Khlebnikov, A S; Senin, R A; Voronin, P A; Anokhin, K V

    2013-08-01

    The method of contrasting with iodine ions was developed to obtain high-resolution 3D images of large biological specimens using a synchrotron X-ray microtomography unit. It was shown that the samples (late mouse embryos) treated with 50% Lugol solution with addition of 25% ethanol for 48 h followed by a 48-h washout in phosphate buffered saline had maximum contrast and lowest compression artifacts. Processing of samples by this protocol allowed detecting zones of active proliferation. Incubation of brain samples for 120 h in 7.6% meglumine/sodium diatrizoate without washout ensured the best contrast during myelin identification. PMID:24143358

  6. 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.

  7. 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 PAGESBeta

    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

  8. An apparatus for in situ x-ray scattering measurements during polymer injection molding

    NASA Astrophysics Data System (ADS)

    Rendon, Stanley; Fang, Jun; Burghardt, Wesley R.; Bubeck, Robert A.

    2009-04-01

    We report a novel instrument for synchrotron-based in situ x-ray scattering measurements during injection molding processing. It allows direct, real-time monitoring of molecular-scale structural evolution in polymer materials undergoing a complex processing operation. The instrument is based on a laboratory-scale injection molding machine, and employs customized mold tools designed to allow x-ray access during mold filling and subsequent solidification, while providing sufficient robustness to withstand high injection pressures. The use of high energy, high flux synchrotron radiation, and a fast detector allows sufficiently rapid data acquisition to resolve time-dependent orientation dynamics in this transient process. Simultaneous monitoring of temperature and pressure signals allows transient scattering data to be referenced to various stages of the injection molding cycle. Representative data on a commercial liquid crystalline polymer, Vectra® B950, are presented to demonstrate the features of this apparatus; however, it may find application in a wide range of polymeric materials such as nanocomposites, semicrystalline polymers and fiber-reinforced thermoplastics.

  9. In situ high-resolution X-ray photoelectron spectroscopy - Fundamental insights in surface reactions

    NASA Astrophysics Data System (ADS)

    Papp, Christian; Steinrück, Hans-Peter

    2013-11-01

    Since the advent of third generation synchrotron light sources optimized for providing soft X-rays up to 2 keV, X-ray photoelectron spectroscopy (XPS) has been developed to be an outstanding tool to study surface properties and surface reactions at an unprecedented level. The high resolution allows identifying various surface species, and for small molecules even the vibrational fine structure can be resolved in the XP spectra. The high photon flux reduces the required measuring time per spectrum to the domain of a few seconds or even less, which enables to follow surface processes in situ. Moreover, it also provides access to very small coverages down to below 0.1% of a monolayer, enabling the investigation of minority species or processes at defect sites. The photon energy can be adjusted according to the requirement of a particular experiment, i.e., to maximize or minimize the surface sensitivity or the photoionization cross-section of the substrate or the adsorbate. For a few instruments worldwide, a next step forward was taken by combining in situ high-resolution spectrometers with supersonic molecular beams. These beams allow to control and vary the kinetic and internal energies of the incident molecules and provide a local pressure of up to ~10-5 mbar, which can be switched on and off in a controllable way, thus offering a well-defined time structure to study adsorption or reaction processes.

  10. 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.

  11. 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

  12. 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.

  13. 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.

  14. 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

  15. 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. PMID:26057665

  16. 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

  17. 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.

  18. Anomalous X-ray diffraction with soft X-ray synchrotron radiation.

    PubMed

    Carpentier, P; Berthet-Colominas, C; Capitan, M; Chesne, M L; Fanchon, E; Lequien, S; Stuhrmann, H; Thiaudière, D; Vicat, J; Zielinski, P; Kahn, R

    2000-07-01

    Anomalous diffraction with soft X-ray synchrotron radiation opens new possibilities in protein crystallography and materials science. Low-Z elements like silicon, phosphorus, sulfur and chlorine become accessible as new labels in structural studies. Some of the heavy elements like uranium exhibit an unusually strong dispersion at their M(V) absorption edge (lambdaMV = 3.497 A, E(MV) = 3545 eV) and so does thorium. Two different test experiments are reported here showing the feasibility of anomalous X-ray diffraction at long wavelengths with a protein containing uranium and with a salt containing chlorine atoms. With 110 electrons the anomalous scattering amplitude of uranium exceeds by a factor of 4 the resonance scattering of other strong anomalous scatterers like that of the lanthanides at their L(III) edge. The resulting exceptional phasing power of uranium is most attractive in protein crystallography using the multi-wavelength anomalous diffraction (MAD) method. The anomalous dispersion of an uranium derivative of asparaginyl-tRNA synthetase (hexagonal unit cell; a = 123.4 A, c = 124.4 A) has been measured for the first time at 4 wavelengths near the M(V) edge using the beamline ID1 of ESRF (Grenoble, France). The present set up allowed to measure only 30% of the possible reflections at a resolution of 4 A, mainly because of the low sensitivity of the CCD detector. In the second experiment, the dispersion of the intensity of 5 X-ray diffraction peaks from pentakismethylammonium undecachlorodibismuthate (PMACB, orthorhombic unit cell; a = 13.003 A, b = 14.038 A, c = 15.450 A) has been measured at 30 wavelengths near the K absorption edge of chlorine (lambdaK = 4.397 A, EK= 2819.6 eV). All reflections within the resolution range from 6.4 A to 3.4 A expected in the 20 degree scan were observed. The chemical state varies between different chlorine atoms of PMACB, and so does the dispersion of different Bragg peaks near the K-edge of chlorine. The results reflect

  19. 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

  20. Experimental novaculite deformation: interpretation of in-situ X-ray diffraction data using EPSC models

    NASA Astrophysics Data System (ADS)

    Thomas, S.; Willenweber, A.; Cline, C. J.; Sas, M.; Pape, D.; Erickson, B.; Bright, T.; Burnley, P. C.

    2012-12-01

    The deformation behavior of fine-grained polycrystalline quartz (novaculite) was studied experimentally using in-situ X-ray diffraction and theoretically by elastic plastic self consistent modeling (EPSC). Previous experimental work has shown that different subpopulations of crystals experience different stress levels during high pressure deformation and reflection stresses may lead to poor approximations of macroscopic sample stresses, since in-situ diffraction data originates from grain scale phenomena rather than macroscopic sample properties [1]. In this context EPSC models have been utilized to interpret diffraction data, i.e., to independently derive the macroscopic sample load and to directly compare results with diffraction data. In our study a series of novaculite samples with 645 ± 50 wt ppm H2O was deformed in different regimes of disclocation-creep, at 2.5 GPa and up to ~1000 °C, in the D-DIA apparatus at the NSLS X17B2 beamline. In-situ synchrotron X-ray diffraction was used to monitor the sample stress state during controlled deformation and to observe the strain behavior of the individual lattice reflections of novaculite. Lattice strains were calculated from measured lattice spacings. The macroscopic sample strain was determined by sample radiographs. The strains provide information about how individual grains or grain populations react to stress depending on their orientation within the aggregate. We observe a reproducible elastic slope across the series of experiments and a temperature dependence of individual lattice strains and yield strength. In addition, EPSC models were calculated to theoretically determine macroscopic sample stresses and to match measured rheological sample properties with simulations. Depending on deformation conditions measured elastic lattice strains could be matched by activating basal and/or prism and/or pyramidal slip systems of the crystal structure. Here, we present EPSC models, compare macroscopic stresses

  1. 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

  2. Combined in Situ X-ray absorption and diffuse reflectance infraredspectroscopy: An attractive tool for catalytic investigations

    SciTech Connect

    Marinkovic, N.S.; Ehrlich, S.; Wang, Q.; Barrio, L.; Khalid, S.; et.al.

    2010-11-24

    Catalysis investigations are often followed in a range of spectroscopic techniques. While diffuse reflectance infrared Fourier transform spectroscopy (DRIFTS) can be done on a bench-top instrument, X-ray absorption spectroscopy (XAS) techniques, such as extended X-ray absorption fine structure (EXAFS) and X-ray absorption near-edge structure (XANES) require synchrotron light. In order to ensure the same conditions during in situ catalysis for each method, a combined XAS/DRIFTS has been developed at beamline X18A at the National Synchrotron Light Source, Brookhaven National Laboratory. A rapid-scan FTIR spectrometer capable of both mid- and far-infrared measurements is equipped with an arm to redirect the IR beam outside the spectrometer. An in situ reaction chamber, equipped with glassy carbon windows for X-ray light and a KBr window for IR light passage is installed firmly on the arm. The reaction cell can be heated to 600 C and allows passage of gases through the catalyst so that both XAS and DRIFTS techniques can be done simultaneously in controlled environment conditions. Together with a fast-moving monochromator for quick-EXAFS and mass-spectrometric residual gas analysis, this new tool is a powerful method for testing catalytic reactions in real time.

  3. Synchrotron x-ray reticulography: principles and applications

    NASA Astrophysics Data System (ADS)

    Lang, A. R.; Makepeace, A. P. W.

    1999-05-01

    Synchrotron x-ray reticulography is a versatile new technique for mapping misorientations in single crystals. It is nearly as simple to perform as conventional single-crystal Laue topography, yet it yields quantitative data on misorientations that would demand long sequences of images if the double-crystal technique were applied. In reticulography a fine-scale x-ray absorbing mesh is placed between a Laue-diffracting crystal specimen and the topograph-recording photographic plate. The mesh splits the diffracted beam into an array of individually identifiable microbeams. Direction differences between microbeams, which give the orientation differences between the crystal elements reflecting them, are measured from their relative shifts within the array when mesh-to-plate distance is changed. The angular sensitivity of reticulography depends upon the angular size of the x-ray source. At Station 7.6 at the SRS, Daresbury, 80 m from the tangent point, and with source size FWHM (full width half maximum) = 0.23 mm vertically, the incidence angular range in the vertical plane is only 0.6 arcsec, and misorientations down to this magnitude are measurable. Applications of reticulography to three quite different problems are described, illustrating the method's versatility. The problems are: (1) measuring surface lattice-plane tilts due to an array of dislocations in a large synthetic diamond; (2) determining the sense of the Burgers vector of a giant screw dislocation in SiC; and (3) measuring lattice curvature above an energetic ion implant in a natural diamond.

  4. 3D synchrotron x-ray microtomography of paint samples

    NASA Astrophysics Data System (ADS)

    Ferreira, Ester S. B.; Boon, Jaap J.; van der Horst, Jerre; Scherrer, Nadim C.; Marone, Federica; Stampanoni, Marco

    2009-07-01

    Synchrotron based X-ray microtomography is a novel way to examine paint samples. The three dimensional distribution of pigment particles, binding media and their deterioration products as well as other features such as voids, are made visible in their original context through a computing environment without the need of physical sectioning. This avoids manipulation related artefacts. Experiments on paint chips (approximately 500 micron wide) were done on the TOMCAT beam line (TOmographic Microscopy and Coherent rAdiology experimenTs) at the Paul Scherrer Institute in Villigen, CH, using an x-ray energy of up to 40 keV. The x-ray absorption images are obtained at a resolution of 350 nm. The 3D dataset was analysed using the commercial 3D imaging software Avizo 5.1. Through this process, virtual sections of the paint sample can be obtained in any orientation. One of the topics currently under research are the ground layers of paintings by Cuno Amiet (1868- 1961), one of the most important Swiss painters of classical modernism, whose early work is currently the focus of research at the Swiss Institute for Art Research (SIK-ISEA). This technique gives access to information such as sample surface morphology, porosity, particle size distribution and even particle identification. In the case of calcium carbonate grounds for example, features like microfossils present in natural chalks, can be reconstructed and their species identified, thus potentially providing information towards the mineral origin. One further elegant feature of this technique is that a target section can be selected within the 3D data set, before exposing it to obtain chemical data. Virtual sections can then be compared with cross sections of the same samples made in the traditional way.

  5. 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.

  6. 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.

  7. 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.

  8. 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).

  9. 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. PMID:26625184

  10. 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

  11. 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.

  12. 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

  13. Synchrotron X-ray microtomographic study of tablet swelling.

    PubMed

    Laity, P R; Cameron, R E

    2010-06-01

    Tablet swelling behaviour was investigated by following the movements of embedded glass microsphere tracers, using X-ray microtomography (XmicroT) with intense illumination from a synchrotron. Specimens were prepared using combinations of hydroxypropyl-methyl-cellulose (HPMC) and microcrystalline cellulose (MCC) or pre-gelatinised starch (PGS), three materials commonly used as excipients for compacted tablets. The results revealed significant differences in swelling behaviour due to excipient type and compaction conditions. In particular, a sudden change was observed from gel-forming behaviour of formulations containing PGS or high HPMC content, to more rapid expansion and disintegration for formulations above 70% MCC. Although some radial expansion was observable with the higher PGS formulations and during later stages of swelling, axial expansion (i.e. the reverse of the compaction process) appeared to dominate in most cases. This was most pronounced for the 10/90 HPMC/MCC specimens, which rapidly increased in thickness, while the diameter remained almost unchanged. The expansion appeared to be initiated by hydration and may be due to the relaxation of residual compaction stress. This occurred within 'expansion zones', which initially appeared as thin bands close to the compacted (upper and lower) faces, but gradually advanced towards the centre and spread around the sides of the tablets. These zones exhibited lower X-ray absorbance, probably because they contained significant amounts of bubbles, which were formed by air released from the swelling excipients. Although, in most cases, these bubbles were too small to be resolved (<60 microm), larger bubbles (diameter up to 1mm) were clearly evident in the rapidly swelling 10/90 HPMC/MCC specimens. It is suggested that the presence of these bubbles may affect subsequent water ingress, by increasing the tortuosity and occluding part of the gel, which may affect the apparent diffusion kinetics (i.e. Fickian or Case II

  14. Geoscience Applications of Synchrotron X-ray Computed Microtomography

    NASA Astrophysics Data System (ADS)

    Rivers, M. L.

    2009-05-01

    Computed microtomography is the extension to micron spatial resolution of the CAT scanning technique developed for medical imaging. Synchrotron sources are ideal for the method, since they provide a monochromatic, parallel beam with high intensity. High energy storage rings such as the Advanced Photon Source at Argonne National Laboratory produce x-rays with high energy, high brilliance, and high coherence. All of these factors combine to produce an extremely powerful imaging tool for earth science research. Techniques that have been developed include: - Absorption and phase contrast computed tomography with spatial resolution approaching one micron - Differential contrast computed tomography, imaging above and below the absorption edge of a particular element - High-pressure tomography, imaging inside a pressure cell at pressures above 10GPa - High speed radiography, with 100 microsecond temporal resolution - Fluorescence tomography, imaging the 3-D distribution of elements present at ppm concentrations. - Radiographic strain measurements during deformation at high confining pressure, combined with precise x- ray diffraction measurements to determine stress. These techniques have been applied to important problems in earth and environmental sciences, including: - The 3-D distribution of aqueous and organic liquids in porous media, with applications in contaminated groundwater and petroleum recovery. - The kinetics of bubble formation in magma chambers, which control explosive volcanism. - Accurate crystal size distributions in volcanic systems, important for understanding the evolution of magma chambers. - The equation-of-state of amorphous materials at high pressure using both direct measurements of volume as a function of pressure and also by measuring the change x-ray absorption coefficient as a function of pressure. - The formation of frost flowers on Arctic sea-ice, which is important in controlling the atmospheric chemistry of mercury. - The distribution of

  15. Microdiffraction Study of Polycrystalline Copper during UniaxialTension Deformation using a Synchrotron X-ray Source

    SciTech Connect

    Joo, H.D.; Kim, J.S.; Bark, C.W.; Kim, J.Y.; Koo, Y.M.; Tamura, N.

    2004-10-04

    In-situ measurement of local orientation and strain has been carried out for a copper polycrystals under a uniaxial loading using a synchrotron x-ray microdiffraction method at the Advanced Light Source.The heterogeneities of deformation-induced microstructure within single grains were observed. There were differences in the selection of simultaneously acting slip systems among neighboring volume elements within a grain.

  16. 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

  17. 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

  18. Reactive sputter magnetron reactor for preparation of thin films and simultaneous in situ structural study by X-ray diffraction.

    PubMed

    Bürgi, J; Neuenschwander, R; Kellermann, G; García Molleja, J; Craievich, A F; Feugeas, J

    2013-01-01

    The purpose of the designed reactor is (i) to obtain polycrystalline and∕or amorphous thin films by controlled deposition induced by a reactive sputtering magnetron and (ii) to perform a parallel in situ structural study of the deposited thin films by X-ray diffraction, in real time, during the whole growth process. The designed reactor allows for the control and precise variation of the relevant processing parameters, namely, magnetron target-to-sample distance, dc magnetron voltage, and nature of the gas mixture, gas pressure and temperature of the substrate. On the other hand, the chamber can be used in different X-ray diffraction scanning modes, namely, θ-2θ scanning, fixed α-2θ scanning, and also low angle techniques such as grazing incidence small angle X-ray scattering and X-ray reflectivity. The chamber was mounted on a standard four-circle diffractometer located in a synchrotron beam line and first used for a preliminary X-ray diffraction analysis of AlN thin films during their growth on the surface of a (100) silicon wafer. PMID:23387690

  19. Reactive sputter magnetron reactor for preparation of thin films and simultaneous in situ structural study by X-ray diffraction

    SciTech Connect

    Buergi, J.; Molleja, J. Garcia; Feugeas, J.; Neuenschwander, R.; Kellermann, G.; Craievich, A. F.

