WorldWideScience

Sample records for situ x-ray study

  1. In Situ Ptychography of Heterogeneous Catalysts using Hard X-Rays

    DEFF Research Database (Denmark)

    Baier, Sina; Damsgaard, Christian Danvad; Scholz, Maria

    2016-01-01

    A new closed cell is presented for in situ X-ray ptychography which allows studies under gas flow and at elevated temperature. In order to gain complementary information by transmission and scanning electron microscopy, the cell makes use of a Protochips E-chipTM which contains a small, thin...... the same sample holder for ex situ electron microscopy before and after the in situ study underlines the unique possibilities available with this combination of electron microscopy and X-ray microscopy on the same sample....

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

    Science.gov (United States)

    Takahasi, Masamitu

    2018-05-01

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

  3. Capillary based Li-air batteries for in situ synchrotron X-ray powder diffraction studies

    DEFF Research Database (Denmark)

    Storm, Mie Møller; Johnsen, Rune E.; Younesi, Reza

    2015-01-01

    For Li-air batteries to reach their full potential as energy storage system, a complete understanding of the conditions and reactions in the battery during operation is needed. To follow the reactions in situ a capillary-based Li-O2 battery has been developed for synchrotron-based in situ X......-ray powder diffraction (XRPD). In this article, we present the results for the analysis of 1st and 2nd deep discharge and charge for a cathode being cycled between 2 and 4.6 V. The crystalline precipitation of Li2O2 only is observed in the capillary battery. However, there are indications of side reactions...... of constant exposure of X-ray radiation to the electrolyte and cathode during charge of the battery was also investigated. X-ray exposure during charge leads to changes in the development of the intensity and the FWHM of the Li2O2 diffraction peaks. The X-ray diffraction results are supported by ex situ X...

  4. In situ synchrotron X-ray studies during metal-organic chemical vapor deposition of semiconductors

    Energy Technology Data Exchange (ETDEWEB)

    Thompson, Carol [Northern Illinois Univ., DeKalb, IL (United States); Argonne National Lab., Argonne, IL (United States); Highland, Matthew J.; Perret, Edith; Fuoss, Paul H.; Streiffer, Stephen K.; Stephenson, G. Brian [Argonne National Lab., Argonne, IL (United States); Richard, Marie-Ingrid [Universite Paul Cezanne Aix-Marseille, Marseille (France)

    2012-07-01

    In-situ, time-resolved techniques provide valuable insight into the complex interplay of surface structural and chemical evolution occurring during materials synthesis and processing of semiconductors. Our approach is to observe the evolution of surface structure and morphology at the atomic scale in real-time during metal organic vapor phase deposition (MOCVD) by using grazing incidence x-ray scattering and X-ray fluorescence, coupled with visible light scattering. Our vertical-flow MOCVD chamber is mounted on a 'z-axis' surface diffractometer designed specifically for these studies of the film growth, surface evolution and the interactions within a controlled growth environment. These techniques combine the ability of X-rays to penetrate a complex environment for measurements during growth and processing, with the sensitivity of surface scattering techniques to atomic and nanoscale structure. In this talk, we outline our program and discuss examples from our in-situ and real-time X-ray diffraction and fluorescence studies of InN, GaN, and InGaN growth on GaN(0001).

  5. In-Situ Synchrotron X-ray Study of the Phase and Texture Evolution of Ceria and Superconductor Films Deposited by Chemical Solution Method

    DEFF Research Database (Denmark)

    Yue, Zhao; Grivel, Jean-Claude; He, Dong

    2012-01-01

    In situ synchrotron x-ray diffraction is used to study the phase and texture formation of ceria based films and superconductor films deposited by the chemical solution method on technical substrates. Combined analysis using in situ synchrotron x-ray diffraction, thermogravimetry/differential ther......In situ synchrotron x-ray diffraction is used to study the phase and texture formation of ceria based films and superconductor films deposited by the chemical solution method on technical substrates. Combined analysis using in situ synchrotron x-ray diffraction, thermogravimetry...

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

    International Nuclear Information System (INIS)

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

    2014-01-01

    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.

  7. The adsorption of methanol and water on SAPO-34: in situ and ex situ X-ray diffraction studies

    DEFF Research Database (Denmark)

    Wragg, David S.; Johnsen, Rune; Norby, Poul

    2010-01-01

    The adsorption of methanol on SAPO-34 has been studied using a combination of in situ synchrotron powder X-ray diffraction to follow the process and ex situ high resolution powder diffraction to determine the structure. The unit cell volume of SAPO-34 is found to expand by 0.5% during methanol ad...

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

    Science.gov (United States)

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

    2007-11-01

    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 (LN2) temperature sample cooling unit is installed. The snapshots of growth of particles with fluence of 90MeV Ni ions were recorded using in situ XRD experiment, illustrating the potential of this in situ facility. A thin film of C60 was used to test the sample cooling unit. It shows that the phase of the C60 film transforms from a cubic lattice (at room temperature) to a fcc lattice at around T =255K.

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

    Science.gov (United States)

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

    2007-11-01

    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 (LN2) 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 C60 was used to test the sample cooling unit. It shows that the phase of the C60 film transforms from a cubic lattice (at room temperature) to a fcc lattice at around T=255 K.

  10. In situ X-ray diffraction studies on the piezoelectric response of PZT thin films

    Energy Technology Data Exchange (ETDEWEB)

    Davydok, A., E-mail: davydok@mpie.de [Aix Marseille Université, CNRS, Université de Toulon, IM2NP UMR 7334, 13397 Marseille (France); Max-Planck-Institut für Eisenforschung, Department Structure and Nano-/Micromechanics of Materials, D-40237 Düsseldorf (Germany); Cornelius, T.W. [Aix Marseille Université, CNRS, Université de Toulon, IM2NP UMR 7334, 13397 Marseille (France); Mocuta, C. [SOLEIL Synchrotron, DiffAbs beamline, L' Orme des Merisiers, Saint-Aubin - BP 48, 91192 Gif-sur-Yvette Cedex (France); Lima, E.C. [Universidade Federal do Tocantins, 77500-000 Porto Nacional, TO (Brazil); Araujo, E.B. [Departamento de Fisica e Quimica, Universidade Estadual Paulista, Av. Brasil, 56 Centro, 15385-000 Ilha Solteira, SP (Brazil); Thomas, O. [Aix Marseille Université, CNRS, Université de Toulon, IM2NP UMR 7334, 13397 Marseille (France)

    2016-03-31

    Piezoelectric properties of randomly oriented self-polarized PbZr{sub 0.50}Ti{sub 0.50}O{sub 3} (PZT) thin films were investigated using in situ synchrotron X-ray diffraction. Possibilities for investigating the piezoelectric effect using micro-sized hard X-ray beams are demonstrated and perspectives for future dynamical measurements on PZT samples with variety of compositions and thicknesses are given. Studies performed on the crystalline [100, 110] directions evidenced piezoelectric anisotropy. The piezoelectric coefficient d{sub 33} was calculated in terms of the lab reference frame (d{sub perp}) and found to be two times larger along the [100] direction than along the [110] direction. The absolute values for the d{sub perp} amount to 120 and 230 pm/V being in good agreement with experimental and theoretical values found in literature for bulk PZT ceramics. - Highlights: • We performed in situ synchrotron X-ray diffraction studies on (PZT) thin films. • We discuss anisotropy of piezo effect in different crystallographic directions. • Perpendicular component Piezo coefficient of thin PZT layer is defined.

  11. In Situ X-ray Diffraction Studies of Cathode Materials in Lithium Batteries

    International Nuclear Information System (INIS)

    Yang, X. Q.; Sun, X.; McBreen, J.; Mukerjee, S.; Gao, Yuan; Yakovleva, M. V.; Xing, X. K.; Daroux, M. L.

    1998-01-01

    There is an increasing interest in lithiated transition metal oxides because of their use as cathodes in lithium batteries. LiCoO 2 , LiNiO 2 and LiMn 2 O 4 are the three most widely used and studied materials, At present, although it is relative expensive and toxic, LiCoO 2 is the material of choice in commercial lithium ion batteries because of its ease of manufacture, better thermal stability and cycle life. However, the potential use of lithium ion batteries with larger capacity for power tools and electric vehicles in the future will demand new cathode materials with higher energy density, lower cost and better thermal stability. LiNiO 2 is isostructural with LiCoO 2 . It offers lower cost and high energy density than LiCoO 2 . However, it has much poorer thermal stability than LiCoO 2 , in the charged (delithiated) state. Co, Al, and other elements have been used to partially replace Ni in LiNiO 2 system in order to increase the thermal stability. LiMn 2 O 4 has the highest thermal stability and lowest cost and toxicity. However, the low energy density and poor cycle life at elevated temperature are the major obstacles for this material. In order to develop safer, cheaper, and better performance cathode materials, the in-depth understanding of the relationships between the thermal stability and structure, performance and structure are very important. The performance here includes energy density and cycle life of the cathode materials. X-ray diffraction (XRD) is one of the most powerful tools to study these relationships. The pioneer ex situ XRD work on cathode materials for lithium batteries was done by Ohzuku. His XRD studies on LiMn 2 O 4 , LiCoO 2 , LiNiO 2 , LiNi 0.5 Co 0.5 O 2 , and LiAl x Ni 1-x O 2 cathodes at different states of charge have provided important guidelines for the development of these new materials. However, the kinetic nature of the battery system definitely requires an in situ XRD technique to study the detail structural changes of the

  12. In Situ X-ray Diffraction Studies of (De)lithiation Mechanism in Silicon Nanowire Anodes

    KAUST Repository

    Misra, Sumohan; Liu, Nian; Nelson, Johanna; Hong, Seung Sae; Cui, Yi; Toney, Michael F.

    2012-01-01

    -Si product has been observed. In this work, we use an X-ray transparent battery cell to perform in situ synchrotron X-ray diffraction on SiNWs in real time during electrochemical cycling. At deep lithiation voltages the known metastable Li 15Si 4 phase forms

  13. In situ X-ray studies of film cathodes for solid oxide fuel cells

    International Nuclear Information System (INIS)

    Fuoss, Paul; Chang, Kee-Chul; You, Hoydoo

    2013-01-01

    Highlights: •Synchrotron X-rays are used to study in operando the structural and chemical changes of LSM and LSCF film cathodes during half-cell operations. •A-site and B-site cations actively segregate or desegregate on the changes of temperature, pO 2 , and electrochemical potential. •Chemical lattice expansions show that oxygen-cathode interface is the primary source of rate-limiting processes. •The surface and subsurface of the LSM and LSCF films have different oxidation-states due to vacancy concentration changes. •Liquid-phase infiltration and coarsening processes of cathode materials into porous YSZ electrolyte backbone were monitored by USAXS. -- Abstract: Synchrotron-based X-ray techniques have been used to study in situ the structural and chemical changes of film cathodes during half-cell operations. The X-ray techniques used include X-ray reflectivity (XR), total-reflection X-ray fluorescence (TXRF), high-resolution diffraction (HRD), ultra-small angle X-ray scattering (USAXS). The epitaxial thin film model cathodes for XR, TXRF, and HRD measurements are made by pulse laser deposition and porous film cathodes for USAX measurements are made by screen printing technique. The experimental results reviewed here include A-site and B-site segregations, lattice expansion, oxidation-state changes during cell operations and liquid-phase infiltration and coarsening of cathode to electrolyte backbone

  14. In situ x-ray reflectivity and grazing incidence x-ray diffraction study of L 1{sub 0} ordering in {sup 57}Fe/Pt multilayers

    Energy Technology Data Exchange (ETDEWEB)

    Raghavendra Reddy, V; Gupta, Ajay; Gome, Anil [UGC-DAE Consortium for Scientific Research, University Campus, Khandwa Road, Indore-452 017 (India); Leitenberger, Wolfram [Institute of Physics, University of Potsdam, 14469 Potsdam (Germany); Pietsch, U [Physics Department, University of Siegen, D-57068 Siegen (Germany)], E-mail: vrreddy@csr.ernet.in, E-mail: varimalla@yahoo.com

    2009-05-06

    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{sub 0} phase formation in [Fe(19 A)/Pt(25 A)]{sub x 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{sub 0} phase, (ii) the ordered fct L 1{sub 0} FePt peaks start to appear at 320 deg. 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 Moessbauer spectroscopies are used to study the magnetic properties of the as-deposited and 400 deg. C annealed multilayers. The magnetic data for the 400 {sup 0}C annealed sample indicate that the magnetization is at an angle of {approx}50 deg. from the plane of the film.

  15. A flexible gas flow reaction cell for in situ x-ray absorption spectroscopy studies

    Energy Technology Data Exchange (ETDEWEB)

    Kroner, Anna B., E-mail: anna.kroner@diamond.ac.uk; Gilbert, Martin; Duller, Graham; Cahill, Leo; Leicester, Peter; Woolliscroft, Richard; Shotton, Elizabeth J. [Diamond Light Source Ltd., Diamond House, Harwell Science and Innovation Campus, Chilton, Oxfordshire, OX110DE (United Kingdom); Mohammed, Khaled M. H. [UK Catalysis Hub, Research Complex at Harwell, Rutherford Appleton Laboratory, Chilton, Oxfordshire, OX110FA (United Kingdom); School of Chemistry, University of Southampton, Southampton, SO17 1BJ (United Kingdom)

    2016-07-27

    A capillary-based sample environment with hot air blower and integrated gas system was developed at Diamond to conduct X-ray absorption spectroscopy (XAS) studies of materials under time-resolved, in situ conditions. The use of a hot air blower, operating in the temperature range of 298-1173 K, allows introduction of other techniques e.g. X-ray diffraction (XRD), Raman spectroscopy for combined techniques studies. The flexibility to use either quartz or Kapton capillaries allows users to perform XAS measurement at energies as low as 5600 eV. To demonstrate performance, time-resolved, in situ XAS results of Rh catalysts during the process of activation (Rh K-edge, Ce L{sub 3}-edge and Cr K-edge) and the study of mixed oxide membrane (La{sub 0.6}Sr{sub 0.4}Co{sub 0.2}Fe{sub 0.8}O{sub 3−δ}) under various partial oxygen pressure conditions are described.

  16. Thermal expansion behavior study of Co nanowire array with in situ x-ray diffraction and x-ray absorption fine structure techniques

    Science.gov (United States)

    Mo, Guang; Cai, Quan; Jiang, Longsheng; Wang, Wei; Zhang, Kunhao; Cheng, Weidong; Xing, Xueqing; Chen, Zhongjun; Wu, Zhonghua

    2008-10-01

    In situ x-ray diffraction and x-ray absorption fine structure techniques were used to study the structural change of ordered Co nanowire array with temperature. The results show that the Co nanowires are polycrystalline with hexagonal close packed structure without phase change up until 700 °C. A nonlinear thermal expansion behavior has been found and can be well described by a quadratic equation with the first-order thermal expansion coefficient of 4.3×10-6/°C and the second-order thermal expansion coefficient of 5.9×10-9/°C. The mechanism of this nonlinear thermal expansion behavior is discussed.

  17. In-situ oxidation study of Pd(100) by surface x-ray diffraction

    Energy Technology Data Exchange (ETDEWEB)

    Kilic, Volkan; Franz, Dirk; Stierle, Andreas [AG Grenzflaechen, Universitaet Siegen (Germany); Martin, Natalia; Lundgren, Edvin [Department of Synchrotron Radiation Research, Lund University (Sweden); Mantilla, Miguel [MPI fuer Metallforschung, Stuttgart (Germany)

    2011-07-01

    The oxidation of the Pd(100) surface at oxygen pressures in the 10{sup -6} mbar to 10{sup 3} mbar range and temperatures up to 1000 K has been studied in-situ by surface x-ray diffraction (SXRD). The SXRD experiments were performed at the MPI beamline at the Angstrom Quelle Karlsruhe (ANKA). We present the surface and crystal truncation rod (CTR) data from the ({radical}(5) x {radical}(5)) surface layer. We show that the transformation from the surface oxide to PdO bulk oxide can be observed in-situ under specific pressure and temperature conditions. We compare our results with previously proposed structure models based on low energy electron diffraction (LEED) I(V) curves and density functional theory calculations. Finally, we elucidate the question of commensurability of the surface oxide layer with respect to the Pd(100) substrate.

  18. Final Report on Developing Microstructure-Property Correlation in Reactor Materials using in situ High-Energy X-rays

    Energy Technology Data Exchange (ETDEWEB)

    Li, Meimei [Argonne National Lab. (ANL), Argonne, IL (United States); Almer, Jonathan D. [Argonne National Lab. (ANL), Argonne, IL (United States); Yang, Yong [Univ. of Florida, Gainesville, FL (United States); Tan, Lizhen [Oak Ridge National Lab. (ORNL), Oak Ridge, TN (United States)

    2016-01-01

    This report provides a summary of research activities on understanding microstructure – property correlation in reactor materials using in situ high-energy X-rays. The report is a Level 2 deliverable in FY16 (M2CA-13-IL-AN_-0403-0111), under the Work Package CA-13-IL-AN_- 0403-01, “Microstructure-Property Correlation in Reactor Materials using in situ High Energy Xrays”, as part of the DOE-NE NEET Program. The objective of this project is to demonstrate the application of in situ high energy X-ray measurements of nuclear reactor materials under thermal-mechanical loading, to understand their microstructure-property relationships. The gained knowledge is expected to enable accurate predictions of mechanical performance of these materials subjected to extreme environments, and to further facilitate development of advanced reactor materials. The report provides detailed description of the in situ X-ray Radiated Materials (iRadMat) apparatus designed to interface with a servo-hydraulic load frame at beamline 1-ID at the Advanced Photon Source. This new capability allows in situ studies of radioactive specimens subject to thermal-mechanical loading using a suite of high-energy X-ray scattering and imaging techniques. We conducted several case studies using the iRadMat to obtain a better understanding of deformation and fracture mechanisms of irradiated materials. In situ X-ray measurements on neutron-irradiated pure metal and model alloy and several representative reactor materials, e.g. pure Fe, Fe-9Cr model alloy, 316 SS, HT-UPS, and duplex cast austenitic stainless steels (CASS) CF-8 were performed under tensile loading at temperatures of 20-400°C in vacuum. A combination of wide-angle X-ray scattering (WAXS), small-angle X-ray scattering (SAXS), and imaging techniques were utilized to interrogate microstructure at different length scales in real time while the specimen was subject to thermal-mechanical loading. In addition, in situ X-ray studies were

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

    Energy Technology Data Exchange (ETDEWEB)

    Lee, J. H.; Freeland, J. W.; Hong, Hawoong, E-mail: hhong@aps.anl.gov [Advanced Photon Source, Argonne National Laboratory, Argonne, Illinois 60439 (United States); Tung, I. C. [Advanced Photon Source, Argonne National Laboratory, Argonne, Illinois 60439 (United States); Department of Materials Science and Engineering, Northwestern University, Evanston, Illinois 60208 (United States); Chang, S.-H.; Bhattacharya, A.; Fong, D. D. [Materials Science Division, Argonne National Laboratory, Argonne, Illinois 60439 (United States)

    2016-01-15

    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.

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

    International Nuclear Information System (INIS)

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

    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

  1. A Next-Generation Hard X-Ray Nanoprobe Beamline for In Situ Studies of Energy Materials and Devices

    Science.gov (United States)

    Maser, Jörg; Lai, Barry; Buonassisi, Tonio; Cai, Zhonghou; Chen, Si; Finney, Lydia; Gleber, Sophie-Charlotte; Jacobsen, Chris; Preissner, Curt; Roehrig, Chris; Rose, Volker; Shu, Deming; Vine, David; Vogt, Stefan

    2014-01-01

    The Advanced Photon Source is developing a suite of new X-ray beamlines to study materials and devices across many length scales and under real conditions. One of the flagship beamlines of the APS upgrade is the In Situ Nanoprobe (ISN) beamline, which will provide in situ and operando characterization of advanced energy materials and devices under varying temperatures, gas ambients, and applied fields, at previously unavailable spatial resolution and throughput. Examples of materials systems include inorganic and organic photovoltaic systems, advanced battery systems, fuel cell components, nanoelectronic devices, advanced building materials and other scientifically and technologically relevant systems. To characterize these systems at very high spatial resolution and trace sensitivity, the ISN will use both nanofocusing mirrors and diffractive optics to achieve spots sizes as small as 20 nm. Nanofocusing mirrors in Kirkpatrick-Baez geometry will provide several orders of magnitude increase in photon flux at a spatial resolution of 50 nm. Diffractive optics such as zone plates and/or multilayer Laue lenses will provide a highest spatial resolution of 20 nm. Coherent diffraction methods will be used to study even small specimen features with sub-10 nm relevant length scale. A high-throughput data acquisition system will be employed to significantly increase operations efficiency and usability of the instrument. The ISN will provide full spectroscopy capabilities to study the chemical state of most materials in the periodic table, and enable X-ray fluorescence tomography. In situ electrical characterization will enable operando studies of energy and electronic devices such as photovoltaic systems and batteries. We describe the optical concept for the ISN beamline, the technical design, and the approach for enabling a broad variety of in situ studies. We furthermore discuss the application of hard X-ray microscopy to study defects in multi-crystalline solar cells, one

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

    Science.gov (United States)

    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.

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

    International Nuclear Information System (INIS)

    Eveno, Myriam; Duran, Adrian; Castaing, Jacques

    2010-01-01

    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. (orig.)

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

    Energy Technology Data Exchange (ETDEWEB)

    Chakraborty, R., E-mail: rupak@alum.mit.edu, E-mail: buonassisi@mit.edu; Serdy, J.; Culpepper, M. L.; Buonassisi, T., E-mail: rupak@alum.mit.edu, E-mail: buonassisi@mit.edu [Department of Mechanical Engineering, Massachusetts Institute of Technology, Cambridge, Massachusetts 02139 (United States); West, B.; Stuckelberger, M.; Bertoni, M. I. [School of Electrical, Computer and Energy Engineering, Arizona State University, Tempe, Arizona 85287 (United States); Lai, B.; Maser, J. [Advanced Photon Source, Argonne National Laboratory, Argonne, Illinois 60439 (United States)

    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.

  5. The Oxford-Diamond In Situ Cell for studying chemical reactions using time-resolved X-ray diffraction

    Science.gov (United States)

    Moorhouse, Saul J.; Vranješ, Nenad; Jupe, Andrew; Drakopoulos, Michael; O'Hare, Dermot

    2012-08-01

    A versatile, infrared-heated, chemical reaction cell has been assembled and commissioned for the in situ study of a range of chemical syntheses using time-resolved energy-dispersive X-ray diffraction (EDXRD) on Beamline I12 at the Diamond Light Source. Specialized reactor configurations have been constructed to enable in situ EDXRD investigation of samples under non-ambient conditions. Chemical reactions can be studied using a range of sample vessels such as alumina crucibles, steel hydrothermal autoclaves, and glassy carbon tubes, at temperatures up to 1200 °C.

  6. In situ x-ray diffraction studies of three-dimensional C60 polymers

    International Nuclear Information System (INIS)

    Wood, R A; Lewis, M H; Bennington, S M; Cain, M G; Kitamura, N; Fukumi, A K

    2002-01-01

    In situ investigations into the P/T field of C 60 fullerene were performed using energy-dispersive x-ray diffraction techniques. Isobars were obtained at 11 and 9 GPa accompanied by isotherms at 750 and 800 K with pressure reaching 13 GPa. The P/T history and pressure isotropy were investigated with the aim of optimizing conditions for 3D polymer formation. Confirmation of the formation of 3D polymers was performed in situ; however, the reclaimed sample did not exhibit the expected high hardness value, due to depolymerization on pressure release. Isotropy in the pressure field promoted formation and retention of the face-centred-cubic structure

  7. Electrochemical cell for in situ x-ray diffraction under ultrapure conditions

    DEFF Research Database (Denmark)

    Koop, T.; Schindler, W.; Kazimirov, A.

    1998-01-01

    within a few seconds. The oxygen level in the electrolyte is reduced by continuous N(2) flow to less than 0.2% compared to that of a fresh electrolyte. This can be done while rotating the cell by 360 degrees about the surface normal. The electrode potential is accurately measured at the position......An electrochemical cell has been developed for in situ x-ray diffraction from a working electrode under clean conditions equivalent to ultrahigh vacuum conditions of 5 x 10(-10) mbar. The substrate crystals can be prepared ex situ and transferred into the cell under protection of ultrapure water...... of the crystal using a Luggin capillary and a standard reference electrode. We demonstrate the performance of our cell by in situ synchrotron x-ray diffraction measurements on ultrathin Co layers electrodeposited on Cu(001) in an aqueous H(2)SO(4)/CoSO(4) solution. (C) 1998 American Institute of Physics....

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

    Science.gov (United States)

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

    2017-09-01

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

  9. Combining X-ray Absorption and X-ray Diffraction Techniques for in Situ Studies of Chemical Transformations in Heterogeneous Catalysis: Advantages and Limitations

    International Nuclear Information System (INIS)

    Frenkel, A.I.; Hanson, J.; Wang, Q.; Marinkovic, N.; Chen, J.G.; Barrio, L.; Si, R.; Lopez Camara, A.; Estrella, A.M.; Rodriguez, J.A.

    2011-01-01

    Recent advances in catalysis instrumentations include synchrotron-based facilities where time-resolved X-ray scattering and absorption techniques are combined in the same in situ or operando experiment to study catalysts at work. To evaluate the advances and limitations of this method, we performed a series of experiments at the new XAFS/XRD instrument in the National Synchrotron Light Source. Nearly simultaneous X-ray diffraction (XRD) and X-ray absorption fine-structure (XAFS) measurements of structure and kinetics of several catalysts under reducing or oxidizing conditions have been performed and carefully analyzed. For CuFe 2 O 4 under reducing conditions, the combined use of the two techniques allowed us to obtain accurate data on kinetics of nucleation and growth of metallic Cu. For the inverse catalyst CuO/CeO 2 that underwent isothermal reduction (with CO) and oxidation (with O 2 ), the XAFS data measured in the same experiment with XRD revealed strongly disordered Cu species that went undetected by diffraction. These and other examples emphasize the unique sensitivity of these two complementary methods to follow catalytic processes in the broad ranges of length and time scales.