    2013-01-15

    The purpose of the designed reactor is (i) to obtain polycrystalline and/or amorphous thin films by controlled deposition induced by a reactive sputtering magnetron and (ii) to perform a parallel in situ structural study of the deposited thin films by X-ray diffraction, in real time, during the whole growth process. The designed reactor allows for the control and precise variation of the relevant processing parameters, namely, magnetron target-to-sample distance, dc magnetron voltage, and nature of the gas mixture, gas pressure and temperature of the substrate. On the other hand, the chamber can be used in different X-ray diffraction scanning modes, namely, {theta}-2{theta} scanning, fixed {alpha}-2{theta} scanning, and also low angle techniques such as grazing incidence small angle X-ray scattering and X-ray reflectivity. The chamber was mounted on a standard four-circle diffractometer located in a synchrotron beam line and first used for a preliminary X-ray diffraction analysis of AlN thin films during their growth on the surface of a (100) silicon wafer.

  20. System for in situ studies of atmospheric corrosion of metal films using soft x-ray spectroscopy and quartz crystal microbalance.

    PubMed

    Forsberg, J; Duda, L-C; Olsson, A; Schmitt, T; Andersson, J; Nordgren, J; Hedberg, J; Leygraf, C; Aastrup, T; Wallinder, D; Guo, J-H

    2007-08-01

    We present a versatile chamber ("atmospheric corrosion cell") for soft x-ray absorption/emission spectroscopy of metal surfaces in a corrosive atmosphere allowing novel in situ electronic structure studies. Synchrotron x rays passing through a thin window separating the corrosion cell interior from a beamline vacuum chamber probe a metal film deposited on a quartz crystal microbalance (QCM) or on the inside of the window. We present some initial results on chloride induced corrosion of iron surfaces in humidified synthetic air. By simultaneous recording of QCM signal and soft x-ray emission from the corroding sample, correlation between mass changes and variations in spectral features is facilitated. PMID:17764316

  1. System for in situ studies of atmospheric corrosion of metal films using soft x-ray spectroscopy and quartz crystal microbalance

    NASA Astrophysics Data System (ADS)

    Forsberg, J.; Duda, L.-C.; Olsson, A.; Schmitt, T.; Andersson, J.; Nordgren, J.; Hedberg, J.; Leygraf, C.; Aastrup, T.; Wallinder, D.; Guo, J.-H.

    2007-08-01

    We present a versatile chamber ("atmospheric corrosion cell") for soft x-ray absorption/emission spectroscopy of metal surfaces in a corrosive atmosphere allowing novel in situ electronic structure studies. Synchrotron x rays passing through a thin window separating the corrosion cell interior from a beamline vacuum chamber probe a metal film deposited on a quartz crystal microbalance (QCM) or on the inside of the window. We present some initial results on chloride induced corrosion of iron surfaces in humidified synthetic air. By simultaneous recording of QCM signal and soft x-ray emission from the corroding sample, correlation between mass changes and variations in spectral features is facilitated.

  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. In situ/operando soft x-ray spectroscopy characterization of ion solvation and catalysis

    NASA Astrophysics Data System (ADS)

    Liu, Yi-Sheng; Guo, Jinghua

    Many important systems especially in energy-related regime are based on the complexity of material architecture, chemistry and interactions among constituents within. To understand and thus ultimately control the varying applications calls for in-situ/operando characterization tools. We will present the recent development of the in-situ/operando soft X-ray spectroscopic in the studies of catalytic and alkali ion solvation under bias condition, and reveal how to overcome the challenge that soft X-rays cannot easily peek into the high-pressure catalytic cells or liquid electrochemical cells. Also the different feasible detection approaches can provide surface and bulk sensitivity experimentally from those in-situ cells. The unique design of in-situ/operando soft X-ray spectroscopy instrumentation and fabrication principle with examples in Ca, Na, Mg based solutions at ambient pressure/temperature and high temperature (~250°C) gas catalysis will be shown.

  5. Lead adsorption at the calcite-water interface: Synchrotron x-ray standing wave and x-ray reflectivity studies

    SciTech Connect

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

    1997-01-01

    By combining synchrotron X-ray standing wave (XSW) measurements with synchrotron X-ray reflectivity measurements, we have determined: (1) the precise three-dimensional location within the calcite unit cell of submonolayer Pb ions adsorbed at the calcite (104) surface from dilute aqueous solutions, and (2) the precise one-dimensional location of these unit cells relative to the calcite surface. Our XSW measurements, using three separate calcite Bragg reflections for triangulation, show that most adsorbed Pb ions occupy Ca sites in the calcite lattice with an ordered coverage of 0.05 equivalent monolayers, while the remaining Pb ions are disordered with a coverage of 0.03 equivalent monolayers. Our X-ray reflectivity measurements show that the ordered Ph ions occur primarily (>70%) in the surface atomic layer of calcite. Atomic force microscopy (AFM) was used to characterize the topography of the calcite (104) surface under conditions similar to the X-ray experiments. The quantitative morphological information obtained by AFM was used to develop realistic models of the calcite surface. The calculated X-ray reflectivities for these model surfaces were compared with the measured X-ray reflectivities. The new combined X-ray method that we have developed can be used to determine the atomic-scale structure of other metals adsorbed at mineral-water interfaces. Such high-resolution structural determinations are essential before detailed conceptual and theoretical models can be further developed to understand and predict the behavior of dissolved metals in mineral-water systems. 60 refs., 8 figs., 3 tabs.

  6. Development of a Compact System for In-situ X-ray Scattering Studies of Organic Thin Film Deposition

    SciTech Connect

    Headrick, R.L.; Malliaras, G.G.; Mayer, A.C.; Deyhim, A.K.; Hunt, A.C.

    2004-05-12

    We have developed a compact vacuum deposition chamber for in-situ x-ray scattering studies of organic thin film growth. The system is based on a small cylindrical chamber that can be mounted on a standard four-circle diffractometer. Incident and scattered x-rays enter and exit the chamber through a curved Be foil window that covers 200 degrees, and is sealed to the body of the chamber. The sample is mounted on a support tube with heating and cooling from liquid nitrogen temperature to >100 deg. C. Integral to the sample stage is a multi-wire feedthrough to facilitate in-situ electrical transport characterization of organic semiconductor thin films. This is one of the novel capabilities of the system. In addition, the sample stage is mounted on a rotary vacuum feedthrough, which is mechanically coupled to the 'phi' stage of the diffractometer. An effusion cell, shutter, and quartz oscillator thickness monitor are also incorporated into the system, which is pumped by a small turbomolecular pump. The system thus configured is capable of access to full reciprocal space, within the limits of the Be window. Results of initial experiments performed at the 48-pole wiggler beamline A2, at the Cornell High Energy Synchrotron Source show that in-situ x-ray scattering is sensitive to the early stages of nucleation and growth of organic semiconductor thin films.

  7. Electrochemical cell for in-situ x-ray characterization

    SciTech Connect

    Doughty, D.H.; Ingersoll, D.; Rodriguez, M.A.

    1998-08-04

    An electrochemical cell suitable for in-situ XRD analysis is presented. Qualitative information such as phase formation and phase stability can be easily monitored using the in-situ cell design. Quantitative information such as lattice parameters and kinetic behavior is also straightforward. Analysis of the LiMn&sub2;O&sub4; spinel using this cell design shows that the lattice undergoes two major structural shrinkages at approx. 4.0 V and approx. 4.07 V during charging. These shrinkages correlate well with the two electrochemical waves observed and indicate the likelihood of two separate redox processes which charging and discharging.

  8. Fast synchrotron X-ray tomography study of the rod packing structures

    SciTech Connect

    Zhang Xiaodan; Xia Chengjie; Sun Haohua; Wang Yujie

    2013-06-18

    We present a fast synchrotron X-ray tomography study of the packing structures of rods under tapping. Utilizing the high flux of the X-rays generated from the third-generation synchrotron source, we can complete a tomography scan within several seconds, after which the three-dimensional (3D) packing structure can be obtained for the subsequent structural analysis. Due to the high-energy nature of the X-ray beam, special image processing steps including image phase-retrieval has been implemented. Overall, this study suggests the possibility of acquiring statistically significant static packing structures within a reasonable time scale using high-intensity X-ray sources.

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

    SciTech Connect

    Jisrawi, N.M.; Wiesmann, H.; Ruckman, M.W.; Thurston, T.R.; Reisfeld, G.; Ocko, B.M.; Strongin, M.

    1997-08-01

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

  10. 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.

  11. 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.

  12. 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.

  13. 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.

  14. 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.

  15. 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.

  16. Melting curve of NaCl determined using synchrotron x-ray radiography

    NASA Astrophysics Data System (ADS)

    Chen, J.; Yu, T.; Long, H.; Wang, L.; Garai, J.

    2009-12-01

    NaCl has been widely used as a pressure calibrant in in-situ high pressure synchrotron x-ray study. The applicable pressure and temperature range of this calibrant is from ambient condition up to B1-B2 transition in pressure and to melting in temperature. Melting data of NaCl at high pressures are still very limited. We have conducted comparative experiments to study melting of NaCl using energy dispersive x-ray diffraction and radiographic imaging at high pressure up to 8.8GPa. The experiments were carried out using the cubic-type multi-anvil pressure (SAM85) at the X17B2 beamline of the National Synchrotron Light Source (NSLS). In the x-ray diffraction experiments, melting is inferred when disappearance of diffraction peak of NaCl from a mixture of NaCl+BN (to reduce possible grain growth) is observed. In the x-ray radiography experiment, a WC sphere is place in the top portion of pure NaCl sample; melting is inferred when the WC sphere start to drop in the sample. The experimental result indicates that the melting temperatures determined from the two types of observations may differ by 60°C at 5 GPa. Due to unavoidable grain growth near melting, x-ray diffraction signals may disappear from the point solid state detector even though the melting is not achieved. Therefore the radiography method may reflect more accurate measurement of melting temperature. Melting curve of NaCl was measured up to 1.8 GPa by Clark et al (1), and between 2 and 4 GPa by Pistorius (2). The new melting data are consistent with the previous results. All the experimental are in good agreement with theoretical prediction using Simon fusion equation (2) and the relation between melting temperature and Debye temperature (3). References: (1) Clark, Jr. Effect of Pressure on the Melting Points of Eight Alkali Halides, Journal of Chemical Physics 31 (6) 1526-1531 (1959). (2) Kraut and Kennedy, New Melting Law at High Pressures, Physical Review 151 (2) 668-675 (1966) (3) J. Garai, and J. Chen

  17. Structural characterization of sol-gel derived oxide nanostuctures using synchrotron x-ray techniques

    NASA Astrophysics Data System (ADS)

    Sun, Tao

    Ceramic oxides possess extraordinarily rich functionalities. With the advent of nanofabrication techniques, it is now possible to grow nanostructured oxides with precise control of composition, morphology, and microstructure, which has re-vitalized the research in the field of traditional ceramics. The unexpected behavior and enhanced properties of oxide nanostructures have been extensively reported. However, knowledge about the underlying mechanisms as well as structural implications is still quite limited. Therefore, it is imperative to develop and employ sophisticated characterization tools for unraveling the structure-property relationships for oxide nanostructures. The present thesis work aims at addressing the critical issues associated with fabrication, and more importantly, structural characterization of functional oxide nanostructures. The dissertation starts with introducing the strategy for synthesizing phase-pure and highly controlled oxide nanostructures using sol-gel deposition and an innovative approach called "soft" electron beam lithography. Some specific oxides are chosen for the present study, such as BiFeO3, CoFe2O4, and SnO2, because of their scientific and technological significance. Subsequent to fabrication of tailored oxide nanostructures, advanced synchrotron x-ray scattering techniques have been applied for structural characterization. The nucleation and growth behavior of BiFeO3 thin film was investigated using in situ grazing-incidence small-angle x-ray scattering (GISAXS) technique. The results reveal that the kinetics for early-stage nuclei growth are governed by the oriented-attachment model. Moreover, the porous structures of undoped and Pd-doped semiconducting SnOx thin films were quantitatively characterized using GISAXS. By correlating the structural parameters with H2 sensitivity of SnOx films, it is found out that the microstructure of doped film is favorable for gas sensing, but it is not the major reason for the overall

  18. Cell for simultaneous synchrotron radiation X-ray and electrochemical corrosion measurements on cultural heritage metals and other materials.

    PubMed

    Dowsett, Mark G; Adriaens, Annemie

    2006-05-15

    We describe the construction of an electrochemical cell of the Bragg type suitable for in situ synchrotron X-ray measurements on rough, heterogeneous metals such as cultural heritage alloys and simulants with corroding or passivated surfaces. The cell features a working electrode, which may be moved under remote control from a position close to an X-ray window to full immersion in the electrolyte. A pocket of electrolyte in contact with the bulk can be maintained on the working electrode surface at all times. Its thickness (typically 100-200 microm) can be controlled by adjusting the working electrode position and, independently, altering the conformation of the X-ray window with hydrostatic pressure. Alternatively, the electrode may be lowered into the bulk of the electrolyte. Early results from the cell showing a time-resolved study of the reduction of nantokite to cuprite in sodium sesquicarbonate, accompanied by corrosion potential measurements obtained in parallel, are presented here. PMID:16689538

  19. Real-time microstructure of shocked LiF crystals: Use of synchrotron x-rays

    NASA Astrophysics Data System (ADS)

    Turneaure, Stefan J.; Gupta, Y. M.; Zimmerman, K.; Perkins, K.; Yoo, C. S.; Shen, G.

    2009-03-01

    We describe the use of a third generation synchrotron facility to obtain in situ, real-time, x-ray diffraction measurements in plate impact experiments. Subnanosecond duration x-ray pulses were utilized to record diffraction data from pure and magnesium-doped LiF single crystals shocked along the [111] and [100] orientations. The peak stresses were 3.0 GPa for the [111] oriented LiF and between 3.0 and 5.0 GPa for the [100] oriented LiF. For these stresses, shock compression along [111] results in elastic deformation and shock compression along [100] results in elastic-plastic deformation. Because of the quality of the synchrotron x-ray pulses, both shifting and broadening of the diffraction data were obtained simultaneously. As expected, shifts for elastic compression and elastic-plastic compression in shocked LiF were consistent with uniaxial and isotropic lattice compression, respectively. More importantly, diffraction patterns from crystals shocked along [100] exhibited substantial broadening due to elastic-plastic deformation. The broadening indicates that the shocked LiF(100) crystals developed substructure with a characteristic size for coherently diffracting domains (0.1-10 μm) and a distribution of (100) microlattice-plane rotations (˜1° wide). In contrast to the LiF(100) results, broadening of the diffraction pattern did not occur for elastically deformed LiF(111). Another important finding was that the amount of lattice disorder for shocked LiF(100) depends on the loading history; the broadening was larger for the magnesium-doped LiF(100) (large elastic precursor) than for ultrapure LiF(100) (small elastic precursor) shocked to the same peak stress. The data are simulated by calculating the diffraction pattern from LiF(100) with a model microstructure consisting of coherently diffracting domains. The lattice orientation and longitudinal strain is assumed uniform within domains, but they vary from domain to domain with Gaussian distributions

  20. 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. PMID:26917133

  1. 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.

  2. 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.

  3. 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.

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

    PubMed

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

    2015-01-01

    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(-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 Bi2O3-SiO2 glass frit obtained during heating with ramp rates 5 °C s(-1) and 100 °C s(-1), revealing numerous phase changes. PMID:25638092

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

    NASA Astrophysics Data System (ADS)

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

    2015-01-01

    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-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 Bi2O3-SiO2 glass frit obtained during heating with ramp rates 5 °C s-1 and 100 °C s-1, revealing numerous phase changes.

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

    NASA Astrophysics Data System (ADS)

    Serrano, A.; Gálvez, F.; Rodríguez de la Fuente, O.; García, M. A.

    2013-03-01

    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.

  7. 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.

  8. 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).

  9. 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.

  10. 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.

  11. 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.

  12. 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.