  10. In-situ x-ray absorption study of copper films in ground water solutions

    International Nuclear Information System (INIS)

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

    2007-01-01

    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 HCO 3 - 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 3 - prevented or slowed down the corrosion processes

  11. A study of the reactivity of elemental Cr/Se/Te thin multilayers using X-ray reflectometry, in situ X-ray diffraction and X-ray absorption spectroscopy

    International Nuclear Information System (INIS)

    Behrens, Malte; Tomforde, Jan; May, Enno; Kiebach, Ragnar; Bensch, Wolfgang; Haeussler, Dietrich; Jaeger, Wolfgang

    2006-01-01

    The reactivity of [Cr/Se/Te] multilayers under annealing was investigated using X-ray reflectometry, in situ X-ray diffraction, X-ray absorption fine structure (XAFS) measurements and transmission electron microscopy. For all samples, interdiffusion was complete at temperatures between 100 and 300 deg. C, depending on the repeating tri-layer thickness. A crystalline phase nucleated approximately 20 deg. C above the temperature where interdiffusion was finished. The first crystalline phase in a binary Cr/Te sample was layered CrTe 3 nucleating at 230 deg. C. In ternary samples (Se:Te=0.6-1.2), the low-temperature nucleation of such a layered CrQ 3 (Q=Se, Te) phase is suppressed and instead the phase Cr 2 Q 3 nucleates first. Interestingly, this phase decomposes around 500 deg. C into layered CrQ 3 . In contrast, binary Cr/Se samples form stable amorphous alloys after interdiffusion and Cr 3 Se 4 nucleates around 500 deg. C as the only crystalline phase. Evaluation of the XAFS data of annealed samples yield Se-Cr distances of 2.568(1) and 2.552(1) A for Cr 2 Q 3 and CrQ 3 , respectively. In the latter sample, higher coordination shells around Se are seen accounting for the Se-Te contacts in the structure. - Graphical abstract: The first step of the reaction of elemental Cr/Te/Se-multilayers is the interdiffusion of the elements as evidenced by the decay of the modulation peaks in the low-angle region of the X-ray diffraction patterns. The subsequent growth of Bragg peaks at higher scattering angles indicates crystallization of chromium chalcogenide Cr 2 Te 3- x Se x

  12. Ex-situ time-lapse x-ray CT study of 3D micro-structural fatigue damage evolution in uni-directional composites

    DEFF Research Database (Denmark)

    Jespersen, Kristine Munk; Wang, Ying; Zangenberg Hansen, Jens

    2016-01-01

    In this study, the progress of damage under tension-tension fatigue of a uni-directional (UD) glass fibre composite made from a non-crimp fabric is studied using transilluminated white light imaging (TWLI) and X-ray computed tomography (CT). TWLI images are automatically captured throughout...... to initiate already after the first cycle, whereas some grow gradually and others appear suddenly during cycling. The off-axis cracks are observed to saturate after a few thousand cycles. The UD fibre fracture damage in the region observed by X-ray CT is probably already saturated at the first interruption...... point, as no significant change is seen between the two X-ray images. However, the study indicates how TWLI can be used as an initial indicator to locate damage regions at an early stage for the future ex-situ X-ray CT experiments....

  13. Methodology for studying strain inhomogeneities in polycrystalline thin films during in situ thermal loading using coherent x-ray diffraction

    Energy Technology Data Exchange (ETDEWEB)

    Vaxelaire, N; Labat, S; Thomas, O [Aix-Marseille University, IM2NP, FST avenue Escadrille Normandie Niemen, F-13397 Marseille Cedex (France); Proudhon, H; Forest, S [MINES ParisTech, Centre des materiaux, CNRS UMR 7633, BP 87, 91003 Evry Cedex (France); Kirchlechner, C; Keckes, J [Erich Schmid Institute for Material Science, Austrian Academy of Science and Institute of Metal Physics, University of Leoben, Jahnstrasse 12, 8700 Leoben (Austria); Jacques, V; Ravy, S [Synchrotron SOLEIL, L' Orme des merisiers, Saint-Aubin BP 48, 91192 Gif-sur-Yvette Cedex (France)], E-mail: nicolas.vaxelaire@univ-cezanne.fr

    2010-03-15

    Coherent x-ray diffraction is used to investigate the mechanical properties of a single grain within a polycrystalline thin film in situ during a thermal cycle. Both the experimental approach and finite element simulation are described. Coherent diffraction from a single grain has been monitored in situ at different temperatures. This experiment offers unique perspectives for the study of the mechanical properties of nano-objects.

  14. Methodology for studying strain inhomogeneities in polycrystalline thin films during in situ thermal loading using coherent x-ray diffraction

    International Nuclear Information System (INIS)

    Vaxelaire, N; Labat, S; Thomas, O; Proudhon, H; Forest, S; Kirchlechner, C; Keckes, J; Jacques, V; Ravy, S

    2010-01-01

    Coherent x-ray diffraction is used to investigate the mechanical properties of a single grain within a polycrystalline thin film in situ during a thermal cycle. Both the experimental approach and finite element simulation are described. Coherent diffraction from a single grain has been monitored in situ at different temperatures. This experiment offers unique perspectives for the study of the mechanical properties of nano-objects.

  15. Ultrahigh-vacuum in situ electrochemistry with solid polymer electrolyte and x-ray photoelectron spectroscopy studies of polypyrrole

    International Nuclear Information System (INIS)

    Skotheim, T.A.; Florit, M.I.; Melo, A.; O'Grady, W.E.

    1984-01-01

    A new in situ combined electrochemistry and x-ray-photoelectron-spectroscopy (XPS) technique using solid polymer electrolytes has been used to characterize electrically conducting films of polypyrrole perchlorate. The technique allows in situ electrochemical oxidation and reduction (doping and undoping) in ultrahigh vacuum and the simultaneous study of the polymer with XPS as a function of its electrochemical potential. We demonstrate that some anion species interact strongly electrostatically with the nitrogen heteroatoms. We also show conclusively that the electrochemistry of polypyrrole is highly irreversible

  16. A Rotational and Axial Motion System Load Frame Insert for In Situ High Energy X-Ray Studies (Postprint)

    Science.gov (United States)

    2015-09-08

    Paul A. Shade, Jay C. Schuren, and Todd J. Turner AFRL/RX Basil Blank PulseRay Peter Kenesei, Kurt Goetze, Ulrich Lienert, and Jonathan Almer...AFRL/RX 2) Basil Blank – PulseRay (continued on page 2) 5d. PROJECT NUMBER 4349 5e. TASK NUMBER 0001 5f...2015) A rotational and axial motion system load frame insert for in situ high energy x-ray studies Paul A. Shade,1,a) Basil Blank,2 Jay C. Schuren,1,b

  17. In-situ studies of the recrystallization process of CuInS2 thin films by energy dispersive X-ray diffraction

    International Nuclear Information System (INIS)

    Thomas, D.; Mainz, R.; Rodriguez-Alvarez, H.; Marsen, B.; Abou-Ras, D.; Klaus, M.; Genzel, Ch.; Schock, H.-W.

    2011-01-01

    Recrystallization processes during the sulfurization of CuInS 2 (CIS) thin films have been studied in-situ using energy dispersive X-ray diffraction (EDXRD) with synchrotron radiation. In order to observe the recrystallization isolated from other reactions occurring during film growth, Cu-poor, small grained CIS layers covered with CuS on top were heated in a vacuum chamber equipped with windows for synchrotron radiation in order to analyze the grain growth mechanism within the CIS layer. In-situ monitoring of the grain size based on diffraction line profile analysis of the CIS-112 reflection was utilized to interrupt the recrystallization process at different points. Ex-situ studies by electron backscatter diffraction (EBSD) and energy dispersive X-ray spectroscopy (EDX) performed on samples of intermediate recrystallization states reveal that during the heat treatment Cu and In interdiffuse inside the layer indicating the importance of the mobility of these two elements during CuInS 2 grain growth.

  18. Methodology for in situ synchrotron X-ray studies in the laser-heated diamond anvil cell

    DEFF Research Database (Denmark)

    Mezouar, M.; Giampaoli, R.; Garbarino, G.

    2017-01-01

    A review of some important technical challenges related to in situ diamond anvil cell laser heating experimentation at synchrotron X-ray sources is presented. The problem of potential chemical reactions between the sample and the pressure medium or the carbon from the diamond anvils is illustrated...

  19. Application of in situ x-ray diffraction techniques in heterogenous catalytic systems

    International Nuclear Information System (INIS)

    Sharifah Bee Abd Hamid

    2002-01-01

    A broad range of techniques is available today for the characterisation of catalysts and the investigation of catalyst reaction mechanisms. However, only a limited number of those are suitable for in situ studies, i.e experiments performed in conditions mimicking or close as possible to real operating conditions. Various commercially and in-house developed in situ X-Ray diffraction (XRD) cells have been used to obtain information on the phase and structure of materials at the initial formation stage, activation methodology, calcination, reduction and carburization. A major advantage of the in situ X-ray cells is that it allows direct observations on the decomposition of precursors leading to various phases in a controlled environment, i.e. controlled temperature and pressure under specified gases. The cells can be operated both at high temperatures and high pressures, equipped with Position Sensitive Detector (PSD), feature which was used to study phase transformation occurring during the activation of various solids. In MoO 3 , XRD results provide detailed information on the hydrogen insertion into its lattice, followed by carburization providing good understanding on the mechanism in the solid transformation leading to the metastable MoC 1 -x phase. For the Bi-SnO x systems, the environmental cell coupled with XRD and PSD allow the design of activation procedure to obtain the active Bi 2 Sn 2 O 7 . The in situ XRD technique reveals crucial information on the initial stage of oxides formations prior to condensation reaction shown in MCM-41 and titania systems. In this presentation, discussions on general achievements and problems relating to the use of in situ XRD techniques as well as of specific examples selected to illustrate the use and potential of in situ XRD are made. It is not intended to be a review of the art but a highlight of the challenges which the catalytic and material scientists face when entering the avenue. (Author)

  20. Structural study on Ni nanowires in an anodic alumina membrane by using in situ heating extended x-ray absorption fine structure and x-ray diffraction techniques

    International Nuclear Information System (INIS)

    Cai Quan; Chen Xing; Chen Zhongjun; Wang Wei; Mo Guang; Wu Zhonghua; Zhang Junxi; Zhang Lide; Pan Wei

    2008-01-01

    Polycrystalline Ni nanowires have been prepared by electrochemical deposition in an anodic alumina membrane template with a nanopore size of about 60 nm. In situ heating extended x-ray absorption fine structure and x-ray diffraction techniques are used to probe the atomic structures. The nanowires are identified as being mixtures of nanocrystallites and amorphous phase. The nanocrystallites have the same thermal expansion coefficient, of 1.7 x 10 -5 K -1 , as Ni bulk; however, the amorphous phase has a much larger thermal expansion coefficient of 3.5 x 10 -5 K -1 . Details of the Ni nanowire structures are discussed in this paper

  1. An in-situ X-ray diffraction study on the electrochemical formation of PtZn alloys on Pt(1 1 1) single crystal electrode

    Energy Technology Data Exchange (ETDEWEB)

    Drnec, J., E-mail: drnec@esrf.fr [ESRF, Grenoble (France); Bizzotto, D. [Department of Chemistry, AMPEL, University of British Columbia, Vancouver, BC (Canada); Carlà, F. [ESRF, Grenoble (France); Fiala, R. [Charles University, Faculty of Mathematics and Physics, Prague (Czech Republic); Sode, A. [Ruhr-Universität Bochum, Bochum (Germany); Balmes, O.; Detlefs, B.; Dufrane, T. [ESRF, Grenoble (France); Felici, R., E-mail: felici@esrf.fr [ESRF, Grenoble (France)

    2015-11-01

    Highlights: • PtZn electrochemical alloying is observed on single crystal Pt electrodes. • In-situ X-ray characterization during alloy formation and dissolution is provided. • Structural model of the surface during alloying and dissolution is discussed. • X-ray based techniques can be used in in-operando studies of bimetallic fuel cell catalysts. - Abstract: The electrochemical formation and dissolution of the oxygen reduction reaction (ORR) PtZn catalyst on Pt(1 1 1) surface is followed by in-situ X-ray diffraction (XRD) and X-ray reflectivity (XRR) measurements. When the crystalline Pt surface is polarized to sufficiently negative potential values, with respect to an Ag/AgCl|KCl reference electrode, the electrodeposited zinc atoms diffuse into the bulk and characteristic features are observed in the X-ray patterns. The surface structure and composition during deposition and dissolution is determined from analysis of XRR curves and measurements of crystal truncation rods. Thin Zn-rich surface layer is present during the alloy formation while a Zn-depleted layer forms during dissolution.

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

    DEFF Research Database (Denmark)

    Wejdemann, Christian; Lienert, U.; Pantleon, Wolfgang

    2010-01-01

    Two copper samples, pre-deformed in tension to 5% plastic strain, are subjected to an in situ tensile deformation of 1% plastic strain while X-ray peak profiles from individual bulk grains are obtained. One sample is oriented with the in situ tensile axis parallel to the pre-deformation axis...

  3. Reduction of variable-truncation artifacts from beam occlusion during in situ x-ray tomography

    DEFF Research Database (Denmark)

    Borg, Leise; Jørgensen, Jakob Sauer; Frikel, Jürgen

    2017-01-01

    Many in situ x-ray tomography studies require experimental rigs which may partially occlude the beam and cause parts of the projection data to be missing. In a study of fluid flow in porous chalk using a percolation cell with four metal bars drastic streak artifacts arise in the filtered...... and artifact-reduction methods are designed in context of FBP reconstruction motivated by computational efficiency practical for large, real synchrotron data. While a specific variable-truncation case is considered, the proposed methods can be applied to general data cut-offs arising in different in situ x-ray...... backprojection (FBP) reconstruction at certain orientations. Projections with non-trivial variable truncation caused by the metal bars are the source of these variable-truncation artifacts. To understand the artifacts a mathematical model of variable-truncation data as a function of metal bar radius and distance...

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

    Energy Technology Data Exchange (ETDEWEB)

    Gumí-Audenis, B. [ESRF, The European Synchrotron, Grenoble (France); Institute for Bioengineering of Catalonia (IBEC), Barcelona (Spain); Physical Chemistry Department, Universitat de Barcelona, Barcelona (Spain); Networking Biomedical Research Center on Bioengineering, Biomaterials and Nanomedicine (CIBER-BBN), Madrid (Spain); Carlà, F. [ESRF, The European Synchrotron, Grenoble (France); Vitorino, M. V. [University of Lisboa, Falculty of Science, Biosystems and Integrative Sciences Institute - BIOISI, Lisbon (Portugal); Panzarella, A. [ESRF, The European Synchrotron, Grenoble (France); Porcar, L. [Institut Laue-Langevin, Grenoble (France); Boilot, M. [ORTEC, Marseille (France); Guerber, S. [CEA, LETI Grenoble (France); Bernard, P. [ESRF, The European Synchrotron, Grenoble (France); Rodrigues, M. S. [University of Lisboa, Falculty of Science, Biosystems and Integrative Sciences Institute - BIOISI, Lisbon (Portugal); Sanz, F.; Giannotti, M. I. [Institute for Bioengineering of Catalonia (IBEC), Barcelona (Spain); Physical Chemistry Department, Universitat de Barcelona, Barcelona (Spain); Networking Biomedical Research Center on Bioengineering, Biomaterials and Nanomedicine (CIBER-BBN), Madrid (Spain); Costa, L., E-mail: luca.costa@esrf.fr [ESRF, The European Synchrotron, Grenoble (France)

    2015-09-30

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

  5. In Situ X-ray Diffraction Studies of (De)lithiation Mechanism in Silicon Nanowire Anodes

    KAUST Repository

    Misra, Sumohan

    2012-06-26

    Figure Persented: Silicon is a promising anode material for Li-ion batteries due to its high theoretical specific capacity. From previous work, silicon nanowires (SiNWs) are known to undergo amorphorization during lithiation, and no crystalline Li-Si product has been observed. In this work, we use an X-ray transparent battery cell to perform in situ synchrotron X-ray diffraction on SiNWs in real time during electrochemical cycling. At deep lithiation voltages the known metastable Li 15Si 4 phase forms, and we show that avoiding the formation of this phase, by modifying the SiNW growth temperature, improves the cycling performance of SiNW anodes. Our results provide insight on the (de)lithiation mechanism and a correlation between phase evolution and electrochemical performance for SiNW anodes. © 2012 American Chemical Society.

  6. In Situ Soft X-ray Spectromicroscopy of Early Tricalcium Silicate Hydration

    Directory of Open Access Journals (Sweden)

    Sungchul Bae

    2016-12-01

    Full Text Available The understanding and control of early hydration of tricalcium silicate (C3S is of great importance to cement science and concrete technology. However, traditional characterization methods are incapable of providing morphological and spectroscopic information about in situ hydration at the nanoscale. Using soft X-ray spectromicroscopy, we report the changes in morphology and molecular structure of C3S at an early stage of hydration. In situ C3S hydration in a wet cell, beginning with induction (~1 h and acceleration (~4 h periods of up to ~8 h, was studied and compared with ex situ measurements in the deceleration period after 15 h of curing. Analysis of the near-edge X-ray absorption fine structure showed that the Ca binding energy and energy splitting of C3S changed rapidly in the early age of hydration and exhibited values similar to calcium silicate hydrate (C–S–H. The formation of C–S–H nanoseeds in the C3S solution and the development of a fibrillar C–S–H morphology on the C3S surface were visualized. Following this, silicate polymerization accompanied by C–S–H precipitation produced chemical shifts in the peaks of the main Si K edge and in multiple scattering. However, the silicate polymerization process did not significantly affect the Ca binding energy of C–S–H.

  7. In situ X-ray probing reveals fingerprints of surface platinum oxide.

    Science.gov (United States)

    Friebel, Daniel; Miller, Daniel J; O'Grady, Christopher P; Anniyev, Toyli; Bargar, John; Bergmann, Uwe; Ogasawara, Hirohito; Wikfeldt, Kjartan Thor; Pettersson, Lars G M; Nilsson, Anders

    2011-01-07

    In situ X-ray absorption spectroscopy (XAS) at the Pt L(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 FEFF 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.

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

    Science.gov (United States)

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

    2007-06-26

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

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

    International Nuclear Information System (INIS)

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

    2009-01-01

    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

  10. In situ study of the growth and degradation processes in tetragonal lysozyme crystals on a silicon substrate by high-resolution X-ray diffractometry

    Science.gov (United States)

    Kovalchuk, M. V.; Prosekov, P. A.; Marchenkova, M. A.; Blagov, A. E.; D'yakova, Yu. A.; Tereshchenko, E. Yu.; Pisarevskii, Yu. V.; Kondratev, O. A.

    2014-09-01

    The results of an in situ study of the growth of tetragonal lysozyme crystals by high-resolution X-ray diffractometry are considered. The crystals are grown by the sitting-drop method on crystalline silicon substrates of different types: both on smooth substrates and substrates with artificial surface-relief structures using graphoepitaxy. The crystals are grown in a special hermetically closed crystallization cell, which enables one to obtain images with an optical microscope and perform in situ X-ray diffraction studies in the course of crystal growth. Measurements for lysozyme crystals were carried out in different stages of the crystallization process, including crystal nucleation and growth, developed crystals, the degradation of the crystal structure, and complete destruction.

  11. First use of portable system coupling X-ray diffraction and X-ray fluorescence for in-situ analysis of prehistoric rock art.

    Science.gov (United States)

    Beck, L; Rousselière, H; Castaing, J; Duran, A; Lebon, M; Moignard, B; Plassard, F

    2014-11-01

    Study of prehistoric art is playing a major role in the knowledge of human evolution. Many scientific methods are involved in this investigation including chemical analysis of pigments present on artefacts or applied to cave walls. In the past decades, the characterization of coloured materials was carried on by taking small samples. This procedure had two main disadvantages: slight but existing damage of the paintings and limitation of the number of samples. Thanks to the advanced development of portable systems, in-situ analysis of pigment in cave can be now undertaken without fear for this fragile Cultural Heritage. For the first time, a portable system combining XRD and XRF was used in an underground and archaeological environment for prehistoric rock art studies. In-situ non-destructive analysis of black prehistoric drawings and determination of their composition and crystalline structure were successfully carried out. Original results on pigments used 13,000 years ago in the cave of Rouffignac (France) were obtained showing the use of two main manganese oxides: pyrolusite and romanechite. The capabilities of the portable XRD-XRF system have been demonstrated for the characterization of pigments as well as for the analysis of rock in a cave environment. This first in-situ experiment combining X-ray diffraction and X-ray fluorescence open up new horizons and can fundamentally change our approach of rock art studies. Copyright © 2014 Elsevier B.V. All rights reserved.

  12. In situ X-ray powder diffraction studies of the synthesis of graphene oxide and formation of reduced graphene oxide

    International Nuclear Information System (INIS)

    Storm, Mie Møller; Johnsen, Rune E.; Norby, Poul

    2016-01-01

    Graphene oxide (GO) and reduced graphene oxide (rGO) are important materials in a wide range of fields. The modified Hummers methods, for synthesizing GO, and subsequent thermal reduction to rGO, are often employed for production of rGO. However, the mechanism behinds these syntheses methods are still unclear. We present an in situ X-ray diffraction study of the synthesis of GO and thermal reduction of GO. The X-ray diffraction revealed that the Hummers method includes an intercalation state and finally formation of additional crystalline material. The formation of GO is observed during both the intercalation and the crystallization stage. During thermal reduction of GO three stages were observed: GO, a disordered stage, and the rGO stage. The appearance of these stages depends on the heating ramp. The aim of this study is to provide deeper insight into the chemical and physical processes during the syntheses. - Graphical abstract: In situ X-ray diffraction results for of the modified Hummers synthesis and the thermal reduction of graphene oxide, revealing three stages for both syntheses as well as new GO diffraction peaks and unidentified crystalline material for the Hummers synthesis and a disordered stage for the thermal reduction of graphene oxide. Display Omitted - Highlights: • Hummers synthesis consists of three stages: dissolution, intercalation and crystal. • GO is produced early on during the synthesis and display new diffraction peaks. • An unidentified triclinic phase is observed for the Hummers synthesis. • Thermal reduction of GO display three stages: GO, a disordered stage and rGO. • In situ XRD indicate reformation of rGO even for fast heated thermal reduction.

  13. In situ X-ray powder diffraction studies of the synthesis of graphene oxide and formation of reduced graphene oxide

    Energy Technology Data Exchange (ETDEWEB)

    Storm, Mie Møller, E-mail: mmst@dtu.dk; Johnsen, Rune E.; Norby, Poul

    2016-08-15

    Graphene oxide (GO) and reduced graphene oxide (rGO) are important materials in a wide range of fields. The modified Hummers methods, for synthesizing GO, and subsequent thermal reduction to rGO, are often employed for production of rGO. However, the mechanism behinds these syntheses methods are still unclear. We present an in situ X-ray diffraction study of the synthesis of GO and thermal reduction of GO. The X-ray diffraction revealed that the Hummers method includes an intercalation state and finally formation of additional crystalline material. The formation of GO is observed during both the intercalation and the crystallization stage. During thermal reduction of GO three stages were observed: GO, a disordered stage, and the rGO stage. The appearance of these stages depends on the heating ramp. The aim of this study is to provide deeper insight into the chemical and physical processes during the syntheses. - Graphical abstract: In situ X-ray diffraction results for of the modified Hummers synthesis and the thermal reduction of graphene oxide, revealing three stages for both syntheses as well as new GO diffraction peaks and unidentified crystalline material for the Hummers synthesis and a disordered stage for the thermal reduction of graphene oxide. Display Omitted - Highlights: • Hummers synthesis consists of three stages: dissolution, intercalation and crystal. • GO is produced early on during the synthesis and display new diffraction peaks. • An unidentified triclinic phase is observed for the Hummers synthesis. • Thermal reduction of GO display three stages: GO, a disordered stage and rGO. • In situ XRD indicate reformation of rGO even for fast heated thermal reduction.

  14. A rotational and axial motion system load frame insert for in situ high energy x-ray studies

    Energy Technology Data Exchange (ETDEWEB)

    Shade, Paul A., E-mail: paul.shade.1@us.af.mil; Schuren, Jay C.; Turner, Todd J. [Materials and Manufacturing Directorate, Air Force Research Laboratory, Wright-Patterson AFB, Ohio 45433 (United States); Blank, Basil [PulseRay, Beaver Dams, New York 14812 (United States); Kenesei, Peter; Goetze, Kurt; Lienert, Ulrich; Almer, Jonathan [Advanced Photon Source, Argonne National Laboratory, Argonne, Illinois 60439 (United States); Suter, Robert M. [Carnegie Mellon University, Pittsburgh, Pennsylvania 15213 (United States); Bernier, Joel V.; Li, Shiu Fai [Engineering Directorate, Lawrence Livermore National Laboratory, Livermore, California 94550 (United States); Lind, Jonathan [Carnegie Mellon University, Pittsburgh, Pennsylvania 15213 (United States); Engineering Directorate, Lawrence Livermore National Laboratory, Livermore, California 94550 (United States)

    2015-09-15

    High energy x-ray characterization methods hold great potential for gaining insight into the behavior of materials and providing comparison datasets for the validation and development of mesoscale modeling tools. A suite of techniques have been developed by the x-ray community for characterizing the 3D structure and micromechanical state of polycrystalline materials; however, combining these techniques with in situ mechanical testing under well characterized and controlled boundary conditions has been challenging due to experimental design requirements, which demand new high-precision hardware as well as access to high-energy x-ray beamlines. We describe the design and performance of a load frame insert with a rotational and axial motion system that has been developed to meet these requirements. An example dataset from a deforming titanium alloy demonstrates the new capability.

  15. Instrumentation for in situ flow electrochemical Scanning Transmission X-ray Microscopy (STXM)

    Science.gov (United States)

    Prabu, Vinod; Obst, Martin; Hosseinkhannazer, Hooman; Reynolds, Matthew; Rosendahl, Scott; Wang, Jian; Hitchcock, Adam P.

    2018-06-01

    We report the design and performance of a 3-electrode device for real time in situ scanning transmission X-ray microscopy studies of electrochemical processes under both static (sealed, non-flow) conditions and with a continuous flow of electrolytes. The device was made using a combination of silicon microfabrication and 3D printing technologies. The performance is illustrated by results of a study of copper deposition and stripping at a gold working electrode. X-ray absorption spectromicroscopy at the Cu 2p edge was used to follow the evolution as a function of potential and time of the spatial distributions of Cu(0) and Cu(i) species electro-deposited from an aqueous solution of copper sulphate. The results are interpreted in terms of competing mechanisms for the reduction of Cu(ii).

  16. Effects of X-Ray Dose On Rhizosphere Studies Using X-Ray Computed Tomography

    Science.gov (United States)

    Zappala, Susan; Helliwell, Jonathan R.; Tracy, Saoirse R.; Mairhofer, Stefan; Sturrock, Craig J.; Pridmore, Tony; Bennett, Malcolm; Mooney, Sacha J.

    2013-01-01

    X-ray Computed Tomography (CT) is a non-destructive imaging technique originally designed for diagnostic medicine, which was adopted for rhizosphere and soil science applications in the early 1980s. X-ray CT enables researchers to simultaneously visualise and quantify the heterogeneous soil matrix of mineral grains, organic matter, air-filled pores and water-filled pores. Additionally, X-ray CT allows visualisation of plant roots in situ without the need for traditional invasive methods such as root washing. However, one routinely unreported aspect of X-ray CT is the potential effect of X-ray dose on the soil-borne microorganisms and plants in rhizosphere investigations. Here we aimed to i) highlight the need for more consistent reporting of X-ray CT parameters for dose to sample, ii) to provide an overview of previously reported impacts of X-rays on soil microorganisms and plant roots and iii) present new data investigating the response of plant roots and microbial communities to X-ray exposure. Fewer than 5% of the 126 publications included in the literature review contained sufficient information to calculate dose and only 2.4% of the publications explicitly state an estimate of dose received by each sample. We conducted a study involving rice roots growing in soil, observing no significant difference between the numbers of root tips, root volume and total root length in scanned versus unscanned samples. In parallel, a soil microbe experiment scanning samples over a total of 24 weeks observed no significant difference between the scanned and unscanned microbial biomass values. We conclude from the literature review and our own experiments that X-ray CT does not impact plant growth or soil microbial populations when employing a low level of dose (<30 Gy). However, the call for higher throughput X-ray CT means that doses that biological samples receive are likely to increase and thus should be closely monitored. PMID:23840640

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

    Energy Technology Data Exchange (ETDEWEB)

    Mi, Jiawei; Tan, Dongyue; Lee, Tung Lik (Hull)

    2014-12-11

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

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

    International Nuclear Information System (INIS)

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

    2013-01-01

    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 1-x Co 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

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

    CERN Document Server

    Ellmer, K; Weiss, V; Rossner, H

    2001-01-01

    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 deg. and 10 deg., 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.