  13. Comparison of Synchrotron X-Ray Fluorescence Mapping and Micro-XANES to Bulk X-Ray Absorption Spectra in Metal-Contaminated Sediments

    SciTech Connect

    O'Day, P; Carroll, S A; Bajt, S

    2003-01-16

    Synchrotron X-ray absorption spectroscopy (XAS) is one of the few techniques that can supply molecular-scale information for a variety of elements at concentrations relevant to natural systems in non-vacuum conditions. Bulk XAS analysis supplies the dominant chemical bonding mode(s) for a specific element. In complex materials such as natural soils and sediments, however, the dominant mode may not necessarily be the most reactive because changes in speciation at surfaces may results in changes in reactivity. Our previous work at Naval Air Station (NAS) Alameda (CA) focused on in situ metal chemistry in surface and deep sediments, and the impact of metal mobility by sediment oxidation. Estuary sediments at the Alameda Naval Station Air in California have elevated metal concentrations that increase with increasing depth. The metal concentrations in these sediments are: Cd (10-350 ppm), Cr (200-1000 ppm), Cu (100-230 ppm), Pb (200-1200 ppm) and Zn (250-600 ppm). We have extensively characterized these sediments using bulk XAS and other non-synchrotron supporting methods [ 1]. In this experiment, we collected fluorescence element maps using synchrotron X-ray microprobe of unreacted and seawater-oxidized sediment samples from Alameda NAS to determine the spatial distribution and correlation of lead, zinc, and iron. We then compared micro-XANES spectra for lead and zinc collected with the X-ray microprobe to previously collected bulk XANES spectra. The results from our bulk XAS characterization of the sediments showed both oxide and sulfide components for the trace metals. However, the bulk XAS data were not able to identify the composition of the oxide component (i.e. carbonate or hydroxide), nor could absorbed species or solid solutions be definitively identified. Our objective in using micro-XANES and fluorescence element maps was to attempt a more precise identification of metal speciation in or on individual particles.

  14. Setup for in situ x-ray diffraction study of swift heavy ion irradiated materials

    SciTech Connect

    Kulriya, P. K.; Singh, F.; Tripathi, A.; Ahuja, R.; Kothari, A.; Dutt, R. N.; Mishra, Y. K.; Kumar, Amit; Avasthi, D. K.

    2007-11-15

    An in situ x-ray diffraction (XRD) setup is designed and installed in the materials science beam line of the Pelletron accelerator at the Inter-University Accelerator Centre for in situ studies of phase change in swift heavy ion irradiated materials. A high vacuum chamber with suitable windows for incident and diffracted X-rays is integrated with the goniometer and the beamline. Indigenously made liquid nitrogen (LN{sub 2}) temperature sample cooling unit is installed. The snapshots of growth of particles with fluence of 90 MeV Ni ions were recorded using in situ XRD experiment, illustrating the potential of this in situ facility. A thin film of C{sub 60} was used to test the sample cooling unit. It shows that the phase of the C{sub 60} film transforms from a cubic lattice (at room temperature) to a fcc lattice at around T=255 K.

  15. Probing electrode/electrolyte interfaces in situ by X-ray spectroscopies: old methods, new tricks.

    PubMed

    Wu, Cheng Hao; Weatherup, Robert S; Salmeron, Miquel B

    2015-11-11

    Electrode/electrolyte interfaces play a vital role in various electrochemical systems, but in situ characterization of such buried interfaces remains a major challenge. Several efforts to develop techniques or to modify existing techniques to study such interfaces are showing great promise to overcome this challenge. Successful examples include electrochemical scanning tunneling microscopy (EC-STM), surface-sensitive vibrational spectroscopies, environmental transmission electron microscopy (E-TEM), and surface X-ray scattering. Other techniques such as X-ray core-level spectroscopies are element-specific and chemical-state-specific, and are being widely applied in materials science research. Herein we showcase four types of newly developed strategies to probe electrode/electrolyte interfaces in situ with X-ray core-level spectroscopies. These include the standing wave approach, the meniscus approach, and two liquid cell approaches based on X-ray photoelectron spectroscopy and soft X-ray absorption spectroscopy. These examples demonstrate that with proper modifications, many ultra-high-vacuum based techniques can be adapted to study buried electrode/electrolyte interfaces and provide interface-sensitive, element- and chemical-state-specific information, such as solute distribution, hydrogen-bonding network, and molecular reorientation. At present, each method has its own specific limitations, but all of them enable in situ and operando characterization of electrode/electrolyte interfaces that can provide important insights into a variety of electrochemical systems. PMID:26514115

  16. In situ energy-dispersive x-ray diffraction system for time-resolved thin-film growth studies

    NASA Astrophysics Data System (ADS)

    Ellmer, K.; Mientus, R.; Weiß, V.; Rossner, H.

    2003-03-01

    Energy-dispersive x-ray diffraction (EDXRD) with synchrotron light can be used for in situ-structural analysis during polycrystalline thin-film growth, due to its fast data collection and the fixed diffraction angle. An in situ deposition and analysis set-up for the investigation of nucleation and growth of thin films during magnetron sputtering was constructed and installed at the synchrotron radiation source Hamburger Synchrotronstrahlungs Labor (Hamburg). The polychromatic synchrotron beam passes the sputtering chamber through Kapton windows and hits the substrate with the growing film. The diffracted beam, observed under a fixed diffraction angle of between 1° and 10° was energy-analysed by a high-purity germanium detector. The measurement time for a single XRD spectrum can be as short as 10 s for a beam line at a bending magnet, which allows a time-resolved monitoring of film growth. The performance of the in situ EDXRD set-up is demonstrated for the growth of zinc oxide and tin-doped indium oxide films prepared by reactive magnetron sputtering from ceramic and metallic targets. From the position and the width of the diffraction lines the internal mechanical strain and the grain size of the growing films can be derived. The prospects for thin-film growth investigations using such an instrument are assessed.

  17. 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.

  18. 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.

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

    PubMed

    Peterson, Vanessa K; Papadakis, Christine M

    2015-03-01

    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

  20. 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

  1. Hydrothermal Transformation of the Calcium Aluminum Oxide Hydrates CaAl2O4 . 10H2O and Ca2Al2O. 8H2O to Ca3Al2(OH)12 Investigated by In Situ Synchrotron X-ray Powder Diffraction

    SciTech Connect

    Jensen,T.; Christensen, A.; Hanson, J.

    2005-01-01

    The hydrothermal transformation of calcium aluminate hydrates were investigated by in situ synchrotron X-ray powder diffraction in the temperature range 25 to 170 C. This technique allowed the study of the detailed reaction mechanism and identification of intermediate phases. The material CaAl{sub 2}O{sub 4}{center_dot}10H{sub 2}O converted to Ca{sub 3}Al{sub 2}(OH){sub 12} and amorphous aluminum hydroxide. Ca{sub 2}Al{sub 2}O{sub 5}{center_dot}8H{sub 2}O transformed via the intermediate phase Ca{sub 4}Al{sub 2}O{sub 7}{center_dot}13H{sub 2}O to Ca{sub 3}Al{sub 2}(OH){sub 12} and gibbsite, Al(OH){sub 3}. The phase Ca{sub 4}Al{sub 2}O{sub 7}{center_dot}19H{sub 2}O reacted via the same intermediate phase to Ca{sub 3}Al{sub 2}(OH){sub 12} and mainly amorphous aluminum hydroxide. The powder pattern of the intermediate phase is reported.

  2. 3D-printed photo-spectroelectrochemical devices for in situ and in operando X-ray absorption spectroscopy investigation.

    PubMed

    Achilli, Elisabetta; Minguzzi, Alessandro; Visibile, Alberto; Locatelli, Cristina; Vertova, Alberto; Naldoni, Alberto; Rondinini, Sandra; Auricchio, Ferdinando; Marconi, Stefania; Fracchia, Martina; Ghigna, Paolo

    2016-03-01

    Three-dimensional printed multi-purpose electrochemical devices for X-ray absorption spectroscopy are presented in this paper. The aim of this work is to show how three-dimensional printing can be a strategy for the creation of electrochemical cells for in situ and in operando experiments by means of synchrotron radiation. As a case study, the description of two cells which have been employed in experiments on photoanodes for photoelectrochemical water splitting are presented. The main advantages of these electrochemical devices are associated with their compactness and with the precision of the three-dimensional printing systems which allows details to be obtained that would otherwise be difficult. Thanks to these systems it was possible to combine synchrotron-based methods with complementary techniques in order to study the mechanism of the photoelectrocatalytic process. PMID:26917152

  3. Recent advances in X-ray nanolithography using synchrotron radiation at Super-ACO

    NASA Astrophysics Data System (ADS)

    Rousseaux, F.; Chen, Y.; Haghiri-Gosnet, A. M.; Launois, H.

    1995-02-01

    This paper describes our recent advances in high resolution synchrotron radiation lithography. Fabrication processes of high resolution X-ray masks based on our current {SiC}/{W} technology have been optimized to be compatible with a commercial Karl Süss stepper. As a result, well defined 50 nm wide isolated lines and small gratings of period down to 100 nm have been fabricated and tested in proximity X-ray lithography with the stepper. Replication tests were done with a minimum gap setting down to 5 μm. Results show that proximity X-ray lithography using synchrotron radiation is a viable technology for printing 50 nm linewidth features.

  4. X-ray phase-contrast tomography with a compact laser-driven synchrotron source

    PubMed Central

    Eggl, Elena; Schleede, Simone; Bech, Martin; Achterhold, Klaus; Loewen, Roderick; Ruth, Ronald D.; Pfeiffer, Franz

    2015-01-01

    Between X-ray tubes and large-scale synchrotron sources, a large gap in performance exists with respect to the monochromaticity and brilliance of the X-ray beam. However, due to their size and cost, large-scale synchrotrons are not available for more routine applications in small and medium-sized academic or industrial laboratories. This gap could be closed by laser-driven compact synchrotron light sources (CLS), which use an infrared (IR) laser cavity in combination with a small electron storage ring. Hard X-rays are produced through the process of inverse Compton scattering upon the intersection of the electron bunch with the focused laser beam. The produced X-ray beam is intrinsically monochromatic and highly collimated. This makes a CLS well-suited for applications of more advanced––and more challenging––X-ray imaging approaches, such as X-ray multimodal tomography. Here we present, to our knowledge, the first results of a first successful demonstration experiment in which a monochromatic X-ray beam from a CLS was used for multimodal, i.e., phase-, dark-field, and attenuation-contrast, X-ray tomography. We show results from a fluid phantom with different liquids and a biomedical application example in the form of a multimodal CT scan of a small animal (mouse, ex vivo). The results highlight particularly that quantitative multimodal CT has become feasible with laser-driven CLS, and that the results outperform more conventional approaches. PMID:25902493

  5. X-ray phase-contrast tomography with a compact laser-driven synchrotron source.

    PubMed

    Eggl, Elena; Schleede, Simone; Bech, Martin; Achterhold, Klaus; Loewen, Roderick; Ruth, Ronald D; Pfeiffer, Franz

    2015-05-01

    Between X-ray tubes and large-scale synchrotron sources, a large gap in performance exists with respect to the monochromaticity and brilliance of the X-ray beam. However, due to their size and cost, large-scale synchrotrons are not available for more routine applications in small and medium-sized academic or industrial laboratories. This gap could be closed by laser-driven compact synchrotron light sources (CLS), which use an infrared (IR) laser cavity in combination with a small electron storage ring. Hard X-rays are produced through the process of inverse Compton scattering upon the intersection of the electron bunch with the focused laser beam. The produced X-ray beam is intrinsically monochromatic and highly collimated. This makes a CLS well-suited for applications of more advanced--and more challenging--X-ray imaging approaches, such as X-ray multimodal tomography. Here we present, to our knowledge, the first results of a first successful demonstration experiment in which a monochromatic X-ray beam from a CLS was used for multimodal, i.e., phase-, dark-field, and attenuation-contrast, X-ray tomography. We show results from a fluid phantom with different liquids and a biomedical application example in the form of a multimodal CT scan of a small animal (mouse, ex vivo). The results highlight particularly that quantitative multimodal CT has become feasible with laser-driven CLS, and that the results outperform more conventional approaches. PMID:25902493

  6. 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.

  7. 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. PMID:25204894

  8. 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.

  9. 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.

  10. 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.

  11. 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.

  12. Interactions between synchrotron radiation X-ray and biological tissues — theoretical and clinical significance

    PubMed Central

    Chen, Heyu; He, Xin; Sheng, Caibin; Ma, Yingxin; Nie, Hui; Xia, Weiliang; Ying, Weihai

    2011-01-01

    Synchrotron radiation (SR) X-ray has great potential for its applications in both diagnosis and treatment of diseases, due to its characteristic properties including coherence, collimation, monochromaticity, and exceptional brightness. Great advances have been made regarding potential medical applications of SR X-ray in recent years, particularly with the development of the third generation of SR light sources. However, multiple studies have also suggested damaging effects of SR X-ray on biological samples ranging from protein crystals to cells and biological tissues. It has become increasingly important to conduct comprehensive studies on two closely related topics regarding SR X-ray in medical applications: The safety issues regarding the medical applications of SR X-ray and the fundamental mechanisms underlying the interactions between SR X-ray and biological tissues. In this article, we attempted to provide an overview of the literatures regarding these two increasingly significant topics. We also proposed our hypothesis that there are significant differences between the biological tissue-damaging mechanisms of SR X-ray and those of normal X-ray, due to the characteristic properties of SR X-ray such as high dose rate. Future studies are warranted to test this hypothesis, which may profoundly improve our understanding regarding the fundamental mechanisms underlying the interactions between light and matter. These studies would also constitute an essential basis for establishing the safety standard for the medical applications of SR X-ray. PMID:22162780

  13. In situ x-ray, electrochemical, and modeling investigation of the oxygen electrode activation.

    SciTech Connect

    Yildiz, B.; Chang, K.-C.; Meyers, D.; Carter, J. D.; You, H.

    2006-01-01

    Oxygen electrodes of solid oxide electrochemical cells have been shown to improve under strong cathodic and anodic polarization. Our study investigates the mechanism causing such improvement, using in situ x-ray and electrochemical characterization and electrochemical impedance modeling of the oxygen electrodes. Several porous and dense thin-film model electrodes of La{sub 0.8}Sr{sub 0.2}MnO{sub 3} (LSM) and La{sub 0.8}Sr{sub 0.2}MnO{sub 3} (LCM) on single crystal yttria-stabilized zirconia (YSZ) electrolytes have been analyzed in situ at the Advanced Photon Source (APS) using x-ray reflectivity and x-ray absorption near edge spectroscopy (XANES) at the Mn K-edge and La LII-edge. In situ x-ray reflectivity analysis show that no clear correlation between the polarization of the electrode and any further changes in the roughness of the LSM/YSZ interface exist. XANES measurements illustrate that the cathodic or anodic dc polarization at high temperature induces no detectable changes in Mn chemical state either in the bulk or at the surface of the LCM and LSM electrodes on YSZ, while the La chemical state changes reversibly at the electrode surface. This field-induced chemical change of La at the surface of electrodes is assumed to be a cause of the electrochemical activation through enhanced surface exchange of oxygen on the doped lanthanum manganite electrodes.

  14. In situ observation of cellular organelles with a contact x-ray microscope

    NASA Astrophysics Data System (ADS)

    Kado, M.; Kishimoto, M.; Tamotsu, S.; Yasuda, K.; Shinohara, K.

    2013-10-01

    A contact x-ray microscope coupled with a highly intense laser plasma soft x-ray source has been developed and in situ observations of cellular organelles have been conducted. The soft x-rays were generated by irradiating a high power laser pulse onto a thin-foiled gold target and about 1.3×1015 photons/sr were obtained, which allowed the inner structures of live wet biological cells to be imaged. Single shot flash imaging is a key technique to image cellular organelles of live biological cells avoiding degradation of the spatial resolution of the images resulting from motion blur and radiation damage. The use of a fluorescence microscope to identify cellular organelles in conjunction with the soft x-ray microscope has allowed several cellular organelles to be identified precisely in the soft x-ray images. Combining the fluorescence microscope with the soft x-ray microscope will be very useful and will establish the technique as a powerful tool to analyze living function of biological cells.

  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. 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.

  17. In-situ small-angle X-ray scattering study of the precipitation behavior in a Fe-25 at.%Co-9 at.%Mo alloy

    SciTech Connect

    Zickler, Gerald A. Eidenberger, Elisabeth; Leitner, Harald; Stergar, Erich; Clemens, Helmut; Staron, Peter; Lippmann, Thomas; Schreyer, Andreas

    2008-12-15

    Fe-Co-Mo alloys show extraordinary mechanical properties which make them potential candidates for various high-performance applications. In the present study, for the first time, the precipitation behavior in a Fe-25 at.%Co-9 at.%Mo alloy was studied by small-angle X-ray scattering using high-energy synchrotron radiation. The specimens were isothermally aged in an in-situ furnace. The small-angle X-ray scattering patterns showed scaling behavior and were evaluated by employing a model function from the literature. This approach provides information about the characteristic length scale and the volume fraction of the precipitates in the alloy.

  18. 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.

  19. Using Synchrotron X-Ray Nano-CT to Characterize SOFC Electrode Microstructures in Three-Dimensions at Operating Temperature

    SciTech Connect

    Shearing, P.R.; Bradley, R.S.; Gelb, J.; Lee, S.N.; Atkinson, A.; Withers, P.J.; Brandon, N.P.