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

    International Nuclear Information System (INIS)

    Antonio, M.R.; Soderholm, L.

    1995-01-01

    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 3 -edge XANES (X-ray Absorption Near Edge Structure) throughout the course of electrolysis of an aqueous solution of EuCl 3 ·6H 2 O in 1 M H 2 SO 4 . The europium L 3 -edge resonances reported here for the Eu III and Eu II ions demonstrate that their 2p 3/2 → 5d electronic transition probabilities are not the same

  1. Rapid detection of chromosome rearrangement in medical diagnostic X-ray workers by using fluorescence in situ hybridization and study on dose estimation

    International Nuclear Information System (INIS)

    Wang Zhiquan; Sun Yuanming; Li Jin

    1998-01-01

    Objective: Biological doses were estimated for medical diagnostic X-ray workers. Methods: Chromosome rearrangements in X-ray workers were analysed by fluorescence in situ hybridization (FISH) with composite whole chromosome paintings number 4 and number 7. Results: The frequency of translocation in medical diagnostic X-ray workers was much higher than that in control group (P<0.01). The biological doses to individual X-ray workers were calculated by their translocation frequency. The translocation frequencies of both FISH and G-banding were in good agreement. Conclusion: The biological doses to X-ray workers are estimated by FISH first when their dosimetry records are not documented

  2. In situ X-ray powder diffraction, synthesis, and magnetic properties of InVO 3

    Science.gov (United States)

    Lundgren, Rylan J.; Cranswick, Lachlan M. D.; Bieringer, Mario

    2006-12-01

    We report the first synthesis and high-temperature in situ X-ray diffraction study of InVO 3. Polycrystalline InVO 3 has been prepared via reduction of InVO 4 using a carbon monoxide/carbon dioxide buffer gas. InVO 3 crystallizes in the bixbyite structure in space group Ia-3 (206) with a=9.80636(31) Å with In 3+/V 3+ disorder on the (8 b) and (24 d) cation sites. In situ powder X-ray diffraction experiments and thermal gravimetric analysis in a CO/CO 2 buffer gas revealed the existence of the metastable phase InVO 3. Bulk samples with 98.5(2)% purity were prepared using low-temperature reduction methods. The preparative methods limited the crystallinity of this new phase to approximately 225(50) Å. Magnetic susceptibility and neutron diffraction experiments suggest a spin-glass ground state for InVO 3.

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

    Energy Technology Data Exchange (ETDEWEB)

    Wang, Hongchang, E-mail: hongchang.wang@diamond.ac.uk; Kashyap, Yogesh; Laundy, David; Sawhney, Kawal [Diamond Light Source Ltd, Harwell Science and Innovation Campus, Didcot OX11 0DE (United Kingdom)

    2015-06-06

    The two-dimensional slope error of an X-ray mirror has been retrieved by employing the speckle scanning technique, which will be valuable at synchrotron radiation facilities and in astronomical telescopes. 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.

  4. Studying fatigue damage evolution in uni-directional composites using x-ray computed tomography

    DEFF Research Database (Denmark)

    Mikkelsen, Lars Pilgaard

    , it will be possible to lower the costs of energy for wind energy based electricity. In the present work, a lab-source x-ray computed tomography equipment (Zeiss Xradia 520 Versa) has been used in connection with ex-situ fatigue testing of uni-directional composites in order to identify fibre failure during...... comparable x-ray studies) have been used in order to ensure a representative test volume during the ex-situ fatigue testing. Using the ability of the x-ray computed tomography to zoom into regions of interest, non-destructive, the fatigue damage evolution in a repeating ex-situ fatigue loaded test sample has...... improving the fatigue resistance of non-crimp fabric used in the wind turbine industry can be made....

  5. Probing the influence of X-rays on aqueous copper solutions using time-resolved in situ combined video/X-ray absorption near-edge/ultraviolet-visible spectroscopy

    NARCIS (Netherlands)

    Mesu, J. Gerbrand; Beale, Andrew M.; de Groot, Frank M. F.; Weckhuysen, Bert M.

    2006-01-01

    Time-resolved in situ video monitoring and ultraviolet-visible spectroscopy in combination with X-ray absorption near-edge spectroscopy (XANES) have been used for the first time in a combined manner to study the effect of synchrotron radiation on a series of homogeneous aqueous copper solutions in a

  6. The development of in situ photon-in/photon-out soft X-ray spectroscopy on beamline 7.0.1 at the ALS

    International Nuclear Information System (INIS)

    Guo, Jinghua

    2013-01-01

    Highlights: ► Development of various cells for in-situ electronic structure study. ► Gas cell for study of gas molecules and catalytic reactions. ► Liquid cell for study of molecular liquids and ion salvation. ► In-situ cell for study of electrochemical reactions. -- Abstract: This is a mini-review about the development of various cells built over the years for in situ electronic structure study of gas molecules, molecular liquids, gas/solid and liquid/solid interfaces. In the study of gas molecules, the role of the parity selection rule in the case of homonuclear diatomic molecules (N 2 and O 2 ) is revealed and illustrated by the resonant X-ray emission spectra, while the occurrence of forbidden transitions in CO 2 is explained in terms of dynamical symmetry breaking due to vibronic coupling. X-ray emission spectroscopy has been used to elucidate the molecular structure of liquid water, liquid methanol, methanol–water mixtures, as well as cation–water solutions, and to reveal the influence of the intermolecular interaction on the local electronic structure of water molecules. The in situ soft X-ray spectroscopy experimental studies of electrochemical reactions were also performed under ambient conditions

  7. Chromosome translocations in chinese medical X-ray workers analyzed by fluorescence in situ hybridization

    International Nuclear Information System (INIS)

    Sun Yuanming; Li Jin; Wang Qin; Tang Weisheng; Wang Zhiquan

    2002-01-01

    Objective: To study long-term radiation effect in occupational workers exposed to low dose X-rays using the method of fluorescence in situ hybridization (FISH). Method: Chromosome translocations of 25 medical X-ray workers were analyzed by FISH with chromosome No. 4 and No. 7 probes according to PAINT (The Protocol for Aberration Identification and Nomenclature Terminology) system. Results: The frequency of genome translocation in X-ray workers was (13.14 ± 1.23)/1000 cells. The rate of complete and incomplete translocation was 1:1.7. According to the calendar year of entry before/after the year of 1965 as the border, the data showed that the incomplete translocation of the after 1965 group was obviously higher than those of the controls (P < 0.01 and P < 0.05, respectively). Conclusion: The chromosome translocation in early Chinese medical X-ray workers is mainly the incomplete one, the frequency of translocation does not dependent on chromosomal DNA content, and incomplete and complete ones increase along with prolongation of working years in their position

  8. Combined in situ small and wide angle X-ray scattering studies of TiO2 nano-particle annealing to 1023 K

    DEFF Research Database (Denmark)

    Kehres, Jan; Andreasen, Jens Wenzel; Krebs, Frederik C

    2010-01-01

    Combined in situ small- and wide-angle X-ray scattering (SAXS/WAXS) studies were performed in a recently developed laboratory setup to investigate the dynamical properties of dry oleic acid-capped titanium dioxide nanorods during annealing in an inert gas stream in a temperature interval of 298-1...

  9. In situ x-ray diffraction study on AgI nanowire arrays

    International Nuclear Information System (INIS)

    Wang Yinhai; Ye Changhui; Wang Guozhong; Zhang Lide; Liu Yanmei; Zhao Zhongyan

    2003-01-01

    The AgI nanowire arrays were prepared in the ordered porous alumina membrane by an electrochemical method. Transmission electron microscopy observation shows that the AgI nanowires are located in the channels of the alumina membrane. In situ x-ray diffractions show that the nanowire arrays possess hexagonal close-packed structure (β-AgI) at 293 K, orienting along the (002) plane, whereas at 473 K, the nanowire arrays possess a body-centered cubic structure (α-AgI), orienting along the (110) plane. The AgI nanowire arrays exhibit a negative thermal expansion property from 293 to 433 K, and a higher transition temperature from the β to α phase. We ascribe the negative thermal expansion behavior to the phase transition from the β to α phase, and the elevated transition temperature to the radial restriction by the channels of alumina membrane

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

    Energy Technology Data Exchange (ETDEWEB)

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

    Science.gov (United States)

    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.

  12. Studies in useful hard x-ray induced chemistry

    Science.gov (United States)

    Pravica, Michael; Bai, Ligang; Sneed, Daniel; Park, Changyong

    2013-06-01

    The observed rapid decomposition of potassium chlorate (via 2KClO3 + h ν --> 2KCl +3O2) via synchrotron hard x-ray irradiation (>10 keV) has enabled experiments that are developing novel and useful hard x-ray chemistry. We have observed a number of radiation-induced in situ decomposition reactions in various substances which release O2, H2, N2, NH3, and H2O in a diamond anvil cell (DAC) at ambient and high pressures. These novel acatalytic and isothermal reactions represent a highly controllable, penetrating, and focused method to initiate chemistry (including x-ray induced combustion) in sealed and/or isolated chambers which maintain matter under extreme conditions. During our studies, we have typically observed a slowing of decomposition with pressure including phase dependent decomposition of KClO3. Energy dependent studies have observed an apparent resonance near 15 keV at which the decomposition rate is maximized. This may enable use of much lower flux and portable x-ray sources (e.g. x-ray tubes) in larger scale experiments. These developments support novel means to load DACs and control chemical reactions providing novel routes of synthesis of novel materials under extreme conditions.

  13. Structural investigations of LiFePO4 electrodes and in situ studies by Fe X-ray absorption spectroscopy

    International Nuclear Information System (INIS)

    Deb, Aniruddha; Bergmann, Uwe; Cramer, S.P.; Cairns, Elton J.

    2005-01-01

    Fe K-edge X-ray absorption near edge spectroscopy (XANES) and extended X-ray absorption fine structure (EXAFS) have been performed on electrodes containing LiFePO 4 to determine the local atomic and electronic structure and their stability with electrochemical cycling. A versatile electrochemical in situ cell has been constructed for long-term soft and hard X-ray experiments for the structural investigation on battery electrodes during the lithium-insertion/extraction processes. The device is used here for an X-ray absorption spectroscopic study of lithium insertion/extraction in a LiFePO 4 electrode, where the electrode contained about 7.7 mg of LiFePO 4 on a 20 μm thick Al-foil. Fe K-edge X-ray absorption near edge spectroscopy (XANES) and extended X-ray absorption fine structure (EXAFS) have been performed on this electrode to determine the local atomic and electronic structure and their stability with electrochemical cycling. The initial state (LiFePO 4 ) showed iron to be in the Fe 2+ state corresponding to the initial state (0.0 mAh) of the cell, whereas in the delithiated state (FePO 4 ) iron was found to be in the Fe 3+ state corresponding to the final charged state (3 mAh). XANES region of the XAS spectra revealed a high spin configuration for the two states (Fe (II), d 6 and Fe (III), d 5 ). The results confirm that the olivine structure of the LiFePO 4 and FePO 4 is retained by the electrodes in agreement with the XRD observations reported previously. These results confirm that LiFePO 4 cathode material retains good structural short-range order leading to superior cycling capability

  14. In situ flash x-ray high-speed computed tomography for the quantitative analysis of highly dynamic processes

    Science.gov (United States)

    Moser, Stefan; Nau, Siegfried; Salk, Manfred; Thoma, Klaus

    2014-02-01

    The in situ investigation of dynamic events, ranging from car crash to ballistics, often is key to the understanding of dynamic material behavior. In many cases the important processes and interactions happen on the scale of milli- to microseconds at speeds of 1000 m s-1 or more. Often, 3D information is necessary to fully capture and analyze all relevant effects. High-speed 3D-visualization techniques are thus required for the in situ analysis. 3D-capable optical high-speed methods often are impaired by luminous effects and dust, while flash x-ray based methods usually deliver only 2D data. In this paper, a novel 3D-capable flash x-ray based method, in situ flash x-ray high-speed computed tomography is presented. The method is capable of producing 3D reconstructions of high-speed processes based on an undersampled dataset consisting of only a few (typically 3 to 6) x-ray projections. The major challenges are identified, discussed and the chosen solution outlined. The application is illustrated with an exemplary application of a 1000 m s-1 high-speed impact event on the scale of microseconds. A quantitative analysis of the in situ measurement of the material fragments with a 3D reconstruction with 1 mm voxel size is presented and the results are discussed. The results show that the HSCT method allows gaining valuable visual and quantitative mechanical information for the understanding and interpretation of high-speed events.

  15. In Situ X-Ray Diffraction Study on Surface Melting of Bi Nanoparticles Embedded in a SiO2 Matrix

    International Nuclear Information System (INIS)

    Chen Xiao-Ming; Huo Kai-Tuo; Liu Peng

    2014-01-01

    Bi nanoparticles embedded in a SiO 2 matrix were prepared via the high energy ball milling method. The melting behavior of Bi nanoparticles was studied by means of differential scanning calorimetry (DSC) and high-temperature in situ X-ray diffraction (XRD). DSC cannot distinguish the surface melting from ‘bulk’ melting of the Bi nanoparticles. The XRD intensity of the Bi nanoparticles decreases progressively during the in situ heating process. The variation in the normalized integrated XRD intensity versus temperature is related to the average grain size of Bi nanoparticles. Considering the effects of temperature on Debye—Waller factor and Lorentz-polarization factor, we discuss the XRD results in accordance with surface melting. Our results show that the in situ XRD technique is effective to explore the surface melting of nanoparticles

  16. Non-destructive in situ study of “Mad Meg” by Pieter Bruegel the Elder using mobile X-ray fluorescence, X-ray diffraction and Raman spectrometers

    Energy Technology Data Exchange (ETDEWEB)

    Van de Voorde, Lien, E-mail: lien.vandevoorde@ugent.be [Ghent University, Department of Analytical Chemistry, X-ray Microspectroscopy and Imaging Research Group, Krijgslaan 281 S12, B-9000 Gent (Belgium); Van Pevenage, Jolien [Ghent University, Department of Analytical Chemistry, Raman Spectroscopy Research Group, Krijgslaan 281 S12, B-9000 Gent (Belgium); De Langhe, Kaat [Ghent University, Department of Archaeology, Archaeometry Research Group, Sint-Pietersnieuwstraat 35, B-9000 Gent (Belgium); De Wolf, Robin; Vekemans, Bart; Vincze, Laszlo [Ghent University, Department of Analytical Chemistry, X-ray Microspectroscopy and Imaging Research Group, Krijgslaan 281 S12, B-9000 Gent (Belgium); Vandenabeele, Peter [Ghent University, Department of Archaeology, Archaeometry Research Group, Sint-Pietersnieuwstraat 35, B-9000 Gent (Belgium); Martens, Maximiliaan P.J. [Ghent University, Department of Art, Music and Theatre Sciences, Blandijnberg 2, B-9000 Gent (Belgium)

    2014-07-01

    “Mad Meg”, a figure of Flemish folklore, is the subject of a famous oil-on-panel painting by the Flemish renaissance artist Pieter Bruegel the Elder, exhibited in the Museum Mayer van den Bergh (Antwerp, Belgium). This article reports on the in situ chemical characterization of this masterpiece by using currently available state-of-the-art portable analytical instruments. The applied non-destructive analytical approach involved the use of a) handheld X-ray fluorescence instrumentation for retrieving elemental information and b) portable X-ray fluorescence/X-ray diffraction instrumentation and laser-based Raman spectrometers for obtaining structural/molecular information. Next to material characterization of the used pigments and of the different preparation layers of the painting, also the verification of two important historical iconographic hypotheses is performed concerning the economic way of painting by Brueghel, and whether or not he used blue smalt pigment for painting the boat that appears towards the top of the painting. The pigments identified are smalt pigment (65% SiO{sub 2} + 15% K{sub 2}O + 10% CoO + 5% Al{sub 2}O{sub 3}) for the blue color present in all blue areas of the painting, probably copper resinate for the green colors, vermillion (HgS) as red pigment and lead white is used to form different colors. The comparison of blue pigments used on different areas of the painting gives no differences in the elemental fingerprint which confirms the existing hypothesis concerning the economic painting method by Bruegel. - Highlights: • In situ, non-destructive investigation of a famous painting by Pieter Bruegel. • Use of a new, commercial available, portable XRF/XRD instrumentation. • Multi-methodological approach: make also use of a mobile Raman spectrometer. • Used pigments and different preparation layers of the painting are characterized. • The verification of two important historical iconographic hypotheses are performed.

  17. Non-destructive in situ study of “Mad Meg” by Pieter Bruegel the Elder using mobile X-ray fluorescence, X-ray diffraction and Raman spectrometers

    International Nuclear Information System (INIS)

    Van de Voorde, Lien; Van Pevenage, Jolien; De Langhe, Kaat; De Wolf, Robin; Vekemans, Bart; Vincze, Laszlo; Vandenabeele, Peter; Martens, Maximiliaan P.J.

    2014-01-01

    “Mad Meg”, a figure of Flemish folklore, is the subject of a famous oil-on-panel painting by the Flemish renaissance artist Pieter Bruegel the Elder, exhibited in the Museum Mayer van den Bergh (Antwerp, Belgium). This article reports on the in situ chemical characterization of this masterpiece by using currently available state-of-the-art portable analytical instruments. The applied non-destructive analytical approach involved the use of a) handheld X-ray fluorescence instrumentation for retrieving elemental information and b) portable X-ray fluorescence/X-ray diffraction instrumentation and laser-based Raman spectrometers for obtaining structural/molecular information. Next to material characterization of the used pigments and of the different preparation layers of the painting, also the verification of two important historical iconographic hypotheses is performed concerning the economic way of painting by Brueghel, and whether or not he used blue smalt pigment for painting the boat that appears towards the top of the painting. The pigments identified are smalt pigment (65% SiO 2 + 15% K 2 O + 10% CoO + 5% Al 2 O 3 ) for the blue color present in all blue areas of the painting, probably copper resinate for the green colors, vermillion (HgS) as red pigment and lead white is used to form different colors. The comparison of blue pigments used on different areas of the painting gives no differences in the elemental fingerprint which confirms the existing hypothesis concerning the economic painting method by Bruegel. - Highlights: • In situ, non-destructive investigation of a famous painting by Pieter Bruegel. • Use of a new, commercial available, portable XRF/XRD instrumentation. • Multi-methodological approach: make also use of a mobile Raman spectrometer. • Used pigments and different preparation layers of the painting are characterized. • The verification of two important historical iconographic hypotheses are performed

  18. A sample cell to study hydrate formation with x-ray scattering

    International Nuclear Information System (INIS)

    Conrad, Heiko; Lehmkuehler, Felix; Sternemann, Christian; Feroughi, Omid; Tolan, Metin; Simonelli, Laura; Huotari, Simo

    2009-01-01

    We present a new sample cell for measuring nonresonant inelastic x-ray scattering spectra of a tetrahydrofuran (THF)-water liquid mixture and THF hydrate. The hydrate is formed inside the cell after nucleation seeds have been offered by a special magnetic stirring mechanism. Hydrate formation was verified by wide angle x-ray scattering and nonresonant x-ray Raman scattering spectra at the oxygen K-edge. A broad range of scattering angles can be studied with this cell which is necessary for momentum transfer dependent inelastic x-ray scattering. This cell is ideal to examine other liquid hydrate formers or other liquid samples, which have to be mixed in situ during the measurements.

  19. In-situ measurement of the strain relaxation of GaN nanograins during X-ray irradiation

    International Nuclear Information System (INIS)

    Choe, Hyeokmin; Lee, Sanghwa; Sohn, Yuri; Kim, Chinkyo

    2008-01-01

    GaN nanograins were grown on a c-plane sapphire substrate and their strain relaxation due to X-ray irradiation was investigated in-situ by utilizing synchrotron xray scattering. The GaN nanograins were constantly exposed to the synchrotron X-ray and θ-2θ scans through the (002) Bragg peak of GaN were repeatedly carried out during the irradiation. The Bragg peak of the compressively strained GaN nanograins gradually shifted toward higher angle, which implies that the GaN nanograins in compressive strain experienced strain relaxation during X-ray irradiation. (copyright 2008 WILEY-VCH Verlag GmbH and Co. KGaA, Weinheim) (orig.)

  20. Grain rotation and lattice deformation during photoinduced chemical reactions revealed by in situ X-ray nanodiffraction.

    Science.gov (United States)

    Huang, Zhifeng; Bartels, Matthias; Xu, Rui; Osterhoff, Markus; Kalbfleisch, Sebastian; Sprung, Michael; Suzuki, Akihiro; Takahashi, Yukio; Blanton, Thomas N; Salditt, Tim; Miao, Jianwei

    2015-07-01

    In situ X-ray diffraction (XRD) and transmission electron microscopy (TEM) have been used to investigate many physical science phenomena, ranging from phase transitions, chemical reactions and crystal growth to grain boundary dynamics. A major limitation of in situ XRD and TEM is a compromise that has to be made between spatial and temporal resolution. Here, we report the development of in situ X-ray nanodiffraction to measure high-resolution diffraction patterns from single grains with up to 5 ms temporal resolution. We observed, for the first time, grain rotation and lattice deformation in chemical reactions induced by X-ray photons: Br(-) + hv → Br + e(-) and e(-) + Ag(+) → Ag(0). The grain rotation and lattice deformation associated with the chemical reactions were quantified to be as fast as 3.25 rad s(-1) and as large as 0.5 Å, respectively. The ability to measure high-resolution diffraction patterns from individual grains with a temporal resolution of several milliseconds is expected to find broad applications in materials science, physics, chemistry and nanoscience.

  1. In situ SERS and X-ray photoelectron spectroscopy studies on the pH-dependant adsorption of anthraquinone-2-carboxylic acid on silver electrode

    Energy Technology Data Exchange (ETDEWEB)

    Li, Dan, E-mail: dany@sit.edu.cn [School of Chemical and Environmental Engineering, Shanghai Institute of Technology, 100 Haiquan Road, Shanghai 201418 (China); Jia, Shaojie [School of Chemical and Environmental Engineering, Shanghai Institute of Technology, 100 Haiquan Road, Shanghai 201418 (China); Fodjo, Essy Kouadio [Laboratory of Physical Chemistry, University Felix Houphouet Boigny, 22 BP 582, Abidjan 22, Cote d’Ivoire (Cote d' Ivoire); Xu, Hu [School of Chemical and Environmental Engineering, Shanghai Institute of Technology, 100 Haiquan Road, Shanghai 201418 (China); Wang, Yuhong, E-mail: yuhong_wang502@sit.edu.cn [School of Chemical and Environmental Engineering, Shanghai Institute of Technology, 100 Haiquan Road, Shanghai 201418 (China); Deng, Wei [School of Chemical and Environmental Engineering, Shanghai Institute of Technology, 100 Haiquan Road, Shanghai 201418 (China)

    2016-03-30

    Graphical abstract: The orientation of anthraquinone-2-carboxylic acid (AQ-2-COOH) has been investigated by in situ surface-enhanced Raman scattering (in situ SERS) spectroelectrochemistry and angle-resolved X-ray photoelectron spectroscopy (AR-XPS) on silver surface. - Highlights: • The adsorption behavior of anthraquinone-2-carboxylic acid (AQ-2-COOH) on Ag electrode is influenced by the pH. • The pH-dependant adsorption of AQ-2-COOH has been confirmed by in situ surface-enhanced Raman scattering (in situ SERS) spectroelectrochemistry and angle-resolved X-ray photoelectron spectroscopy (AR-XPS). • The results can provide insights into electron transfer reactions of AQ-2-COOH in biological systems. - Abstract: In this study, in situ surface-enhanced Raman scattering (SERS) spectroelectrochemistry and angle-resolved X-ray photoelectron spectroscopy (AR-XPS) are used to investigate the redox reaction and adsorption behavior of anthraquinone-2-carboxylic acid (AQ-2-COOH) on an Ag electrode at different pH values. The obtained results indicate that AQ-2-COOH is adsorbed tilted on the Ag electrode through O-atom of ring carbonyl in a potential range from −0.3 to −0.5 V vs. SCE, but the orientation turns to more tilted orientation with both O-atom of the ring carbonyl and carboxylate group in positive potential region for pH 6.0 and 7.4. However, at pH 10.0, the orientation adopts tilted conformation constantly on the Ag electrode with both O-atom of the anthraquinone ring and carboxylate group in the potential range from −0.3 to −0.5 V vs. SCE or at positive potentials. Moreover, the adsorption behavior of AQ-2-COOH has been further confirmed by AR-XPS on the Ag surface. Proposed reasons for the observed changes in orientation are presented.

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

    DEFF Research Database (Denmark)

    Kehres, Jan; Pedersen, Thomas; Masini, Federico

    2016-01-01

    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.......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...

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

    Science.gov (United States)

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

    2016-01-01

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

  4. Watching Nanoparticles Form: An In Situ (Small-/Wide-Angle X-ray Scattering/Total Scattering) Study of the Growth of Yttria-Stabilised Zirconia in Supercritical Fluids

    DEFF Research Database (Denmark)

    Tyrsted, Christoffer; Pauw, Brian; Jensen, Kirsten Marie Ørnsbjerg

    2012-01-01

    Understanding nanoparticle formation reactions requires multitechnique in situ characterisation, since no single characterisation technique provides adequate information. Here, the first combined small-angle X-ray scattering (SAXS)/wide-angle X-ray scattering (WAXS)/total-scattering study of nano...... of nanoparticle formation is presented. We report on the formation and growth of yttria-stabilised zirconia (YSZ) under the extreme conditions of supercritical methanol for particles with Y2O3 equivalent molar fractions of 0, 4, 8, 12 and 25%....

  5. In situ X-ray diffraction study of the electrochemical reaction on lead electrodes in sulphate electrolytes

    International Nuclear Information System (INIS)

    Angerer, P.; Mann, R.; Gavrilovic, A.; Nauer, G.E.

    2009-01-01

    The anodic oxidation of pure lead in two acidic sulphate electrolytes with identical ionic strength (pH ∼ 0 and pH ∼ -0.1) was studied by in situ grazing incidence X-ray diffraction method (GIXD). Crystalline products such as lead sulphate (anglesite, PbSO 4 , orthorhombic), α- and β-lead dioxide (α-PbO 2 , orthorhombic, and β-PbO 2 , tetragonal), and tribasic lead sulphate hydrate with the stoichiometric composition 3PbO.PbSO 4 .H 2 O (triclinic) were detected at defined potentials. A method for the semi-quantitative determination of the thickness of the deposited layer from diffraction data is described. After the in situ measurement, the washed and dried working electrodes were additionally characterized ex situ by GIXD measurements at different angles of incidence. The phase litharge (lead oxide, t-PbO, tetragonal) and lead sulphate were observed at the surface of the lead substrate. The quantitative evaluation of the diffraction intensity of this measurement series enables the modelling of a qualitative depth profile of the layer generated during the electrochemical treatment. The anglesite phase is located in the uppermost layer, while the litharge phase was detected closer to the lead substrate

  6. In-situ reactive of x-ray optics by glow discharge

    International Nuclear Information System (INIS)

    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. Application of the nuclear x-ray fluorescence method to prospecting for gold in-situ

    International Nuclear Information System (INIS)

    Zhang, Y.; Xie, T.; Zhou, S.; Ge, L.