    2012-01-20

    In recent years, developments in tomography tools have provided unprecedented insight into the microstructure of electrodes for solid oxide fuel cells, enabling researchers to establish direct links between electrode microstructure and electrochemical performance. Here we present results of high resolution, synchrotron X-ray nano computed tomography experiments, which have enabled microstructural characterisation of a mixed ionic electronic conducting lanthanum strontium cobalt iron oxide (LSCF) cathode with sub-50nm resolution at operating temperature. Using the uniquely non-destructive nano-CT platform, it is possible to characterise microstructural evolution processes associated with heating and operation in-situ.

  20. 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

  1. 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.

  2. 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.

  3. In situ X-ray snapshot analysis of transient molecular adsorption in a crystalline channel

    NASA Astrophysics Data System (ADS)

    Kubota, Ryou; Tashiro, Shohei; Shiro, Motoo; Shionoya, Mitsuhiko

    2014-10-01

    Molecular adsorption is a fundamental phenomenon in porous materials and is usually characterized by the efficiency and selectivity of molecular separations and reactions. However, for functional porous materials, analysis of the dynamic behaviour of molecular adsorbents is a major challenge. Here, we use in situ single-crystal X-ray diffraction to analyse multi-step molecular adsorption in a crystalline nanochannel of a metal-macrocycle framework. The pore surface of the metal-macrocycle framework crystal contains five different enantiomerically paired binding pockets, to which the adsorption of a (1R)-1-(3-chlorophenyl)ethanol solution was monitored with time. The resulting X-ray snapshot analyses suggest that the guest adsorption process takes a two-step pathway before equilibrium, in which the guest molecule is temporarily trapped by a neighbouring binding site. This demonstrates the potential for using X-ray analyses to visualize a transient state during a non-covalent self-assembly process.

  4. 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.

  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. 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.

  7. 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.

  8. 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.

  9. 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.

  10. 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.

  11. Three-dimensional characterization of electrodeposited lithium microstructures using synchrotron X-ray phase contrast imaging.

    PubMed

    Eastwood, David S; Bayley, Paul M; Chang, Hee Jung; Taiwo, Oluwadamilola O; Vila-Comamala, Joan; Brett, Daniel J L; Rau, Christoph; Withers, Philip J; Shearing, Paul R; Grey, Clare P; Lee, Peter D

    2015-01-01

    The electrodeposition of metallic lithium is a major cause of failure in lithium batteries. The 3D microstructure of electrodeposited lithium 'moss' in liquid electrolytes has been characterised at sub-micron resolution for the first time. Using synchrotron X-ray phase contrast imaging we distinguish mossy metallic lithium microstructures from high surface area lithium salt formations by their contrasting X-ray attenuation. PMID:24898258

  12. Fluctuation x-ray scattering from biological particles in frozen solution by using synchrotron radiation.

    PubMed Central

    Kam, Z; Koch, M H; Bordas, J

    1981-01-01

    Determination of the structure of biological particles, randomly oriented in solution, from spatial correlation analysis of fluctuations in x-ray scattering has recently been proposed. The feasibility of scattering fluctuation measurements was evaluated by using an x-ray synchrotron radiation camera to obtain the spatial correlation for a solution of tobacco mosaic virus along a line. The experimental system, analysis of data, and requirements for the determination of structures in solution are discussed using this example. PMID:6943555

  13. Synchrotron x-ray photoemission study of soft x-ray processed ultrathin glycine-water ice films

    SciTech Connect

    Tzvetkov, George; Netzer, Falko P.

    2011-05-28

    Ultrathin glycine-water ice films have been prepared in ultrahigh vacuum by condensation of H{sub 2}O and glycine at 90 K on single crystalline alumina surfaces and processed by soft x-ray (610 eV) exposure for up to 60 min. The physicochemical changes in the films were monitored using synchrotron x-ray photoemission spectroscopy. Two films with different amounts of H{sub 2}O have been considered in order to evaluate the influence of the water ice content on the radiation-induced effects. The analysis of C1s, N1s, and O1s spectral regions together with the changes in the valence band spectra indicates that amino acid degradation occurs fast mainly via decarboxylation and deamination of pristine molecules. Enrichment of the x-ray exposed surfaces with fragments with carbon atoms without strong electronegative substituents (C-C and C-H) is documented as well. In the thinner glycine-water ice film (six layers of glycine + six layers of water) the 3D ice suffers strongly from the x-rays and is largely removed from the sample. The rate of photodecomposition of glycine in this film is about 30% higher than for glycine in the thicker film (6 layers of glycine + 60 layers of water). The photoemission results suggest that the destruction of amino acid molecules is caused by the direct interaction with the radiation and that no chemical attack of glycine by the species released by water radiolysis is detected.

  14. Synchrotron x-ray scattering studies of rapidly evolving nanoscale interfacial systems

    NASA Astrophysics Data System (ADS)

    Dai, Yeling

    In light of the development of third-generation synchrotron sources which deliver extremely bright radiation beam over a board energy band, tremendous progress has been made in x-ray science and the diverse range of disciplines that can be studied with x-ray. The special properties of synchrotron-produced x-ray such as coherence, polarization, etc., combined with different extreme experimental conditions, can meet almost any requirement of the research for material characterization, imaging, molecular dynamics, surface/interface physics and so on. In this work we will demonstrate how outstanding properties of synchrotron x-ray can be use to study the structural and dynamic properties of rapidly evolving nano-scale interfacial systems. A large part of this thesis is devoted to the investigation of the surface capillary fluctuations of laterally confined supported polystyrene films using x-ray photon correlation spectroscopy (XPCS), a young coherent scattering technique that can probes the dynamics of matter. The structural evolution of interfacial/surface system, such as the self-assembled nanoparticle film at water-air interface and the nano-imprinted polystyrene pattern, can be studied by different time-resolved x-ray small angle scattering techniques in grazing incidence geometry (GISAXS,GIXOS,GID), as well as the conventional specular reflectivity (XR) measurement. Particularly in the case of the liquid surface research, special efforts have been made to improve a recently developed diffuse scattering technique Grazing incidence off-specular x-ray scattering (GIXOS) for probing the structure at liquid interface with much better temporal resolution compared with that of XR. In this work We will present all the experimental results together with conclusive data analysis from the studies of these evolving systems with x-ray scattering techniques. In comparison to the reciprocal space studies with x-ray scattering tools, part of this thesis is devoted to the

  15. 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.

  16. 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.

  17. Non-destructive trace element microanalysis of as-received cometary nucleus samples using synchrotron x ray fluorescence

    NASA Technical Reports Server (NTRS)

    Sutton, S. R.

    1989-01-01

    The Synchrotron X ray Fluorescence (SXRF) microprobe at the National Synchrotron Light Source (NSLS), Brookhaven National Laboratory, will be an excellent instrument for non-destructive trace element analyses of cometary nucleus samples. Trace element analyses of as-received cometary nucleus material will also be possible with this technique. Bulk analysis of relatively volatile elements will be important in establishing comet formation conditions. However, as demonstrated for meteorites, microanalyses of individual phases in their petrographic context are crucial in defining the histories of particular components in unequilibrated specimens. Perhaps most informative in comparing cometary material with meteorites will be the halogens and trace metals. In-situ, high spatial resolution microanalyses will be essential in establishing host phases for these elements and identifying terrestrial (collection/processing) overprints. The present SXRF microprobe is a simple, yet powerful, instrument in which specimens are excited with filtered, continuum synchrotron radiation from a bending magnet on a 2.5 GeV electron storage ring. A refrigerated cell will be constructed to permit analyses at low temperatures. The cell will consist essentially of an air tight housing with a cold stage. Kapton windows will be used to allow the incident synchrotron beam to enter the cell and fluorescent x rays to exit it. The cell will be either under vacuum or continuous purge by ultrapure helium during analyses. Several other improvements of the NSLS microprobe will be made prior to the cometary nucleus sample return mission that will greatly enhance the sensitivity of the technique.

  18. 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.

  19. Report of the second workshop on synchrotron radiation sources for x-ray lithography

    SciTech Connect

    Barton, M.Q.; Craft, B.; Williams, G.P.

    1986-01-01

    The reported workshop is part of an effort to implement a US-based x-ray lithography program. Presentations include designs for three storage rings (one superconducting and two conventional) and an overview of a complete lithography program. The background of the effort described, the need for synchrotron radiation, and the international competition in the area are discussed briefly. The technical feasibility of x-ray lithography is discussed, and synchrotron performance specifications and construction options are given, as well as a near-term plan. It is recommended that a prototype synchrotron source be built as soon as possible, and that a research and development plan on critical technologies which could improve cost effectiveness of the synchrotron source be established. It is further recommended that a small number of second generation prototype synchrotrons be distributed to IC manufacturing centers to expedite commercialization. (LEW)

  20. Microbeam, timing and signal-resolved studies of nuclear materials with synchrotron X-ray sources

    SciTech Connect

    Ice, Gene E; Specht, Eliot D

    2012-01-01

    The development of ultra-brilliant synchrotron X-ray sources enables characterization methods that are particularly important for nuclear materials. Here we discuss emerging synchrotron methods with unprecedented signal-to-noise, spatial and time resolution. Microprobe methods are discussed that extend virtually any X-ray characterization measurement to ultra-small sample volumes. This ability is critical to resolve heterogeneities in nuclear materials and for studies on volumes with vastly lower activity than are needed for traditional X-ray characterization. Specific methods discussed include microdiffraction for the characterization of local crystal structure and micro-spectroscopy techniques that allow for characterization of elemental distributions with sensitivity for daughter products, oxidation states and diffusion through buffer layers. Opportunities are also discussed that exploit the high brilliance and pulsed nature of synchrotron radiation to reduce backgrounds from sample radiation and to study materials dynamics.

  1. 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.

  2. 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.

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

    SciTech Connect

    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.

  4. X-ray microtomography with monochromatic synchrotron radiation

    SciTech Connect

    D'Amico, K. L.; Deckman, H. W.; Dunsmuir, J. H.; Flannery, B. P.; Roberge, W. G.

    1989-07-01

    We review results obtained with the Exxon Microtomography apparatus. The technique is based on tomographic methods widely used in medicine and nondestructive evaluation. When used with a tunable x-ray source, it is a powerful diagnostic and research tool for a wide variety of materials problems. It is capable of producing maps of the interior structure and chemical composition of samples approximately 0.5--1.0 mm in size, with spatial resolution in the map of the density variations approaching 10.0 /mu/m.

  5. 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.

  6. 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. PMID:25025342

  7. In Situ Soft X-ray Spectroscopy Characterization of Interfacial Phenomena in Energy Materials and Devices

    NASA Astrophysics Data System (ADS)

    Guo, Jinghua; Liu, Yi-Sheng; Kapilashrami, Mukes; Glans, Per-Anders; Bora, Debajeet; Braun, Artur; Velasco Vélez, Juan Jesús; Salmeron, Miquel; ALS/LBNL Team; EMPA, MSD/LBNL Collaboration

    2015-03-01

    Advanced energy technology arises from the understanding in basic science, thus rest in large on in-situ/operando characterization tools for observing the physical and chemical interfacial processes, which has been largely limited in a framework of thermodynamic and kinetic concepts or atomic and nanoscale. In many important energy systems such as energy conversion, energy storage and catalysis, advanced materials and functionality in devices are based on the complexity of material architecture, chemistry and interactions among constituents within. To understand and thus ultimately control the energy conversion and energy storage applications calls for in-situ/operando characterization tools. Soft X-ray spectroscopy offers a number of very unique features. We will present our development of the in-situ/operando soft X-ray spectroscopic tools of catalytic and electrochemical reactions in recent years, and reveal how to overcome the challenge that soft X-rays cannot easily peek into the high-pressure catalytic cells or liquid electrochemical cells. In this presentation a number of examples are given, including the nanocatalysts and the recent experiment performed for studying the hole generation in a specifically designed photoelectrochemical cell under operando conditions. The ALS is supported by the the U.S. Department of Energy.

  8. Use of Synchrotron X-ray Fluorescence to Measure Trace Metal Distribution in the Brain

    NASA Astrophysics Data System (ADS)

    Linkous, D.; Flinn, J. M.; Lanzirotti, A.; Frederickson, C.; Jones, B. F.; Bertsch, P. M.

    2002-12-01

    X26A, National Synchrotron Light Source, was used to quantitatively evaluate the spatial distribution of trace metals, such as Zn and Cu, in brain tissue. X-ray microprobe techniques offer distinct advantages over other analytical methods by allowing analyses to be done in-situ with little or no chemical pretreatment and low detection limits (about 1 ppm). In the context of neuroscience, SXRF can provide non-destructive measurements of specific metal concentrations and distribution within nerve (brain) tissue. Neuronal tissue from organisms having undergone different normal or experimental conditions may be compared, with analytical capacities not limited by binding states of the metal (i.e., vesicular or enzymatic), as is the case with staining techniques.. Whole regions of tissue may be scanned for detectable trace metals at spatial resolutions of 10um or less using focused monochromatic x-ray beams. Here special attention has been given to zinc because it is the most common trace metal in the brain, and levels have been increasing in the environment. In this investigation, zinc concentrations present within the hilus of a rat hippocampus, and to a lesser extent in the cortex, have been shown to increase following long-term ingestion of zinc-enhanced drinking water that was associated with deficits in spatial memory. Concomitantly, copper concentrations in the internal capsule were comparatively lower. Other first order transition metals, Cr, V, Mn, and Co were not detected. In contrast, elevated levels of Zn, Cu, and Fe have been seen in amyloid plaques associated with Alzheimer's disease.

  9. 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. PMID:26761779

  10. 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.

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

    PubMed Central

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

    2013-01-01

    We present a multicrystal Johann-type hard x-ray spectrometer (∼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°–74°) 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 4π sr. The typical resolving power is in the order of \\documentclass[12pt]{minimal}\\begin{document}$\\frac{E}{\\Delta E} \\sim 10\\,000$\\end{document}EΔE∼10000. 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. PMID:23742527

  12. 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.

  13. 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.

  14. 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

  15. Soft X-Ray Spectrometer Using 100-Pixel STJ Detectors for Synchrotron Radiation

    SciTech Connect

    Shiki, Shigetomo; Zen, Nobuyuki; Ukibe, Masahiro; Ohkubo, Masataka

    2009-12-16

    Fluorescent X-ray absorption fine structure (XAFS) is an important tool for material analysis, especially for the measurement of chemical states or local structures of elements. Semiconductor detectors are usually used for separating the fluorescent of elements in question from background fluorescence. However, the semiconductor detectors cannot always discriminate K-lines of light elements and L-lines of various elements as different X-ray peaks at an energy range below about 3 keV. Superconducting tunnel junction (STJ) detectors are promising device for the soft X-ray at synchrotron radiation beam lines because of excellent energy resolution, high detection efficiency, and high counting rate. We are constructing a fluorescent X-ray spectrometer having 100-pixel array of STJs with 200 {mu}m square. The array detector is mounted on a liquid cryogen-free {sup 3}He cryostat. The sensitive area is the largest among the superconducting X-ray spectrometers operating at synchrotron beam lines. Each pixel is connected to a room temperature readout circuit that consists of a charge sensitive amplifier and a pulse height analyzer. The spectrometer will achieve a total solid angle of {approx}0.01 sr and a maximum counting rate of more than 1 M count per second. The present status of developments of our fluorescent X-ray spectrometer was reported.

  16. 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.

  17. 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

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

    PubMed

    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

  19. 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

  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. PMID:21615981

  1. Soft X-ray synchrotron radiation investigations of actinidematerials systems utilizing X-ray emission spectroscopy and resonantinelastic X-ray scattering

    SciTech Connect

    Shuh, D.K.; Butorin, S.M.; Guo, J.-H.; Nordgren, J.

    2004-01-03

    Synchrotron radiation (SR) methods have been utilized with increasing frequency over the past several years to study topics in actinide science, ranging from those of a fundamental nature to those that address a specifically-targeted technical need. In particular, the emergence of microspectroscopic and fluorescence-based techniques have permitted investigations of actinide materials at sources of soft x-ray SR. Spectroscopic techniques with fluorescence-based detection are useful for actinide investigations since they are sensitive to small amounts of material and the information sampling depth may be varied. These characteristics also serve to simplify both sample preparation and safety considerations. Examples of investigations using these fluorescence techniques will be described along with their results, as well as the prospects for future investigations utilizing these methodologies.

  2. 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.

  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. 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.

  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. 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.

  7. 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.

  8. 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.

  9. 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

  10. Microstructural Characterization and Corrosion Behavior of Al 7075 Alloys Using X-ray Synchrotron Tomography

    NASA Astrophysics Data System (ADS)

    Singh, Sudhanshu Shekhar

    Al 7075 alloys are used in a variety of structural applications, such as aircraft wings, automotive components, fuselage, spacecraft, missiles, etc. The mechanical and corrosion behavior of these alloys are dependent on their microstructure and the environment. Therefore, a comprehensive study on microstructural characterization and stress-environment interaction is necessary. Traditionally, 2D techniques have been used to characterize microstructure, which are inaccurate and inadequate since the research has shown that the results obtained in the bulk are different from those obtained on the surface. There now exist several techniques in 3D, which can be used to characterize the microstructure. Al 7075 alloys contain second phase particles which can be classified as Fe-bearing inclusions, Si-bearing inclusions and precipitates. The variation in mechanical and corrosion properties of aluminum alloys has been attributed to the size, shape, distribution, corrosion properties and mechanical behavior of these precipitates and constituent particles. Therefore, in order to understand the performance of Al 7075 alloys, it is critical to investigate the size and distribution of inclusions and precipitates in the alloys along with their mechanical properties, such as Young's modulus, hardness and stress-strain behavior. X-ray tomography and FIB tomography were used to visualize and quantify the microstructure of constituent particles (inclusions) and precipitates, respectively. Microscale mechanical characterization techniques, such as nanoindentation and micropillar compression, were used to obtain mechanical properties of inclusions. Over the years, studies have used surface measurements to understand corrosion behavior of materials. More recently, in situ mechanical testing has become more attractive and advantageous, as it enables visualization and quantification of microstructural changes as a function of time (4D). In this study, in situ X-ray synchrotron tomography

  11. High counting rates of x-ray photon detection using APD detectors on synchrotron machines

    SciTech Connect

    Kakuno, E. M.; Giacomolli, B. A.; Scorzato, C. R.

    2012-05-17

    In this work we show the results of 10 x 10 mm{sup 2} Si-APD detector's test with guard ring detecting x-rays. The result of mapping surface is also exhibited. We show and discuss the difficulty of single photon detection in high counting rate experiments in synchrotrons machines.

  12. CCD (charge-coupled device) sensors in synchrotron x-ray detectors

    SciTech Connect

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

    1987-01-01

    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/sup 2/ can be imaged on a 2 cm/sup 2/ CCD. With a conversion efficiency of approx.1 CCD electron/x-ray photon, a peak saturation capacity of >10/sup 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 x 10/sup 6/ pixels/s and the shift rate in the parallel registers is 10/sup 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 the rate of approx.1 frame/s or a complete 3-dimensional data set from a single crystal in approx.2 min. 16 refs., 16 figs., 2 tabs.

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

    PubMed

    Withers, P J

    2015-03-01

    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

  14. Multiple powder diffraction data for an accurate charge density study using synchrotron radiation x-ray

    NASA Astrophysics Data System (ADS)

    Kasai, Hidetaka; Nishibori, Eiji

    2016-04-01

    In recent years multiple synchrotron radiation (SR) powder x-ray diffraction profiles have been successfully applied to advanced structural studies such as an accurate charge density study and a structure determination from powder diffraction. The results have been presented with several examples. Abilities and future prospects have been discussed using state of the art powder diffraction data.

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

    DOE PAGESBeta

    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).

  16. 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.

  17. 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

  18. 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.

  19. 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.

  20. Phase-contrast X-ray imaging with synchrotron radiation for materials science applications

    NASA Astrophysics Data System (ADS)

    Stevenson, A. W.; Gureyev, T. E.; Paganin, D.; Wilkins, S. W.; Weitkamp, T.; Snigirev, A.; Rau, C.; Snigireva, I.; Youn, H. S.; Dolbnya, I. P.; Yun, W.; Lai, B.; Garrett, R. F.; Cookson, D. J.; Hyodo, K.; Ando, M.

    2003-01-01

    Since Röntgen's discovery of X-rays just over a century ago the vast majority of radiographs have been collected and interpreted on the basis of absorption contrast and geometrical (ray) optics. Recently the possibility of obtaining new and complementary information in X-ray images by utilizing phase-contrast effects has received considerable attention, both in the laboratory context and at synchrotron sources (where much of this activity is a consequence of the highly coherent X-ray beams which can be produced). Phase-contrast X-ray imaging is capable of providing improved information from weakly absorbing features in a sample, together with improved edge definition. Four different experimental arrangements for achieving phase contrast in the hard X-ray regime, for the purpose of non-destructive characterization of materials, will be described. Two of these, demonstrated at ESRF in France and AR in Japan, are based on parallel-beam geometry; the other two, demonstrated at PLS in Korea and APS in USA, are based on spherical-beam geometry. In each case quite different X-ray optical arrangements were used. Some image simulations will be employed to demonstrate salient features of hard X-ray phase-contrast imaging and examples of results from each of the experiments will be shown.

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

    DOE PAGESBeta

    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

  2. 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

  3. In situ x-ray diffraction measurements of the capillary fountain jet produced via ultrasonic atomization

    NASA Astrophysics Data System (ADS)

    Yano, Yohko F.; Douguchi, Junya; Kumagai, Atsushi; Iijima, Takao; Tomida, Yukinobu; Miyamoto, Toshiaki; Matsuura, Kazuo

    2006-11-01

    In situ x-ray diffraction measurements were carried out for investigating the liquid structure in the ultrasonic fountain jet to consider the mechanism of the "ultrasonic ethanol separation" reported by Sato et al. [J. Chem. Phys. 114, 2382 (2001)]. For pure liquids (water and ethanol), it was found that the high frequency ultrasound does not affect the liquid structure microscopically. For the 20mol% ethanol-water mixture, the estimated ethanol mole fraction in the ultrasonic fountain jet by using the position of the main maximum in the x-ray diffraction profile coincided with that in the reservoir. This result suggests that the ethanol separation is not caused by any distorted liquid structure under the ultrasound irradiation and occurs when or after the generation of the liquid droplet mist.

  4. In situ x-ray diffraction measurements of the capillary fountain jet produced via ultrasonic atomization.

    PubMed

    Yano, Yohko F; Douguchi, Junya; Kumagai, Atsushi; Iijima, Takao; Tomida, Yukinobu; Miyamoto, Toshiaki; Matsuura, Kazuo

    2006-11-01

    In situ x-ray diffraction measurements were carried out for investigating the liquid structure in the ultrasonic fountain jet to consider the mechanism of the "ultrasonic ethanol separation" reported by Sato et al. [J. Chem. Phys. 114, 2382 (2001)]. For pure liquids (water and ethanol), it was found that the high frequency ultrasound does not affect the liquid structure microscopically. For the 20 mol % ethanol-water mixture, the estimated ethanol mole fraction in the ultrasonic fountain jet by using the position of the main maximum in the x-ray diffraction profile coincided with that in the reservoir. This result suggests that the ethanol separation is not caused by any distorted liquid structure under the ultrasound irradiation and occurs when or after the generation of the liquid droplet mist. PMID:17100459

  5. In situ compressive damage of cement paste characterized by lab source X-ray computer tomography

    SciTech Connect

    Wan, Keshu; Xue, Xiaobo

    2013-08-15

    This paper aims at illustrating the potential of lab source X-ray CT for studying the damage behavior of cement based materials through in situ load experiments. This approach permits quantifying the microstructure prior and during loading. The load damage is separated from the specimen deformation using an image interpolation method. A quantitative relationship between external load and internal specimen damage is analyzed using the statistical information of gray scale values of the CT data. Local damage degrees are defined on 3D subset, and the 3D spatial distribution of damage information is clarified in this research. - Highlights: • On line damage is characterized by lab source X-ray CT. • Loading damage is separated with the specimen deformation. • Local damage is analyzed using gray scale values of the CT data. • 3D spatial distribution of the local damage information is clarified.

  6. Solution spectroelectrochemical cell for in situ X-ray absorption fine structure

    SciTech Connect

    Antonio, M.R.; Soderholm, L.; Song, I.

    1995-06-12

    A purpose-built spectroelectrochemical cell for in situ fluorescence XAFS (X-ray Absorption Fine Structure) measurements of bulk solution species during constant-potential electrolysis is described. The cell performance was demonstrated by the collection of europium L{sub 3}-edge XANES (X-ray Absorption Near Edge Structure) throughout the course of electrolysis of an aqueous solution of EuCl{sub 3}{center_dot}6H{sub 2}O in 1 M H{sub 2}SO{sub 4}. The europium L{sub 3}-edge resonances reported here for the Eu{sup III} and Eu{sup II} ions demonstrate that their 2p{sub 3/2} {yields} 5d electronic transition probabilities are not the same.

  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. PMID:27475566

  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. 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

  10. In situ X-ray monitoring of damage accumulation in SiC/RBSN tensile specimens

    NASA Technical Reports Server (NTRS)

    Baaklini, George Y.; Bhatt, Ramkrishna T.

    1991-01-01

    The room-temperature tensile testing of silicon carbide fiber reinforced reaction-bonded silicon nitride (SiC/RBSN) composite specimens was monitored by using in-situ X-ray film radiography. Radiographic evaluation before, during, and after loading provided data on the effect of preexisting volume flaws (high density impurities, and local density variations) on the fracture behavior of composites. Results from (O)1, (O)3, (O)5, and (O)8 composite specimens showed that X-ray film radiography can monitor damage accumulations during tensile loading. Matrix cracking, fiber-matrix debonding, and fiber pullout were imaged throughout the tensile loading history of the specimens. Further, in-situ film radiography was found to be a helpful and practical technique for estimating interfacial shear strength between the SiC fiber and the RBSN matrix by the matrix crack spacing method. It is concluded that pretest, in-situ, and post-test radiography can provide for a greater understanding of ceramic matrix composite mechanical behavior, a verification of related experimental procedures, and a validation and development of related analytical models.

  11. In situ X-ray monitoring of damage accumulation in SiC/RBSN tensile specimens

    SciTech Connect

    Baaklini, G.Y.; Bhatt, R.T.

    1991-08-01

    The room-temperature tensile testing of silicon carbide fiber reinforced reaction-bonded silicon nitride (SiC/RBSN) composite specimens was monitored by using in-situ X-ray film radiography. Radiographic evaluation before, during, and after loading provided data on the effect of preexisting volume flaws (high density impurities, and local density variations) on the fracture behavior of composites. Results from (O)1, (O)3, (O)5, and (O)8 composite specimens showed that X-ray film radiography can monitor damage accumulations during tensile loading. Matrix cracking, fiber-matrix debonding, and fiber pullout were imaged throughout the tensile loading history of the specimens. Further, in-situ film radiography was found to be a helpful and practical technique for estimating interfacial shear strength between the SiC fiber and the RBSN matrix by the matrix crack spacing method. It is concluded that pretest, in-situ, and post-test radiography can provide for a greater understanding of ceramic matrix composite mechanical behavior, a verification of related experimental procedures, and a validation and development of related analytical models. 14 refs.

  12. 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

  13. 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.

  14. In situ x-ray diffraction of shock-driven deformation and phase transformation in titanium

    NASA Astrophysics Data System (ADS)

    Bolme, Cynthia; Lazicki, Amy; Brown, Don; Gleason, Arianna; Cerreta, Ellen; Morrow, Ben; Ali, Suzanne; Swift, Damian; Nagler, Bob; Galtier, Eric; Granados, Eduardo; Milathianaki, Despina; Heimann, Phil

    2015-06-01

    Titanium alloys are employed in demanding engineering applications due to their high strength-to-weight ratio and their resistance to corrosion. Pure titanium and titanium with high levels of oxygen impurities were studied under laser-driven shock compression at the Matter in Extreme Conditions endstation at the Linac Coherent Light Source. In situ x-ray diffraction data were acquired during compression, showing the lattice-level response of titanium as it underwent plastic deformation and phase transformation. The kinetics of these processes and the influence of oxygen impurities on the deformation behavior will be presented.

  15. 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.

  16. In situ X-ray absorption study of copper films in ground water solutions

    NASA Astrophysics Data System (ADS)

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

    2007-10-01

    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 - and HCO3- 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 HCO3- prevented or slowed down the corrosion processes.

  17. In-situ X-ray characterization of the reaction of lithium with InSe

    SciTech Connect

    Levy-Clement, C.; Dahn, J.R.; McKinnon, W.R.; Rioux, J.

    1984-12-01

    The reaction at room temperature of Li with InSe in Li/InSe electrochemical cells was studied using in-situ X-ray diffraction. Li reacts with InSe first to form Li/sub 2/Se and In, then reacts with the In to form InLi. An intermediate phase appears in each of these two steps. The first intermediate phase may be an intercalation compound Li /SUB x/ InSe, the second some In-Li alloy.

  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. 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.

  20. 3D/4D analyses of damage and fracture behaviours in structural materials via synchrotron X-ray tomography.

    PubMed

    Toda, Hiroyuki

    2014-11-01

    X-ray microtomography has been utilized for the in-situ observation of various structural metals under external loading. Recent advances in X-ray microtomography provide remarkable tools to image the interior of materials. In-situ X-ray microtomography provides a unique possibility to access the 3D character of internal microstructure and its time evolution behaviours non-destructively, thereby enabling advanced techniques for measuring local strain distribution. Local strain mapping is readily enabled by processing such high-resolution tomographic images either by the particle tracking technique or the digital image correlation technique [1]. Procedures for tracking microstructural features which have been developed by the authors [2], have been applied to analyse localised deformation and damage evolution in a material [3]. Typically several tens of thousands of microstructural features, such as particles and pores, are tracked in a tomographic specimen (0.2 - 0.3 mm(3) in volume). When a sufficient number of microstructural features is dispersed in 3D space, the Delaunay tessellation algorithm is used to obtain local strain distribution. With these techniques, 3D strain fields can be measured with reasonable accuracy. Even local crack driving forces, such as local variations in the stress intensity factor, crack tip opening displacement and J integral along a crack front line, can be measured from discrete crack tip displacement fields [4]. In the present presentation, complicated crack initiation and growth behaviour and the extensive formation of micro cracks ahead of a crack tip are introduced as examples.A novel experimental method has recently been developed by amalgamating a pencil beam X-Ray diffraction (XRD) technique with the microstructural tracking technique [5]. The technique provides information about individual grain orientations and 1-micron-level grain morphologies in 3D together with high-density local strain mapping. The application of this

  1. 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

  2. Dosimetry of Microdistributed Dose-Enhancing Agents in X-ray Synchrotron Binary Therapy

    NASA Astrophysics Data System (ADS)

    Hugtenburg, Richard P.

    2010-07-01

    Monte Carlo based modelling of the dose distribution in the vicinity of concentrates of iodine (I) and gold (Au) binary radiotherapy agents has been performed for monochromatised synchrotron X-rays. While the KERMA approximation, which ignores electron transport, is often acceptable for kilovoltage X-ray dosimetry in X-ray binary therapy, the range of photoelectrons and Auger electrons may be significant when compared to the microdostributed structure of the binary compound in which case corrections to the approximation may be necessary. Dose is calculated using EGSnrc for microdistributions associated with X-ray radiation synovecotomy, where iodine is taken up in the synovial lining. Dose as a function of the volume of aggregation for an Au-based contrast agent such as Au nanoparticles, ranging in diameter from 5 micron to 100 micron, were calculated using EGSnrc and Penelope, showing that the dose varies slowly for 90 keV X-rays, where much of the dose delivered by short range photoelectrons while 80 keV X-rays, just below the K-edge of Au (80.729 keV) increases linearly with diameter. In general the dose varies slowly as a function of volume suggesting that only small corrections will be needed to account for effects due to the failure of electronic equilibrium.

  3. Dosimetry of Microdistributed Dose-Enhancing Agents in X-ray Synchrotron Binary Therapy

    SciTech Connect

    Hugtenburg, Richard P.

    2010-07-23

    Monte Carlo based modelling of the dose distribution in the vicinity of concentrates of iodine (I) and gold (Au) binary radiotherapy agents has been performed for monochromatised synchrotron X-rays. While the KERMA approximation, which ignores electron transport, is often acceptable for kilovoltage X-ray dosimetry in X-ray binary therapy, the range of photoelectrons and Auger electrons may be significant when compared to the microdostributed structure of the binary compound in which case corrections to the approximation may be necessary. Dose is calculated using EGSnrc for microdistributions associated with X-ray radiation synovecotomy, where iodine is taken up in the synovial lining. Dose as a function of the volume of aggregation for an Au-based contrast agent such as Au nanoparticles, ranging in diameter from 5 micron to 100 micron, were calculated using EGSnrc and Penelope, showing that the dose varies slowly for 90 keV X-rays, where much of the dose delivered by short range photoelectrons while 80 keV X-rays, just below the K-edge of Au (80.729 keV) increases linearly with diameter. In general the dose varies slowly as a function of volume suggesting that only small corrections will be needed to account for effects due to the failure of electronic equilibrium.

  4. X-Ray Synchrotron-emitting Fe-rich Ejecta in Supernova Remnant RCW 86

    NASA Astrophysics Data System (ADS)

    Rho, Jeonghee; Dyer, Kristy K.; Borkowski, Kazimierz J.; Reynolds, Stephen P.