    1989-01-01

    Arsenic and chalcophile elements are often associated with gold, and can be considered indicator elements when prospecting for gold deposits. The nuclear geophysics X-ray fluorescence method can be used to search for hidden gold deposits by measuring fluorescence intensities of the indicator elements in situ. The method can speed geologic investigation and reduce exploration cost. Three types of portable radioisotope X-ray fluorescence analyzers, designed and manufactured by Chengdu College of Geology and Chongqing Geological Instrument Factory, are briefly introduced. These analyzers are widely used in different stages of geologic investigation for gold in China. In the two case histories presented five anomalous zones of X-ray fluorescence intensity related to gold mineralization are located and one hidden gold deposit is discovered with gold content of 23 g/t

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

    International Nuclear Information System (INIS)

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

    2015-01-01

    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 2 -adrenoreceptor–G 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 macromolecular

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

    International Nuclear Information System (INIS)

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

    2015-01-01

    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 Bi 2 O 3 -SiO 2 glass frit obtained during heating with ramp rates 5 °C s −1 and 100 °C s −1 , revealing numerous phase changes

  10. MapX An In Situ, Full-frame X-Ray Spectroscopic Imager for Planetary Science and Astrobiology

    Science.gov (United States)

    Blake, David; Sarrazin, Philippe; Thompson, Kathleen; Bristow, Thomas

    2017-01-01

    Microbial life exploits micron-scale disequilibria at boundaries where valence, chemical potential, pH, Eh, etc. vary on a length scale commensurate with the organisms - 10's to 100's of microns. The detection of accumulations of the biogenic elements C,N,O,P,S at appropriate concentrations on or in a mineral/ice substrate would constitute permissive evidence of extant life, but context is also required. Does the putative biosignature exist under habitable conditions? Under what conditions of P, T, and chemical potential was the host mineralogy formed? MapX is an in situ robotic spacecraft instrument that images the biogenic elements C, N, O, P, S, as well as the cations of the rock-forming minerals (Na, Mg, Al, Si, K, Ca, Ti, Cr, Mn, Fe) and important anions such as Cl, Fl. MapX provides element maps with less than or equal to100 microns resolution over a 2.5 cm X 2.5 cm area, as well as quantitative XRF spectra from ground- or instrument-selected Regions of Interest (ROI). XRF spectra are converted to mineralogies using ground- or instrument-based algorithms. Either X-ray tube or radioisotope sources such as 244Cm (Alpha-particle and gamma- ray fluorescence) can be used. Fluoresced sample Xrays are imaged onto an X-ray sensitive CCD through an X-ray MicroPore Optic (MPO). The MapX design as well as baseline performance requirements for a MapX instrument intended for life detection / identification of habitable environments will be presented.

  11. Structural and microstructural changes during anion exchange of CoAl layered double hydroxides: an in situ X-ray powder diffraction study

    DEFF Research Database (Denmark)

    Johnsen, Rune; Krumeich, Frank; Norby, Poul

    2010-01-01

    Anion-exchange processes in cobalt-aluminium layered double hydroxides (LDHs) were studied by in situ synchrotron X-ray powder diffraction (XRPD). The processes investigated were CoAl-CO3 CoAl-Cl CoAl-CO3, CoAl-Cl CoAl-NO3 and CoAl-CO3 CoAl-SO4. The XRPD data show that the CoAl-CO3 CoAl-Cl process...

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

    International Nuclear Information System (INIS)

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

    2007-01-01

    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

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

    Energy Technology Data Exchange (ETDEWEB)

    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.

  14. Local detection of X-ray spectroscopies with an in-situ Atomic Force Microscope

    International Nuclear Information System (INIS)

    Rodrigues, M S; Dhez, O; Denmat, S Le; Felici, R; Comin, F; Chevrier, J

    2008-01-01

    The in situ combination of Scanning Probe Microscopies with X-ray microbeams adds a variety of new possibilities to the panoply of synchrotron radiation techniques. This paper describes an optics-free Atomic Force Microscope that can be directly installed on most of the synchrotron radiation end-stations for combined X-ray and atomic force microscopy experiments. The instrument can be used for atomic force imaging of the investigated sample or to locally measure the X-ray absorption or diffraction, or it can also be used to mechanically interact with the sample while simultaneously taking spectroscopy or diffraction measurements. The local character of these measurements is intrinsically linked with the use of the Atomic Force Microscope tip. It is the sharp tip that gives the opportunity to measure the photons flux impinging on it, or to locally measure the absorption coefficient or the shape of the diffraction pattern. At the end an estimation of the limits of the various techniques presented is also discussed.

  15. In-Situ X-ray Tomography Study of Cement Exposed to CO2 Saturated Brine

    DEFF Research Database (Denmark)

    Chavez Panduro, E. A.; Torsæter, M.; Gawel, K.

    2017-01-01

    For successful CO2 storage in underground reservoirs, the potential problem of CO2 leakage needs to be addressed. A profoundly improved understanding of the behavior of fractured cement under realistic subsurface conditions including elevated temperature, high pressure and the presence of CO2...... saturated brine is required. Here, we report in situ X-ray micro computed tomography (μ-CT) studies visualizing the microstructural changes upon exposure of cured Portland cement with an artificially engineered leakage path (cavity) to CO2 saturated brine at high pressure. Carbonation of the bulk cement......, self-healing of the leakage path in the cement specimen, and leaching of CaCO3 were thus directly observed. The precipitation of CaCO3, which is of key importance as a possible healing mechanism of fractured cement, was found to be enhanced in confined regions having limited access to CO2...

  16. In Situ High Resolution Synchrotron X-Ray Powder Diffraction Studies of Lithium Batteries

    DEFF Research Database (Denmark)

    Amri, Mahrez; Fitch, Andy; Norby, Poul

    2015-01-01

    allowing diffraction information to be obtained from only the active material during battery operation [2]. High resolution synchrotron x-ray powder diffraction technique has been undertaken to obtain detailed structural and compositional information during lithiation/delithiation of commercial LiFePO4...... materials [3]. We report results from the first in situ time resolved high resolution powder diffraction experiments at beamline ID22/31 at the European Synchrotron Radiation Facility, ESRF. We follow the structural changes during charge of commercial LiFePO4 based battery materials using the Rietveld...... method. Conscientious Rietveld analysis shows slight but continuous deviation of lattice parameters from those of the fully stoichiometric end members LiFePO4 and FePO4 indicating a subsequent variation of stoichiometry during cathode delithiation. The application of an intermittent current pulses during...

  17. Perspectives of in situ/operando resonant inelastic X-ray scattering in catalytic energy materials science

    Energy Technology Data Exchange (ETDEWEB)

    Liu, Yi-Sheng; Glans, Per-Anders [Advanced Light Source, Lawrence Berkeley National Laboratory, Berkeley, CA 94720 (United States); Chuang, Cheng-Hao [Advanced Light Source, Lawrence Berkeley National Laboratory, Berkeley, CA 94720 (United States); Department of Physics, Tamkang University, Tamsui 250, Taiwan, ROC (China); Kapilashrami, Mukes [Center for Engineering Concepts Development, Department of Mechanical Engineering, University of Maryland, College Park, MD 20742 (United States); Advanced Light Source, Lawrence Berkeley National Laboratory, Berkeley, CA 94720 (United States); Guo, Jinghua, E-mail: jguo@lbl.gov [Advanced Light Source, Lawrence Berkeley National Laboratory, Berkeley, CA 94720 (United States); Department of Chemistry and Biochemistry, University of California, Santa Cruz, CA 95064 (United States)

    2015-04-15

    Highlights: • In-situ/operando soft X-ray RXES and RIXS offer unique perspectives in the energy material science. - Abstract: Growing environmental concerns have renewed the interest for light induced catalytic reactions to synthesize cleaner chemical fuels from syngas. This, however, requires a sound understanding for the dynamics taking place at molecular level as a result of light – matter interaction. We present herein the principles of soft X-ray resonant emission spectroscopy (RXES) and resonant inelastic scattering (RIXS) and the importance of these spectroscopic techniques in materials science in light of their unique ability to emanate characteristic fingerprints on the geometric structure, chemical bonding charge and spin states in addition to chemical sensitivity. The addition of in situ/operando RXES and RIXS capability offers new opportunities to project important material properties and functionalities under conditions nearly identical to the operational modes.

  18. Perspectives of in situ/operando resonant inelastic X-ray scattering in catalytic energy materials science

    International Nuclear Information System (INIS)

    Liu, Yi-Sheng; Glans, Per-Anders; Chuang, Cheng-Hao; Kapilashrami, Mukes; Guo, Jinghua

    2015-01-01

    Highlights: • In-situ/operando soft X-ray RXES and RIXS offer unique perspectives in the energy material science. - Abstract: Growing environmental concerns have renewed the interest for light induced catalytic reactions to synthesize cleaner chemical fuels from syngas. This, however, requires a sound understanding for the dynamics taking place at molecular level as a result of light – matter interaction. We present herein the principles of soft X-ray resonant emission spectroscopy (RXES) and resonant inelastic scattering (RIXS) and the importance of these spectroscopic techniques in materials science in light of their unique ability to emanate characteristic fingerprints on the geometric structure, chemical bonding charge and spin states in addition to chemical sensitivity. The addition of in situ/operando RXES and RIXS capability offers new opportunities to project important material properties and functionalities under conditions nearly identical to the operational modes.

  19. A flow cell for transient voltammetry and in situ grazing incidence X-ray diffraction characterization of electrocrystallized cadmium(II) tetracyanoquinodimethane

    Energy Technology Data Exchange (ETDEWEB)

    Veder, Jean-Pierre [Nanochemistry Research Institute, Department of Chemistry, Curtin University, GPO Box U1987, Perth, Western Australia 6845 (Australia); Nafady, Ayman [School of Chemistry, Monash University, Clayton, Victoria 3800 (Australia); Clarke, Graeme [Nanochemistry Research Institute, Department of Chemistry, Curtin University, GPO Box U1987, Perth, Western Australia 6845 (Australia); Williams, Ross P. [Centre for Materials Research, Department of Imaging and Applied Physics, Curtin University, GPO Box U1987, Perth, Western Australia 6845 (Australia); De Marco, Roland, E-mail: r.demarco@curtin.edu.a [Nanochemistry Research Institute, Department of Chemistry, Curtin University, GPO Box U1987, Perth, Western Australia 6845 (Australia); Bond, Alan M. [School of Chemistry, Monash University, Clayton, Victoria 3800 (Australia)

    2011-01-01

    An easy to fabricate and versatile cell that can be used with a variety of electrochemical techniques, also meeting the stringent requirement for undertaking cyclic voltammetry under transient conditions in in situ electrocrystallization studies and total external reflection X-ray analysis, has been developed. Application is demonstrated through an in situ synchrotron radiation-grazing incidence X-ray diffraction (SR-GIXRD) characterization of electrocrystallized cadmium (II)-tetracyanoquinodimethane material, Cd(TCNQ){sub 2}, from acetonitrile (0.1 mol dm{sup -3} [NBu{sub 4}][PF{sub 6}]). Importantly, this versatile cell design makes SR-GIXRD suitable for almost any combination of total external reflection X-ray analysis (e.g., GIXRF and GIXRD) and electrochemical perturbation, also allowing its application in acidic, basic, aqueous, non-aqueous, low and high flow pressure conditions. Nevertheless, the cell design separates the functions of transient voltammetry and SR-GIXRD measurements, viz., voltammetry is performed at high flow rates with a substantially distended window to minimize the IR (Ohmic) drop of the electrolyte, while SR-GIXRD is undertaken using stop-flow conditions with a very thin layer of electrolyte to minimize X-ray absorption and scattering by the solution.

  20. In situ observation of Cu-Ni alloy nanoparticle formation by X-ray diffraction, X-ray absorption spectroscopy, and transmission electron microscopy: Influence of Cu/Ni ratio

    DEFF Research Database (Denmark)

    Wu, Qiongxiao; Duchstein, Linus Daniel Leonhard; Chiarello, Gian Luca

    2014-01-01

    Silica-supported, bimetallic Cu-Ni nanomaterials were prepared with different ratios of Cu to Ni by incipient wetness impregnation without a specific calcination step before reduction. Different in situ characterization techniques, in particular transmission electron microscopy (TEM), X-ray...... diffraction (XRD), and X-ray absorption spectroscopy (XAS), were applied to follow the reduction and alloying process of Cu-Ni nanoparticles on silica. In situ reduction of Cu-Ni samples with structural characterization by combined synchrotron XRD and XAS reveals a strong interaction between Cu and Ni species......, which results in improved reducibility of the Ni species compared with monometallic Ni. At high Ni concentrations silica-supported Cu-Ni alloys form a homogeneous solid solution of Cu and Ni, whereas at lower Ni contents Cu and Ni are partly segregated and form metallic Cu and Cu-Ni alloy phases. Under...

  1. In-situ real-time x-ray scattering for probing the processing-structure-performance relation

    KAUST Repository

    Smilgies, Detlef-M.

    2014-01-01

    © 2014 Materials Research Society. In-situ X-ray scattering methodology is discussed, in order to analyze the microstructure development of soft functional materials during coating, annealing, and drying processes in real-time. The relevance of a fundamental understanding of coating processes for future industrial production is pointed out.

  2. High-temperature dehydration of talc: a kinetics study using in situ X-ray powder diffraction

    Science.gov (United States)

    Wang, Duojun; Yi, Li; Huang, Bojin; Liu, Chuanjiang

    2015-06-01

    High-temperature in situ X-ray powder diffraction patterns were used to study the dehydration kinetics of natural talc with a size of 10-15 µm. The talc was annealed from 1073 to 1223 K, and the variations in the characteristic peaks corresponding to talc with the time were recorded to determine the reaction progress. The decomposition of talc occurred, and peaks corresponding to talc and peaks corresponding to enstatite and quartz were observed. The enstatite and talc exhibited a topotactic relationship. The dehydration kinetics of talc was studied as a function of temperature between 1073 and 1223 K. The kinetics data could be modeled using an Avrami equation that considers nucleation and growth processes ? where n varies from 0.4 to 0.8. The rate constant (k) equation for the natural talc is ? The reaction mechanism for the dehydration of talc is a heterogeneous nucleation and growth mechanism.