    2002-12-01

    Supernova remnants may exhibit both thermal and nonthermal X-ray emission. In a previous study with ASCA data, we found that the middle-aged supernova remnant RCW 86 showed evidence for both processes, and we predicted that observations with much higher spatial resolution would distinguish harder X-rays, which we proposed were primarily synchrotron emission, from softer, thermal X-rays. Here we describe Chandra observations that amply confirm our predictions. Striking differences in the morphology of X-rays below 1 keV and above 2 keV point to a different physical origin. Hard X-ray emission is correlated fairly well with the edges of regions of radio emission, suggesting that these are the locations of shock waves at which both short-lived X-ray-emitting electrons and longer lived radio-emitting electrons are accelerated. Soft X-rays are spatially well correlated with optical emission from nonradiative shocks, which are almost certainly portions of the outer blast wave. These soft X-rays are well fitted with simple thermal plane-shock models. Harder X-rays show Fe Kα emission and are well described with a similar soft thermal component, but a much stronger synchrotron continuum dominating above 2 keV, and a strong Fe Kα line. Quantitative analysis of this line and the surrounding continuum shows that it cannot be produced by thermal emission from a cosmic-abundance plasma; the ionization time is too short, as shown by both the low centroid energy (6.4 keV) and the absence of oxygen lines below 1 keV. Instead, a model of a plane shock in Fe-rich ejecta, with a synchrotron continuum, provides a natural explanation. This requires that reverse shocks in ejecta be accelerating electrons to energies of order 50 TeV. We show that maximum energies of this order can be produced by radiation-limited diffusive shock acceleration at the reverse shocks. In the Appendix, we demonstrate that an explanation of the continuum as being due to nonthermal bremsstrahlung is unlikely.

  5. The first microbeam synchrotron X-ray fluorescence beamline at the Siam Photon Laboratory.

    PubMed

    Tancharakorn, Somchai; Tanthanuch, Waraporn; Kamonsutthipaijit, Nuntaporn; Wongprachanukul, Narupon; Sophon, Methee; Chaichuay, Sarunyu; Uthaisar, Chunmanus; Yimnirun, Rattikorn

    2012-07-01

    The first microbeam synchrotron X-ray fluorescence (µ-SXRF) beamline using continuous synchrotron radiation from Siam Photon Source has been constructed and commissioned as of August 2011. Utilizing an X-ray capillary half-lens allows synchrotron radiation from a 1.4 T bending magnet of the 1.2 GeV electron storage ring to be focused from a few millimeters-sized beam to a micrometer-sized beam. This beamline was originally designed for deep X-ray lithography (DXL) and was one of the first two operational beamlines at this facility. A modification has been carried out to the beamline in order to additionally enable µ-SXRF and synchrotron X-ray powder diffraction (SXPD). Modifications included the installation of a new chamber housing a Si(111) crystal to extract 8 keV synchrotron radiation from the white X-ray beam (for SXPD), a fixed aperture and three gate valves. Two end-stations incorporating optics and detectors for µ-SXRF and SXPD have then been installed immediately upstream of the DXL station, with the three techniques sharing available beam time. The µ-SXRF station utilizes a polycapillary half-lens for X-ray focusing. This optic focuses X-ray white beam from 5 mm × 2 mm (H × V) at the entrance of the lens down to a diameter of 100 µm FWHM measured at a sample position 22 mm (lens focal point) downstream of the lens exit. The end-station also incorporates an XYZ motorized sample holder with 25 mm travel per axis, a 5× ZEISS microscope objective with 5 mm × 5 mm field of view coupled to a CCD camera looking to the sample, and an AMPTEK single-element Si (PIN) solid-state detector for fluorescence detection. A graphic user interface data acquisition program using the LabVIEW platform has also been developed in-house to generate a series of single-column data which are compatible with available XRF data-processing software. Finally, to test the performance of the µ-SXRF beamline, an elemental surface profile has been obtained for

  6. 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.

  7. 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.

  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. Hard-X-ray magnetic microscopy and local magnetization analysis using synchrotron radiation.

    PubMed

    Suzuki, Motohiro

    2014-11-01

    X-ray measurement offers several useful features that are unavailable from other microscopic means including electron-based techniques. By using X-rays, one can observe the internal parts of a thick sample. This technique basically requires no high vacuum environment such that measurements are feasible for wet specimens as well as under strong electric and magnetic fields and even at a high pressure. X-ray spectroscopy using core excitation provides element-selectivity with significant sensitivities to the chemical states and atomic magnetic moments in the matter. Synchrotron radiation sources produce a small and low-divergent X-ray beam, which can be converged to a spot with the size of a micrometer or less using X-ray focusing optics. The recent development in the focusing optics has been driving X-ray microscopy, which has already gone into the era of X-ray nanoscopy. With the use of the most sophisticated focusing devices, an X-ray beam of 7-nm size has successfully been achieved [1]. X-ray microscopy maintains above-mentioned unique features of X-ray technique, being a perfect complement to electron microscopy.In this paper, we present recent studies on magnetic microscopy and local magnetic analysis using hard X-rays. The relevant instrumentation developments are also described. The X-ray nanospectroscopy station of BL39XU at SPring-8 is equipped with a focusing optics consisting of two elliptic mirrors, and a focused X-ray beam with the size of 100 × 100 nm(2) is available [2]. Researchers can perform X-ray absorption spectroscopy: nano-XAFS (X-ray absorption fine structure) using the X-ray beam as small as 100 nm. The available X-ray energy is from 5 to 16 keV, which allows nano-XAFS study at the K edges of 3d transition metals, L edges of rare-earth elements and 5d noble metals. Another useful capability of the nanoprobe is X-ray polarization tunability, enabling magnetic circular dichroism (XMCD) spectroscopy with a sub-micrometer resolution. Scanning

  10. 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

  11. Antioxidant protects blood-testis barrier against synchrotron radiation X-ray-induced disruption

    PubMed Central

    Zhang, Tingting; Liu, Tengyuan; Shao, Jiaxiang; Sheng, Caibin; Hong, Yunyi; Ying, Weihai; Xia, Weiliang

    2015-01-01

    Synchrotron radiation (SR) X-ray has wide biomedical applications including high resolution imaging and brain tumor therapy due to its special properties of high coherence, monochromaticity and high intensity. However, its interaction with biological tissues remains poorly understood. In this study, we used the rat testis as a model to investigate how SR X-ray would induce tissue responses, especially the blood-testis barrier (BTB) because BTB dynamics are critical for spermatogenesis. We irradiated the male gonad with increasing doses of SR X-ray and obtained the testicles 1, 10 and 20 d after the exposures. The testicle weight and seminiferous tubule diameter reduced in a dose- and time-dependent manner. Cryosections of testes were stained with tight junction (TJ) component proteins such as occludin, claudin-11, JAM-A and ZO-1. Morphologically, increasing doses of SR X-ray consistently induced developing germ cell sloughing from the seminiferous tubules, accompanied by shrinkage of the tubules. Interestingly, TJ constituent proteins appeared to be induced by the increasing doses of SR X-ray. Up to 20 d after SR X-ray irradiation, there also appeared to be time-dependent changes on the steady-state level of these protein exhibiting differential patterns at 20-day after exposure, with JAM-A/claudin-11 still being up-regulated whereas occludin/ZO-1 being down-regulated. More importantly, the BTB damage induced by 40 Gy of SR X-ray could be significantly attenuated by antioxidant N-Acetyl-L-Cysteine (NAC) at a dose of 125 mg/kg. Taken together, our studies characterized the changes of TJ component proteins after SR X-ray irradiation, illustrating the possible protective effects of antioxidant NAC to BTB integrity. PMID:26413412

  12. 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.

  13. Monitoring simultaneously the growth of nanoparticles and aggregates by in situ ultra-small-angle x-ray scattering

    NASA Astrophysics Data System (ADS)

    Kammler, Hendrik K.; Beaucage, Gregory; Kohls, Douglas J.; Agashe, Nikhil; Ilavsky, Jan

    2005-03-01

    Ultra-small-angle x-ray scattering can provide information about primary particles and aggregates from a single scattering experiment. This technique is applied in situ to flame aerosol reactors for monitoring simultaneously the primary particle and aggregate growth dynamics of oxide nanoparticles in a flame. This was enabled through the use of a third generation synchrotron source (Advanced Photon Source, Argonne IL, USA) using specialized scattering instrumentation at the UNICAT facility which is capable of simultaneously measuring nanoscales to microscales (1nmto1μm). More specifically, the evolution of primary-particle diameter, mass-fractal dimension, geometric standard deviation, silica volume fraction, number concentration, radius of gyration of the aggregate, and number of primary particles per aggregate are measured along the flame axis for two different premixed flames. All these particle characteristics were derived from a single and nonintrusive measurement technique. Flame temperature profiles were measured in the presence of particles by in situ Fourier transform infrared spectroscopy and thermophoretic sampling was used to visualize particle growth with height above the burner as well as in the radial direction.

  14. 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.

  15. 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.

  16. In situ x-ray photoemission studies of the oxidation of Y-Ba-Cu films

    SciTech Connect

    Price, R.J.; Jackman, R.B.; Foord, J.S.

    1988-12-15

    X-ray photoemission has been used to investigate the formation of Y-Ba-Cu films on Si(100) and as an in situ probe of their subsequent oxidation to yield the associated oxide ceramic. The layers are prepared by coevaporation of the metallic components under ultrahigh vacuum, and pure alloy phases can be deposited at 300 K; reaction with the underlying substrate resulting in loss of Cu and incorporation by Si in the film takes place, however, at higher temperatures. Room-temperature oxidation stabilizes the film against this interaction and results in the preferential oxidation and surface segregation of barium at the expense of Cu. This segregation process becomes even more apparent during higher temperature (approx.600 K) oxidation reactions. Chemical shifts and associated effects in x-ray photoelectron spectra are used to infer information on the chemical changes that occur in the film as oxidation proceeds. The thin-film phases prepared in situ in this work reveal a very similar surface composition to bulk superconducting samples prepared ex situ. This suggests that the surface segregation in bulk samples does not simply result from reaction with species such as water vapor, but instead may represent an equilibrium state of the oxide-oxygen interface.

  17. In Situ X-ray Reflectivity Studies of Protein Adsorption onto Functionalized Surfaces

    NASA Astrophysics Data System (ADS)

    Richter, Andrew

    2007-03-01

    The adsorption of protein films onto solid surfaces, both artificial and naturally occurring, have been widely studied using a variety of techniques due to their importance in medicine, biomedical applications, and the general understanding of protein structure and function. What have yet to be performed are in situ, time-resolved, high-resolution structural studies of these systems. We have begun a project that uses the technique of in situ x-ray reflectivity to obtain highly resolved structural information with time resolution on the order of minutes. This talk will present our first findings of serum albumin and immunoglobulin G films on hydrophobic self-assembled monolayers. The protein films are readily observable, showing extensive denaturing after adsorption with a slow decay of density into the aqueous solution. Additionally, a thin low-density region that occurs between the hydrophobic film and the solution persists after protein deposition. Comparisons to films that are removed from solution, the influence of solution concentration, the effects of x-ray damage, and the time scales for protein film formation and evolution will also be discussed.

  18. Energy dispersive X-ray diffraction in the diamond anvil, high-pressure apparatus - Comparison of synchrotron and conventional X-ray sources

    NASA Technical Reports Server (NTRS)

    Spain, I. L.; Black, D. R.

    1985-01-01

    The use of both conventional fixed-anode X-ray sources and synchrotron radiation to carry out energy-dispersive X-ray diffraction experiments at high pressure in a diamond anvil cell, is discussed. The photon flux at the sample and at the detector for the two cases are compared and the results are presented in graphs. It is shown that synchrotron radiation experiments can be performed with nearly two orders of magnitude increase in data rate if superior detectors and detector electronics are available.

  19. Trace element abundances in single presolar silicon carbide grains by synchrotron X-ray fluorescence

    NASA Astrophysics Data System (ADS)

    Kashiv, Yoav

    2004-12-01

    Synchrotron x-ray fluorescence (SXRF) was applied to the study of presolar grains for the first time in this study. 41 single SiC grains of the KJF size fraction (mass-weighted median size of 1.86 μm) from the Murchison (CM2) Meteorite were analyzed. The absolute abundances of the following elements were determined (not every element in every grain): S, Ca, Ti, V, Cr, Mn, Fe, Co, Ni, Sr, Y, Zr, Nb, Mo, Ru, Os, Ir and Pt (underlined elements were detected here for the first time in single grains). There is good agreement between the heavier trace element abundances in the grains and s-process nucleosynthesis calculations. It suggests that smaller 13C pocket sizes are needed in the parent stars, a free parameter in the stellar models, than is deduced from isotopic analyses of s-, and s-mainly, elements, such as Zr and Mo. In addition, the data confirms the radiogenic nature of the Nb in the grains, due to the in situ decay of 93Zr (t 1/2 = 1.5 × 106 year). The data suggest that the trace elements condensed into the host SiC grains by a combination of condensation in solid solution and incorporation of subgrains. It seems that many of the trace elements reside mainly in subgrains of two solid solution: (1)a TiC based solid solution, and (2)a Mo-Ru carbide based solid solution. The presence of subgrains of an Fe-Ni alloy solid solution is suggested as well. Subgrains of all 3 solid solutions were observed previously in presolar graphite grains.* *This dissertation is a compound document (contains both a paper copy and a CD as part of the dissertation). The CD requires the following system requirements: Adobe Acrobat.

  20. 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.

  1. 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.

  2. 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.

  3. 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.

  4. 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.

  5. 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.

  6. Nanoscale chemical imaging using synchrotron x-ray enhanced scanning tunneling microscopy

    SciTech Connect

    Rose, Volker; Freeland, John W.

    2010-06-23

    The combination of synchrotron radiation with scanning tunneling microscopy provides a promising new concept for chemical imaging of nanoscale structures. It employs detection of local x-ray absorption, which directly yields chemical, electronic, and magnetic sensitivity. The study of the tip current in the far field (800 nm tip/sample separation) shows that insulator-coated tips have to be considered in order to reduce the background from stray photoelectron. A picture of the different channels contributing to the x-ray enhanced STM process is proposed. If during electron tunneling the sample is illuminated with monochromatic x-rays, characteristic absorption will arise, and core electrons are excited, which might modulate the conventional tunnel current and facilitate chemical imaging at the nanoscale.

  7. 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.

  8. Design and application of a high-temperature microfurnace for an in situ X-ray diffraction study of phase transformation.

    PubMed

    Eu, W S; Cheung, W H; Valix, M

    2009-11-01

    Thermal treatment of mineral ores such as ilmenite can initiate phase transformations that could affect their activation or deactivation, subsequently influencing their ability to dissolve in a leaching agent. Most laboratory-based X-ray diffraction (XRD) studies were carried out ex situ in which realistic diffraction patterns could not be obtained simultaneously with occurring reactions and were time-consuming. The availability of synchrotron-radiation-based XRD not only allows in situ analysis, but significantly shortens the data recording time. The present study details the design of a robust high-temperature microfurnace which allows thermal processing of mineral ore samples and the simultaneous collection of high-resolution synchrotron XRD data. In addition, the application of the manufactured microfurnace for in situ study of phase transformations of ilmenite ore under reducing conditions is demonstrated. PMID:19844022

  9. 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

  10. 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.

  11. 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

  12. 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.

  13. 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.

  14. 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.

  15. Progress in Cell Marking for Synchrotron X-ray Computed Tomography

    NASA Astrophysics Data System (ADS)

    Hall, Christopher; Sturm, Erica; Schultke, Elisabeth; Arfelli, Fulvia; Menk, Ralf-Hendrik; Astolfo, Alberto; Juurlink, Bernhard H. J.

    2010-07-01

    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.

  16. 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.

  17. Image alignment for tomography reconstruction from synchrotron X-ray microscopic images.

    PubMed

    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 x-θ 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

  18. 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.

  19. 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.

  20. 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.

  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. 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

  3. 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.

  4. 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.

  5. 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.

  6. Synchrotron X-ray and ab initio studies of beta-Si3N4.

    PubMed

    du Boulay, D; Ishizawa, N; Atake, T; Streltsov, V; Furuya, K; Munakata, F

    2004-08-01

    Almost absorption- and extinction-free single-crystal synchrotron X-ray diffraction data were measured at 150, 200 and 295 K for beta-Si3N4, silicon nitride, at a wavelength of 0.7 A. The true symmetry of this material has been the subject of minor controversy for several decades. No compelling evidence favouring the low-symmetry P6(3) model was identified in this study. PMID:15258397

  7. Applications of synchrotron x-ray fluorescence microprobe techniques to photochromic materials

    SciTech Connect

    Perry, D.L.

    1996-12-31

    Applications of synchrotron x-ray fluorescence microprobe techniques to photochromic materials are presented regarding dopant metal ions in the crystal matrices. Types of samples that are amenable to the technique will be discussed, along with sample format and experimental conditions. The chemical information that one can obtain from samples will be presented, and examples of copant contaminant studies in crystals will be given. New types of samples that are possible to study using this technique will be presented.

  8. A tunable wedge-shaped absorber for hard X-ray synchrotron applications.

    PubMed

    Krywka, C; Brix, M; Müller, M

    2014-07-01

    The concept of a concave aluminium wedge-shaped absorber for hard X-ray synchrotron beamlines is presented. Unlike the commonly used absorber types (fixed-thickness absorber sheets or binary exchangers of individual fixed absorbers), this concept allows a compact system, controlled with a single linear positioner, and provides a wide attenuation range as well as a precise tunability over a large energy range. Data were recorded at the Nanofocus Endstation of the MINAXS beamline, PETRA III, Hamburg, Germany. PMID:24971979

  9. 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.

  10. 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.

  11. Synchrotron X-ray muprobe and its application to human hair analysis

    NASA Astrophysics Data System (ADS)

    Iida, Atsuo; Noma, Takashi

    1993-07-01

    A synchrotron X-ray muprobe system based on Kirkpatrick-Baez optics has been developed. Double-crystal and synthetic multilayer monochromators are used for high energy resolution experiments and for highly sensitive X-ray fluorescence analysis, respectively. The characteristics of the X-ray muprobe were experimentally examined. A beam size of around 5 μm was obtained; the X-ray photon flux at the storage ring current of 300 mA is of the order of 10 7-8 photons/s and 10 9-10 photons/s for the double-crystal and multilayer monochromators, respectively. The concentration distributions of trace elements in cross sections of human hair were measured using an X-ray mubeam with the multilayer monochromator. Inhomogeneous distributions of trace elements in thin cross-section samples show that two-dimensional imaging is effective and indispensable both for the determination of the elemental concentration in hair and for investigating the incorporation mechanism of trace elements into hair from the body.

  12. 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.

  13. 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.

  14. 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

  15. In-situ metrology for the optimization of bent crystals used in hard-X-ray monochromators: Comparison between measurement and simulation

    NASA Astrophysics Data System (ADS)

    Thomasset, Muriel; Moreno, Thierry; Capitanio, Blandine; Idir, Mourad; Bucourt, Samuel

    2010-05-01

    Crystal sagittal focusing is known as one of the most efficient way of focusing synchrotron X-ray radiation from bending magnet sources, thus delivering increases photon flux at the sample position. To optimize the performance of a sagittaly bent crystal inside a monochromator, it is necessary to have knowledge of its radius of curvature. However, this measurement is not very easy to obtain. Even though the use of the X-ray beam is the ultimate source for optimizing the system, it is still necessary to have a prior knowledge of the radius of curvature as a function of the motor bender positions to avoid any catastrophic failure. In this paper, we describe a simple, efficient and accurate method of measuring the radius of curvature of sagitally bent monochromator crystals at several bending magnet beamlines at synchrotron SOLEIL. To optimize the crystal bending inside these monochromators, we used a Shack-Hartmann sensor (HP 26) developed by the Imagine Optic Company (Orsay/France). This high accuracy two-dimensional metrology tool was originally designed to be installed on a Long Trace Profiler translation stage to measure the mirrors profiles. During a period where the SOLEIL synchrotron was in shutdown, this instrument was directly mounted inside the monochromator so that the radius of curvature could be measured in-situ. This method allows us to optimize the curvature and eliminate twist before bending strongly the crystal below radii of curvature of less than 2 m. The second step in the optimization process was to use the X-ray beam for the final adjustments of the bending system, where X-ray images are then used to analyse the residual defaults of the system. Using SpotX, a ray-tracing simulation tool, these errors can be fully analysed and a fully optimized system can then be obtained. Overall, five beamlines at synchrotron SOLEIL have used in this method to optimize their monochromators.

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

    NASA Astrophysics Data System (ADS)

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

    2014-07-01

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

  17. 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.

  18. Direct synchrotron x-ray measurements of local strain fields in elastically and plastically bent metallic glasses

    DOE PAGESBeta

    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

  19. 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

  20. 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.

  1. 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.

  2. 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. PMID:26652294

  3. DIFFUSE HARD X-RAY EMISSION IN STARBURST GALAXIES AS SYNCHROTRON FROM VERY HIGH ENERGY ELECTRONS

    SciTech Connect

    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 {sup {+-}}) can contribute to this emission, because starbursts have strong magnetic fields. We consider three sources of e {sup {+-}} at these energies: (1) primary electrons directly accelerated by supernova remnants, (2) pionic secondary e {sup {+-}} created by inelastic collisions between cosmic ray (CR) protons and gas nuclei in the dense interstellar medium of starbursts, and (3) pair e {sup {+-}} produced between the interactions between 10 and 100 TeV {gamma}-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 {sup {+-}}. We compare these models to extant radio and GeV and TeV {gamma}-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 {approx}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

  4. 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

  5. Near-isothermal furnace for in situ and real time X-ray radiography solidification experiments

    NASA Astrophysics Data System (ADS)

    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.

  6. 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.

  7. 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. PMID:26133847

  8. Use of x-ray fluorescence for in-situ detection of metals

    NASA Astrophysics Data System (ADS)

    Elam, W. T. E.; Whitlock, Robert R.; Gilfrich, John V.

    1995-01-01

    X-ray fluorescence (XRF) is a well-established, non-destructive method of determining elemental concentrations at ppm levels in complex samples. It can operate in atmosphere with no sample preparation, and provides accuracies of 1% or better under optimum conditions. This report addresses two sets of issues concerning the use of x-ray fluorescence as a sensor technology for the cone penetrometer, for shipboard waste disposal, or for other in-situ, real- time environmental applications. The first issue concerns the applicability of XRF to these applications, and includes investigation of detection limits and matrix effects. We have evaluated the detection limits and quantitative accuracy of a sensor mock-up for metals in soils under conditions expected in the field. In addition, several novel ways of improving the lower limits of detection to reach the drinking water regulatory limits have been explored. The second issue is the engineering involved with constructing a spectrometer within the 1.75 inch diameter of the penetrometer pipe, which is the most rigorous physical constraint. Only small improvements over current state-of-the-art are required. Additional advantages of XRF are that no radioactive sources or hazardous materials are used in the sensor design, and no reagents or any possible sources of ignition are involved.

  9. 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

  10. 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.

  11. In situ energy dispersive x-ray reflectometry measurements on organic solar cells upon working

    NASA Astrophysics Data System (ADS)

    Paci, B.; Generosi, A.; Albertini, V. Rossi; Perfetti, P.; de Bettignies, R.; Firon, M.; Leroy, J.; Sentein, C.

    2005-11-01

    The change in the morphology of plastic solar cells was studied by means of time-resolved energy dispersive x-ray reflectivity (XRR). This unconventional application of the XRR technique allowed the follow up of in situ morphological evolution of an organic photovoltaic device upon working. The study consisted of three steps: A preliminary set of XRR measurements on various samples representing the intermediate stages of cell construction, which provided accurate data regarding the electronic densities of the different layers; the verification of the morphological stability of the device under ambient condition; a real-time collection of XRR patterns, both in the dark and during 15h in artificial light conditions which allowed the changes in the system morphology at the electrode-active layer interface to be monitored. In this way, a progressive thickening of this interface, responsible for a reduction in the performances of the device, was observed directly.

  12. 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.

  13. In situ surface X-ray scattering of stepped surface of platinum: Pt(311).

    PubMed

    Nakahara, Akira; Nakamura, Masashi; Sumitani, Kazushi; Sakata, Osami; Hoshi, Nagahiro

    2007-10-23

    Surface structure of a stepped surface of Pt, Pt(311) (=2(100)-(111)), has been determined under potential control in 0.1 M HClO4 with the use of in situ surface X-ray scattering (SXS). The crystal truncation rods (CTRs) are reproduced well with the (1x2) missing-row model. Relaxation of surface layers, which is observed on the low-index planes of Pt, is not found on Pt(311) in the "adsorbed hydrogen region". CTRs at 0.10 (RHE) have the same feature as those at 0.50 V, showing that the surface layers of Pt(311) have no potential dependence. Scanning tunneling microscopy (STM) also supports the (1x2) structure of Pt(311) in 0.1 M HClO4. PMID:17902717

  14. 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.

  15. 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.

  16. 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. PMID:24410395

  17. 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

  18. 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.

  19. 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

  20. 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). PMID:27140147

  1. 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

  2. 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.

  3. Investigation of internal structure of fine granules by microtomography using synchrotron X-ray radiation.

    PubMed

    Noguchi, Shuji; Kajihara, Ryusuke; Iwao, Yasunori; Fujinami, Yukari; Suzuki, Yoshio; Terada, Yasuko; Uesugi, Kentaro; Miura, Keiko; Itai, Shigeru

    2013-03-10

    Computed tomography (CT) using synchrotron X-ray radiation was evaluated as a non-destructive structural analysis method for fine granules. Two kinds of granules have been investigated: a bromhexine hydrochloride (BHX)-layered Celphere CP-102 granule coated with pH-sensitive polymer Kollicoat Smartseal 30-D, and a wax-matrix granule constructed from acetaminophen (APAP), dibasic calcium phosphate dehydrate, and aminoalkyl methacrylate copolymer E (AMCE) manufactured by melt granulation. The diameters of both granules were 200-300 μm. CT analysis of CP-102 granule could visualize the laminar structures of BHX and Kollicoat layers, and also visualize the high talc-content regions in the Kollicoat layer that could not be detected by scanning electron microscopy. Moreover, CT analysis using X-ray energies above the absorption edge of Br specifically enhanced the contrast in the BHX layer. As for granules manufactured by melt granulation, CT analysis revealed that they had a small inner void space due to a uniform distribution of APAP and other excipients. The distribution of AMCE revealed by CT analysis was also found to involve in the differences of drug dissolution from the granules as described previously. These observations demonstrate that CT analysis using synchrotron X-ray radiation is a powerful method for the detailed internal structure analysis of fine granules. PMID:23376507

  4. 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

  5. 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.

  6. Trace element abundance determinations by Synchrotron X Ray Fluorescence (SXRF) on returned comet nucleus mineral grains

    NASA Technical Reports Server (NTRS)

    Flynn, G. J.; Sutton, S. R.

    1989-01-01

    Trace element analyses were performed on bulk cosmic dust particles by Proton Induced X Ray Emission (PIXE) and Synchrotron X Ray Fluorescence (SXRF). When present at or near chondritic abundances the trace elements K, Ti, Cr, Mn, Cu, Zn, Ga, Ge, Se, and Br are presently detectable by SXRF in particles of 20 micron diameter. Improvements to the SXRF analysis facility at the National Synchrotron Light Source presently underway should increase the range of detectable elements and permit the analysis of smaller samples. In addition the Advanced Photon Source will be commissioned at Argonne National Laboratory in 1995. This 7 to 8 GeV positron storage ring, specifically designed for high-energy undulator and wiggler insertion devices, will be an ideal source for an x ray microprobe with one micron spatial resolution and better than 100 ppb elemental sensitivity for most elements. Thus trace element analysis of individual micron-sized grains should be possible by the time of the comet nucleus sample return mission.

  7. In situ x-ray reflectivity and grazing incidence x-ray diffraction study of L 1(0) ordering in (57)Fe/Pt multilayers.

    PubMed

    Raghavendra Reddy, V; Gupta, Ajay; Gome, Anil; Leitenberger, Wolfram; Pietsch, U

    2009-05-01

    In situ high temperature x-ray reflectivity and grazing incidence x-ray diffraction measurements in the energy dispersive mode are used to study the ordered face-centered tetragonal (fct) L 1(0) phase formation in [Fe(19 Å)/Pt(25 Å)]( × 10) multilayers prepared by ion beam sputtering. With the in situ x-ray measurements it is observed that (i) the multilayer structure first transforms to a disordered FePt and subsequently to an ordered fct L 1(0) phase, (ii) the ordered fct L 1(0) FePt peaks start to appear at 320 °C annealing, (iii) the activation energy of the interdiffusion is 0.8 eV and (iv) ordered fct FePt grains have preferential out-of-plane texture. The magneto-optical Kerr effect and conversion electron Mössbauer spectroscopies are used to study the magnetic properties of the as-deposited and 400 °C annealed multilayers. The magnetic data for the 400 °C annealed sample indicate that the magnetization is at an angle of ∼50° from the plane of the film. PMID:21825468

  8. 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.

  9. 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

  10. 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

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

    NASA Astrophysics Data System (ADS)

    Bein, Benjamin; Hsing, Hsiang-Chun; Callori, Sara J.; Sinsheimer, John; Chinta, Priya V.; Headrick, Randall L.; Dawber, Matthew

    2015-12-01

    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.

  12. In situ X-ray observations of gas porosity interactions with dendritic microstructures during solidification of Al-based alloys

    NASA Astrophysics Data System (ADS)

    Murphy, A. G.; Browne, D. J.; Houltz, Y.; Mathiesen, R. H.

    2016-03-01

    In situ X-radiography solidification experiments were performed on Al-based alloys, using both synchrotron and laboratory-based X-ray sources, in conjunction with a gradient furnace and a newly developed isothermal furnace, respectively. The effect of gas porosity nucleation and growth within the semi-solid mush during both columnar and equiaxed solidification was thereby observed. In all experimental cases examined, gas porosity was observed to nucleate and grow within the field-of-view (FOV) causing various levels of distortion to the semi-solid mush, and thereafter disappearing from the sample leaving no permanent voids within the solidified microstructure. During columnar growth, a single bubble caused severe remelting and destruction of primary trunks leading to secondary fragmentation and evidence of blocking of the columnar front. Equiaxed solidification was performed under microgravity-like conditions with restricted grain motion in the FOV. The degree to which the nucleated gas bubbles affected the surrounding grain structure increased with increasing solid fraction. However, bubble sphericity remained unaffected by apparent solid fraction or grain coherency.

  13. 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.

  14. 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

    2015-01-01

    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

  15. 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.

  16. 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

  17. 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.

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

    DOE PAGESBeta

    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

  19. 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.

  20. Structural changes of polymer-coated microgranules and excipients on tableting investigated by microtomography using synchrotron X-ray radiation.

    PubMed

    Kajihara, Ryusuke; Noguchi, Shuji; Iwao, Yasunori; Suzuki, Yoshio; Terada, Yasuko; Uesugi, Kentaro; Itai, Shigeru

    2015-03-15

    Multiple-unit tablets consisting of polymer-coated microgranules and excipients have a number of advantageous pharmaceutical properties. Polymer-coated microgranules are known to often lose their functionality because of damage to the polymer coating caused by tableting, and the mechanism of polymer coating damage as well as the structural changes of excipients upon tableting had been investigated but without in-situ visualization and quantitative analysis. To elucidate the mechanism of coating damage, the internal structures of multiple-unit tablets were investigated by X-ray computed microtomography using synchrotron X-rays. Cross sectional images of the tablets with sub-micron spatial resolution clearly revealed that void spaces remained around the compressed excipient particles in the tablets containing an excipient composed of cellulose and lactose (Cellactose(®) 80), whereas much smaller void spaces remained in the tablets containing an excipient made of sorbitol (Parteck(®) SI 150). The relationships between the void spaces and the physical properties of the tablets such as hardness and disintegration were investigated. Damage to the polymer coating in tablets was found mainly where polymer-coated microgranules were in direct contact with each other in both types of tablets, which could be attributed to the difference in hardness of excipient particles and the core of the polymer-coated microgranules. PMID:25660069

  1. In Situ Ambient Pressure X-ray Photoelectron Spectroscopy Studies of Lithium-Oxygen Redox Reactions

    NASA Astrophysics Data System (ADS)

    Lu, Yi-Chun; Crumlin, Ethan J.; Veith, Gabriel M.; Harding, Jonathon R.; Mutoro, Eva; Baggetto, Loïc; Dudney, Nancy J.; Liu, Zhi; Shao-Horn, Yang

    2012-10-01

    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.

  2. 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

  3. In situ ambient pressure X-ray photoelectron spectroscopy studies of lithium-oxygen redox reactions.

    PubMed

    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 Li(4+x)Ti(5)O(12)/LiPON/Li(x)V(2)O(5) cell and examine in situ the chemistry of Li-O(2) reaction products on Li(x)V(2)O(5) 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 Li(x)V(2)O(5) while molecular oxygen was reduced to form lithium peroxide on Li(x)V(2)O(5) in the presence of oxygen upon discharge. Interestingly, the oxidation of Li(2)O(2) began at much lower overpotentials (~240 mV) than the charge overpotentials of conventional Li-O(2) 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-O(2) chemistry. PMID:23056907

  4. 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.

  5. 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.

  6. Single-crystal sapphire microstructure for high-resolution synchrotron X-ray monochromators

    DOE PAGESBeta

    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

  7. 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.

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

    PubMed

    Fan, D; Huang, J W; Zeng, X L; Li, Y; E, J C; Huang, J Y; Sun, T; Fezzaa, K; Wang, Z; Luo, S N

    2016-05-01

    We develop a mini gas gun system for simultaneous, single-pulse, x-ray diffraction and imaging under high strain-rate loading at the beamline 32-ID of the Advanced Photon Source. In order to increase the reciprocal space covered by a small-area detector, a conventional target chamber is split into two chambers: a narrowed measurement chamber and a relief chamber. The gas gun impact is synchronized with synchrotron x-ray pulses and high-speed cameras. Depending on a camera's capability, multiframe imaging and diffraction can be achieved. The proof-of-principle experiments are performed on single-crystal sapphire. The diffraction spots and images during impact are analyzed to quantify lattice deformation and fracture; fracture is dominated by splitting cracks followed by wing cracks, and diffraction peaks are broadened likely due to mosaic spread. Our results demonstrate the potential of such multiscale measurements for studying high strain-rate phenomena at dynamic extremes. PMID:27250438

  9. Prospects for compact high-intensity laser synchrotron x-ray and gamma sources

    NASA Astrophysics Data System (ADS)

    Pogorelsky, I. V.

    1997-03-01

    A laser interacting with a relativistic electron beam behaves like a virtual wiggler of an extremely short period equal to half of the laser wavelength. This approach opens a route to relatively compact, high-brightness x-ray sources alternative or complementary to conventional synchrotron light sources. Although not new, the laser synchrotron source (LSS) concept is still waiting for a convincing demonstration. Available at the BNL Accelerator Test Facility (ATF), a high-brightness electron beam and the high-power CO2 laser may be used for prototype LSS demonstration. In a feasible demonstration experiment, 10-GW, 100-ps CO2 laser beam will be brought to a head-on collision with a 10-ps, 0.5-nC, 50 MeV electron bunch. Flashes of collimated 4.7 keV (2.6 Å) x-rays of 10-ps pulse duration, with a flux of ˜1019photons/sec, will be produced via linear Compton backscattering. The x-ray spectrum is tunable proportionally to the e-beam energy. A rational short-term extension of the proposed experiment would be further enhancement of the x-ray flux to the 1022 photons/sec level, after the ongoing ATF CO2 laser upgrade to 5 TW peak power and electron bunch shortening to 3 ps is realized. In the future, exploiting the promising approach of a high-gradient laser wake field accelerator, a compact "table-top" LSS of monochromatic gamma radiation may become feasible.

  10. 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

  11. 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. PMID:27505829

  12. 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

  13. 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

  14. Reference-free total reflection X-ray fluorescence analysis of semiconductor surfaces with synchrotron radiation.

    PubMed

    Beckhoff, Burkhard; Fliegauf, Rolf; Kolbe, Michael; Müller, Matthias; Weser, Jan; Ulm, Gerhard

    2007-10-15

    Total reflection X-ray fluorescence (TXRF) analysis is a well-established method to monitor lowest level contamination on semiconductor surfaces. Even light elements on a wafer surface can be excited effectively when using high-flux synchrotron radiation in the soft X-ray range. To meet current industrial requirements in nondestructive semiconductor analysis, the Physikalisch-Technische Bundesanstalt (PTB) operates dedicated instrumentation for analyzing light element contamination on wafer pieces as well as on 200- and 300-mm silicon wafer surfaces. This instrumentation is also suited for grazing incidence X-ray fluorescence analysis and conventional energy-dispersive X-ray fluorescence analysis of buried and surface nanolayered structures, respectively. The most prominent features are a high-vacuum load-lock combined with an equipment front end module and a UHV irradiation chamber with an electrostatic chuck mounted on an eight-axis manipulator. Here, the entire surface of a 200- or a 300-mm wafer can be scanned by monochromatized radiation provided by the plane grating monochromator beamline for undulator radiation in the PTB laboratory at the electron storage ring BESSY II. This beamline provides high spectral purity and high photon flux in the range of 0.078-1.86 keV. In addition, absolutely calibrated photodiodes and Si(Li) detectors are used to monitor the exciting radiant power respectively the fluorescence radiation. Furthermore, the footprint of the excitation radiation at the wafer surface is well-known due to beam profile recordings by a CCD during special operation conditions at BESSY II that allow for drastically reduced electron beam currents. Thus, all the requirements of completely reference-free quantitation of TXRF analysis are fulfilled and are to be presented in the present work. The perspectives to arrange for reference-free quantitation using X-ray tube-based, table-top TXRF analysis are also addressed. PMID:17880182

  15. Iron overload of human colon adenocarcinoma cells studied by synchrotron-based X-ray techniques.

    PubMed

    Mihucz, Victor G; Meirer, Florian; Polgári, Zsófia; Réti, Andrea; Pepponi, Giancarlo; Ingerle, Dieter; Szoboszlai, Norbert; Streli, Christina

    2016-04-01

    Fast- and slow-proliferating human adenocarcinoma colorectal cells, HT-29 and HCA-7, respectively, overloaded with transferrin (Tf), Fe(III) citrate, Fe(III) chloride and Fe(II) sulfate were studied by synchrotron radiation total-reflection X-ray spectrometry (TXRF), TXRF-X-ray absorption near edge structure (TXRF-XANES), and micro-X-ray fluorescence imaging to obtain information on the intracellular storage of overloaded iron (Fe). The determined TfR1 mRNA expression for the investigated cells correlated with their proliferation rate. In all cases, the Fe XANES of cells overloaded with inorganic Fe was found to be similar to that of deliquescent Fe(III) sulfate characterized by a distorted octahedral geometry. A fitting model using a linear combination of the XANES of Tf and deliquescent Fe(III) sulfate allowed to explain the near edge structure recorded for HT-29 cells indicating that cellular overload with inorganic Fe results in a non-ferritin-like fast Fe storage. Hierarchical cluster analysis of XANES spectra recorded for Fe overloaded HT-29 and HCA-7 cells was able to distinguish between Fe treatments performed with different Fe species with a 95 % hit rate, indicating clear differences in the Fe storage system. Micro-X-ray fluorescence imaging of Fe overloaded HT-29 cells revealed that Fe is primarily located in the cytosol of the cells. By characterizing the cellular Fe uptake, Fe/S content ratios were calculated based on the X-ray fluorescence signals of the analytes. These Fe/S ratios were dramatically lower for HCA-7 treated with organic Fe(III) treatments suggesting dissimilarities from the Tf-like Fe uptake. PMID:26759251

  16. 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.

  17. In-situ non-ambient X-ray diffraction studies of indium tungstate

    SciTech Connect

    Baiz, Tamam I.; Heinrich, Christophe P.; Banek, Nathan A.; Vivekens, Boris L.; Lind, Cora

    2012-03-15

    In situ variable temperature and high pressure X-ray diffraction studies were carried out on indium tungstate (In{sub 2}W{sub 3}O{sub 12}). This material displays positive volume expansion in both its low temperature monoclinic and high temperature orthorhombic phases, with negative thermal expansion along the a axis and positive thermal expansion along the b and c axes. Upon hydrostatic compression in a diamond anvil cell, one crystalline to crystalline phase transition is observed in the range 1.9 to 2.7 GPa, and progressive irreversible amorphization occurs at pressures above 4.3 GPa. The crystalline high pressure phase appears to be isostructural to previously observed high pressure phases in other A{sub 2}M{sub 3}O{sub 12} compounds. - Graphical abstract: Variable pressure X-ray diffraction patterns of In{sub 2}W{sub 3}O{sub 12} collected in a diamond anvil cell. A phase transition is clearly observed between 2.2 and 2.7 GPa, followed by irreversible amorphization. Highlights: Black-Right-Pointing-Pointer The structure of In{sub 2}W{sub 3}O{sub 12} was studied as a function of temperature and pressure. Black-Right-Pointing-Pointer Uniaxial negative thermal expansion was observed above 250 Degree-Sign C. Black-Right-Pointing-Pointer A pressure-induced phase transition occurred between 2.2 and 2.7 GPa. Black-Right-Pointing-Pointer Pressure-induced irreversible amorphization was observed above 4.3 GPa.

  18. Probing deformation substructure by synchrotron X-ray diffraction and dislocation dynamics modelling.

    PubMed

    Korsunsky, Alexander M; Hofmann, Felix; Song, Xu; Eve, Sophie; Collins, Steve P

    2010-09-01

    Materials characterization at the nano-scale is motivated by the desire to resolve the structural aspects and deformation behavior at length scales relevant to those mechanisms that define the novel and unusual properties of nano-structured materials. A range of novel techniques has recently become accessible with the help of synchrotron X-ray beams that can be focused down to spot sizes of less than a few microns on the sample. The unique combination of tunability (energy selection), parallelism and brightness of synchrotron X-ray beams allows their use for high resolution diffraction (determination of crystal structure and transformations, analysis of dislocation sub-structures, orientation and texture analysis, strain mapping); small angle X-ray scattering (analysis of nano-scale voids and defects; orientation analysis) and imaging (radiography and tomography). After a brief review of the state-of-the-art capabilities for monochromatic and white beam synchrotron diffraction, we consider the usefulness of these techniques for the task of bridging the gap between experiment and modeling. Namely, we discuss how the experiments can be configured to provide information relevant to the validation and improvement of modeling approaches, and also how the results of various simulations can be post-processed to improve the possibility of (more or less) direct comparison with experiments. Using the example of some recent experiments carried out on beamline 116 at Diamond Light Source near Oxford, we discuss how such experimental results can be interpreted in view and in conjunction with numerical deformation models, particularly those incorporating dislocation effects, e.g., finite-element based pseudo-continuum strain gradient formulations, and discrete dislocation simulations. Post-processing of FE and discrete dislocation simulations is described, illustrating the kind of information that can be extracted from comparisons between modeling and experimental data. PMID

  19. 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.

  20. 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.

  1. 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.

  2. The live lattices become visible in coherent synchrotron X-rays

    NASA Astrophysics Data System (ADS)

    Kohn, V.; Rau, C.; Sergienko, P. M.; Snigireva, I.; Snigirev, A.; Vazina, A.

    2005-05-01

    We demonstrate a great potential of the method of phase contrast imaging for a study of muscles and animal organism in normal and pathological states. The method is applied to image biological tissues that have the unique feature of structure-translation symmetry of 0.1-10 μm periodicity. The cross-striated muscle is the most interesting example of such objects. The experiment was done using high-brilliant coherent X-rays, delivered by synchrotron radiation source of third generation (ESRF, Grenoble), and high-resolution 2D-detector.

  3. Synchrotron total reflection X-ray fluorescence at BL-16 microfocus beamline of Indus-2

    NASA Astrophysics Data System (ADS)

    Tiwari, M. K.; Singh, A. K.; Das, Gangadhar; Chowdhury, Anupam; Lodha, G. S.

    2014-04-01

    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.

  4. 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.

  5. 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.

  6. Porosity characterization of fiber-reinforced ceramic matrix composite using synchrotron X-ray computed tomography

    NASA Astrophysics Data System (ADS)

    Zou, C.; Marrow, T. J.; Reinhard, C.; Li, B.; Zhang, C.; Wang, S.

    2016-03-01

    The pore structure and porosity of a continuous fiber reinforced ceramic matrix composite has been characterized using high-resolution synchrotron X-ray computed tomography (XCT). Segmentation of the reconstructed tomograph images reveals different types of pores within the composite, the inter-fiber bundle open pores displaying a "node-bond" geometry, and the intra-fiber bundle isolated micropores showing a piping shape. The 3D morphology of the pores is resolved and each pore is labeled. The quantitative filtering of the pores measures a total porosity 8.9% for the composite, amid which there is about 7.1~ 9.3% closed micropores.

  7. 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.

  8. 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.

  9. Synchrotron x-ray nano-tomography characterization of the sintering of multilayered systems

    NASA Astrophysics Data System (ADS)

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

    2012-06-01

    Synchrotron x-ray nano-tomography was used to characterize the microstructures of multi-layer ceramic capacitors before and after sintering. 3D microstructures of the same sample were reconstructed and quantitatively analyzed. The discontinuities observed in inner electrodes were found to originate from initial heterogeneities of nickel powders in the electrodes. They are supposed to grow due to the constraint of adjacent dielectric layers. Dielectric layers show anisotropic shrinkage with a decrease in density as function of layer position in the multilayer.

  10. Poly (methyl methacrylate) Formation and Patterning Initiated by Synchrotron X-ray Illumination

    SciTech Connect

    Xiao, J.; Je, J. H.; Wang, C. H.; Yang, T. Y.; Hwu, Y.

    2007-01-19

    A facile radiation method was developed to obtain micro-sized poly (methyl methacrylate) (PMMA) particles and create patterned coating on different substrates by a synchrotron x-ray induced dispersion polymerization. The polymerization of MMA monomer and well defined patterning was successfully realized. The produced PMMA particles and patterning were characterized by Fourier transformation infrared (FTIR), 1H-Nuclear Magnetic Resonance (NMR), and Scanning Electron Microscope (SEM). The observed patterning contrast essentially derived from a variation of size, density and morphology of particles and the type of substrate materials used.

  11. 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.

  12. A low-cost X-ray-transparent experimental cell for synchrotron-based X-ray microtomography studies under geological reservoir conditions.

    PubMed

    Fusseis, Florian; Steeb, Holger; Xiao, Xianghui; Zhu, Wen-lu; Butler, Ian B; Elphick, Stephen; Mäder, Urs

    2014-01-01

    A new modular X-ray-transparent experimental cell enables tomographic investigations of fluid rock interaction under natural reservoir conditions (confining pressure up to 20 MPa, pore fluid pressure up to 15 MPa, temperature ranging from 296 to 473 K). The portable cell can be used at synchrotron radiation sources that deliver a minimum X-ray flux density of 10(9) photons mm(-2) s(-1) in the energy range 30-100 keV to acquire tomographic datasets in less than 60 s. It has been successfully used in three experiments at the bending-magnet beamline 2BM at the Advanced Photon Source. The cell can be easily machined and assembled from off-the-shelf components at relatively low costs, and its modular design allows it to be adapted to a wide range of experiments and lower-energy X-ray sources. PMID:24365944

  13. 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

  14. 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

  15. In situ identification of the metastable phase during solidification from the undercooled YFeO3 melt by fast x-ray diffractometry at 250 Hz

    NASA Astrophysics Data System (ADS)

    Nagashio, K.; Kuribayashi, K.; Vijaya Kumar, M. S.; Niwata, K.; Hibiya, T.; Mizuno, A.; Watanabe, M.; Katayama, Y.

    2006-12-01

    A time-resolved x-ray diffraction (XRD) experiment at 250Hz using a synchrotron radiation source was carried out during the containerless solidification of ReFeO3 (Re =Y and Lu) in order to identify the metastable phase in situ. The metastable phase solidified primarily from the undercooled YFeO3 melt finally transformed to the stable orthorhombic YFeO3 phase during the short period of recalescence (˜0.035s ). Although the metastable phase could not be detected in the as-solidified sample by the powder XRD, the in situ diffraction pattern of the metastable phase in the YFeO3 system was consistent with that of the metastable hexagonal LuFeO3 phase.

  16. Atomic and electronic aspects of the coloration mechanism of gasochromic Pt/Mo-modified V2O5 smart films: an in situ X-ray spectroscopic study.

    PubMed

    Lu, Ying-Rui; Hsu, Hsin-Hua; Chen, Jeng-Lung; Chang, Han-Wei; Chen, Chi-Liang; Chou, Wu-Ching; Dong, Chung-Li

    2016-02-21

    In this work, gasochromic pristine and Mo-modified V2O5 thin films were prepared by the sol-gel spin coating method. Both films exhibit excellent gasochromic coloration. Synchrotron grazing incidence X-ray diffraction reveals that the Mo-modified V2O5 thin film is more amorphous than the pristine V2O5 thin film. X-ray absorption spectroscopy (XAS) was utilized to elucidate the modifications of the local electronic and atomic structures that are caused by Mo. In situ soft-XAS and in situ hard-XAS were performed to monitor the effect of the adsorption of dihydrogen on the charge state of vanadium and local atomic rearrangement in the gasochromic thin films. The gasochromic V2O5 film has a significantly pyramid-like oxygen-coordinated environment. However, the Mo-modified film exhibits mixed pyramid- and octahedral-like structures. Analytic results indicate that upon gasochromic coloration, adsorption of hydrogen adds electrons to the V 3d t2g orbital, lowering the charge state of vanadium. The films undergo structural modification before the valence is changed. The Mo-modified V2O5 film exhibits faster coloration because the apical V-O bond differs from that in the pristine V2O5 film. This in situ XAS allows real-time monitoring of changes in the element-specific local atomic structure during the gasochromic reaction and enables the elucidation of the gasochromic mechanism. PMID:26813863

  17. 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.

  18. The rf system of the Synchrotron X-ray Source at Argonne

    SciTech Connect

    Kustom, R.L.; Mavrogenes, G.; Nicholls, G.

    1987-01-01

    A Positron Storage Ring for the Synchrotron X-ray Source at Argonne is under design. The rf system is described. The rf system is divided into four stations, each using a one-megawatt klystron to excite four single-cell spherical cavities to a gap voltage of 761 kV at the operating frequency of 350.8 MHz. The same klystron also provides the beam power for synchrotron radiation losses of the position beam of up to 300 mA, the higher-order-mode power losses, the power losses in the beam due to the insertion devices, and the rf power transmission losses. The transmission waveguide system includes magic tees for splitting the power of each klystron to four cavities, isolators to protect the klystrons, harmonic and higher-order-mode absorbers, and mechanical phase shifters for fine phase tuning.

  19. 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.

  20. 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.