  3. Fabrication and testing of an electrochemical microcell for in situ soft X-ray microspectroscopy measurements

    Science.gov (United States)

    Gianoncelli, A.; Kaulich, B.; Kiskinova, M.; Mele, C.; Prasciolu, M.; Sgura, I.; Bozzini, B.

    2013-03-01

    In this paper we report on the fabrication and testing of a novel concept of electrochemical microcell for in-situ soft X-ray microspectroscopy in transmission. The microcell, fabricated by electron-beam lithography, implements an improved electrode design, with optimal current density distribution and minimised ohmic drop, allowing the same three-electrode electrochemical control achievable with traditional cells. Moreover standard electroanalytical measurements, such as cyclic voltammetry, can be routinely performed. As far as the electrolyte is concerned, we selected a room-temperature ionic-liquid. Some of the materials belonging to this class, in addition to a broad range of outstanding electrochemical properties, feature two highlights that are crucial for in situ, soft X-ray transmission work: spinnability, enabling accurate thickness control, and stability to UHV, allowing operation of an open cell in the analysis chamber vacuum (10-6 mbar). The cell can, of course, be used also with non-vacuum stable electrolytes in the sealed version developed in previous work in our group. In this study, the microcell designed, fabricated and tested in situ by applying an anodic polarisation to a Au electrode and following the formation of a distribution of corrosion features. This specific material combination presented in this work does not limit the cell concept, that can implement any electrodic material grown by lithography, any liquid electrolyte and any spinnable solid electrolyte.

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

    International Nuclear Information System (INIS)

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

    1995-01-01

    Synchrotron X-ray scattering techniques provide a powerful tool for the in situ study of atomic scale processes occurring at solid-liquid interfaces. We have applied these techniques to characterize and study reactions at mineral-water interfaces. Here we present two examples. The first is the characterization of the calcite (CaCO 3 ) (10 bar 14) cleavage surface, in equilibrium with deionized water, by crystal truncation rod measurements. The second is the in situ study of the heteroepitaxial growth of otavite (CdCO 3 ) on the calcite (10 bar 14) cleavage surface. The results of such studies will lead to significant progress in understanding mineral-water interface geochemistry

  5. X-ray absorption spectroscopy study of the LixFePO4 cathode during cycling using a novel electrochemical in situ reaction cell

    International Nuclear Information System (INIS)

    Deb, A.; Bergmann, U.; Cairns, E.L.; California Univ., Berkeley, CA; Cramer, S.P.; California Univ., Davis, CA

    2004-01-01

    The extraction and insertion of lithium in LiFePO 4 has been investigated in practical Li-ion intercalation electrodes for Li-ion batteries using Fe K-edge X-ray absorption spectroscopy (XAS). A versatile electrochemical in situ reaction cell was utilized, specifically designed for long-term X-ray experiments on battery electrodes during the lithium-extraction/insertion process in electrode materials for Li-ion batteries. The electrode contained about 7.7 mg of LiFePO 4 on a 20 μm-thick Al foil. In order to determine the charge compensation mechanism and structural perturbations occurring in the system during cycling, in situ X-ray absorption fine-structure spectroscopy (XAFS) measurements were conducted on the cell at a moderate rate using typical Li-ion battery operating voltages (3.0-4.1 V versus Li/Li + ).XAS studies of the LiFePO 4 electrode measured at the initial state (LiFePO 4 ) showed iron to be in the Fe(II) state corresponding to the initial state (0.0 mAh) of the battery, whereas in the delithiated state (FePO 4 ) iron was found to be in the FE(III) state corresponding to the final charged state (3 m Ah) of the battery. The X-ray absorption near-edge structure (XANES) region of the XAS spectra revealed a high-spin configuration for the two states [Fe(II), d 6 and Fe(III), d 5 ]. The XAFS data analysis confirmed that the olivine structure of the LeFePO 4 and FePO 4 is retained by the electrodes, which is in agreement with the X-ray diffraction observations on these compounds. The XAFS data that were collected continuously during cycling revealed details about the response of the cathode to Li insertion and extraction. These measurements on the LiFePO 4 cathode show that the material retains good structural short-range order leading to superior cycling

  6. In situ X-ray diffraction study of crystallization process of GeSbTe thin films during heat treatment

    International Nuclear Information System (INIS)

    Kato, Naohiko; Konomi, Ichiro; Seno, Yoshiki; Motohiro, Tomoyoshi

    2005-01-01

    The crystallization processes of the Ge 2 Sb 2 Te 5 thin film used for PD and DVD-RAM were studied in its realistic optical disk film configurations for the first time by X-ray diffraction using an intense X-ray beam of a synchrotron orbital radiation facility (SPring-8) and in situ quick detection with a Position-Sensitive-Proportional-Counter. The dependence of the amorphous-to-fcc phase-change temperature T 1 on the rate of temperature elevation R et gave an activation energy E a : 0.93 eV much less than previously reported 2.2 eV obtained from a model sample 25-45 times thicker than in the real optical disks. The similar measurement on the Ge 4 Sb 1 Te 5 film whose large reflectance change attains the readability by CD-ROM drives gave E a : 1.13 eV with larger T 1 than Ge 2 Sb 2 Te 5 thin films at any R et implying a lower sensitivity in erasing as well as a better data stability of the phase-change disk

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

    Energy Technology Data Exchange (ETDEWEB)

    Ahmad, Md. Imteyaz; Van Campen, Douglas G.; Yu, Jiafan; Pool, Vanessa L.; Van Hest, Maikel F. A. M.; Toney, Michael F., E-mail: mftoney@slac.stanford.edu [SSRL, SLAC National Accelerator Laboratory, 2575, Sand Hill Road, Menlo Park, California 94025 (United States); Fields, Jeremy D.; Parilla, Philip A.; Ginley, David S. [National Renewable Energy Laboratory, Golden, Colorado 80401 (United States)

    2015-01-15

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

  8. Insight into the structure of Pd/ZrO2 during the total oxidation of methane using combined in situ XRD, X.-ray absorption and Raman spectroscopy

    DEFF Research Database (Denmark)

    Grunwaldt, Jan-Dierk; van Vegten, Niels; Baiker, Alfons

    2009-01-01

    The structure of palladium during the total combustion of methane has been studied by a combination of the complementary in situ techniques X-ray absorption spectroscopy, Raman spectroscopy and X-ray diffraction. The study demonstrates that finely dispersed and oxidized palladium is most active f...

  9. In-situ synchrotron x-ray study of the crystallization behavior of Ce0.9La0.1O2−x thin films deposited on NiW alloy substrates by chemical solution method

    DEFF Research Database (Denmark)

    Yue, Zhao; Grivel, Jean-Claude; Abrahamsen, Asger Bech

    2011-01-01

    The phase and texture formation of La doped CeO2 (CLO) films deposited by the chemical solution method are studied by in situ synchrotron x-ray diffraction. It is found that the CLO crystallites forms excellent in-plane texture as soon as the phase appears at 860°C, indicating that interfacial nu...... by diffusion. The success of this work demonstrates the possibility of studying crystallization behaviors of solution derived films using a non-destructive method, which has the potential of being applicable to most types of thin film samples.......The phase and texture formation of La doped CeO2 (CLO) films deposited by the chemical solution method are studied by in situ synchrotron x-ray diffraction. It is found that the CLO crystallites forms excellent in-plane texture as soon as the phase appears at 860°C, indicating that interfacial...

  10. In situ x-ray fluorescence and californium-252 neutron activation analysis for marine and terrestrial mineral exploration

    International Nuclear Information System (INIS)

    Wogman, N.A.

    1976-12-01

    Instrumentation has been designed for in situ analysis of marine and terrestrial minerals using the techniques of x-ray fluorescence and neutron activation analysis. The energy-dispersive x-ray fluorescence analyzer allows more than 20 elements to be quantitatively measured at the 10 ppM level in water depths to 300 m. The analyzer consists of a solid cryogen-cooled Si(Li) detector, a 50 mCi 109 Cd or 57 Co excitation source, and an analyzer-computer system for data storage and manipulation. The neutron activation analysis, which is designed to measure up to 30 elements at parts per hundred to ppM levels, utilizes the man-made element 252 Cf as its neutron activation source. The resulting radioelements which emit characteristic gamma radiation are then analyzed in situ during 2- to 200-s counting intervals with Ge(Li) or NaI(T1) detector systems. An extension of this latter technique, which uses a 252 Cf- 235 U fueled subcritical multiplier, is also being studied. The subcritical facility allows the neutrons from the 252 Cf source to be multiplied, thus providing greater neutron flux. Details of these in situ analysis systems, actual in situ spectra, and recorded data are discussed with respect to the detection of minerals at their varying concentration levels. The system response of each illustrates its usefulness for various rapid environmental mineral exploration studies. These techniques can be utilized on terrestrial surfaces and marine or fresh water sediments. 5 figures, 2 tables

  11. Scanning transmission X-ray microscopy probe for in situ mechanism study of graphene-oxide-based resistive random access memory.

    Science.gov (United States)

    Nho, Hyun Woo; Kim, Jong Yun; Wang, Jian; Shin, Hyun-Joon; Choi, Sung-Yool; Yoon, Tae Hyun

    2014-01-01

    Here, an in situ probe for scanning transmission X-ray microscopy (STXM) has been developed and applied to the study of the bipolar resistive switching (BRS) mechanism in an Al/graphene oxide (GO)/Al resistive random access memory (RRAM) device. To perform in situ STXM studies at the C K- and O K-edges, both the RRAM junctions and the I0 junction were fabricated on a single Si3N4 membrane to obtain local XANES spectra at these absorption edges with more delicate I0 normalization. Using this probe combined with the synchrotron-based STXM technique, it was possible to observe unique chemical changes involved in the BRS process of the Al/GO/Al RRAM device. Reversible oxidation and reduction of GO induced by the externally applied bias voltages were observed at the O K-edge XANES feature located at 538.2 eV, which strongly supported the oxygen ion drift model that was recently proposed from ex situ transmission electron microscope studies.

  12. CCD-based X-ray detectors for X-ray diffraction studies

    International Nuclear Information System (INIS)

    Ito, K.; Amemiya, Y.

    1999-01-01

    CCD-based X-ray detectors are getting to be used for X-ray diffraction studies especially in the studies where real time (automated) measurements and time-resolved measurements are required. Principles and designs of two typical types of CCD-based detectors are described; one is ths system in which x-ray image intensifiers are coupled to maximize the detective quantum efficiency for time-resolved measurements, and the other is the system in which tapered optical fibers are coupled for the reduction of the image into the CCD, which is optimized for automated measurements for protein crystallography. These CCD-based X-ray detectors have an image distortion and non-uniformity of response to be corrected by software. Correction schemes which we have developed are also described. (author)

  13. X-ray Diffraction Study of Arsenopyrite at High Pressure

    Energy Technology Data Exchange (ETDEWEB)

    D Fan; M Ma; W Zhou; S Wei; Z Chen; H Xie

    2011-12-31

    The high-pressure X-ray diffraction study of a natural arsenopyrite was investigated up to 28.2 GPa using in situ angle-dispersive X-ray diffraction and a diamond anvil cell at National Synchrotron Light Source, Brookhaven National Laboratory. The 16:3:1 methanol-ethanol-water mixture was used as a pressure-transmitting medium. Pressures were measured using the ruby-fluorescence method. No phase change has been observed up to 28.2 GPa. The isothermal equation of state (EOS) was determined. The values of K{sub 0}, and K'{sub 0} refined with a third-order Birch-Murnaghan EOS are K{sub 0} = 123(9) GPa, and K'{sub 0} = 5.2(8). Furthermore, we confirm that the linear compressibilities ({beta}) along a, b and c directions of arsenopyrite is elastically isotropic ({beta}{sub a} = 6.82 x 10{sup -4}, {beta}{sub b} = 6.17 x 10{sup -4} and {beta}{sub c} = 6.57 x 10{sup -4} GPa{sup -1}).

  14. XRMON-GF: A novel facility for solidification of metallic alloys with in situ and time-resolved X-ray radiographic characterization in microgravity conditions

    Science.gov (United States)

    Nguyen-Thi, H.; Reinhart, G.; Salloum Abou Jaoude, G.; Mathiesen, R. H.; Zimmermann, G.; Houltz, Y.; Voss, D.; Verga, A.; Browne, D. J.; Murphy, A. G.

    2013-07-01

    As most of the phenomena involved during the growth of metallic alloys from the melt are dynamic, in situ and time-resolved X-ray imaging should be retained as the method of choice for investigating the solidification front evolution. On Earth, the gravity force is the major source of various disturbing effects (natural convection, buoyancy/sedimentation, and hydrostatic pressure) which can significantly modify or mask certain physical mechanisms. Therefore solidification under microgravity is an efficient way to eliminate such perturbations to provide unique benchmark data for the validation of models and numerical simulations. Up to now, in situ observation during microgravity solidification experiments were limited to the investigations on transparent organic alloys, using optical methods. On the other hand, in situ observation on metallic alloys generally required synchrotron facilities. This paper reports on a novel facility we have designed and developed to investigate directional solidification on metallic alloys in microgravity conditions with in situ X-ray radiography observation. The facility consists of a Bridgman furnace and an X-ray radiography device specifically devoted to the study of Al-based alloys. An unprecedented experiment was recently performed on board a sounding rocket, with a 6 min period of microgravity. Radiographs were successfully recorded during the entire experiment including the melting and solidification phases of the sample, with a Field-of-View of about 5 mm×5 mm, a spatial resolution of about 4 µm and a frequency of 2 frames per second. Some preliminary results are presented on the solidification of the Al-20 wt% Cu sample, which validate the apparatus and confirm the potential of in situ X-ray characterization for the investigation of dynamical phenomena in materials processing, and particularly for the studying of metallic alloys solidification.

  15. In situ X-ray and neutron diffraction study of Ba2In2O5

    International Nuclear Information System (INIS)

    Speakman, S.A.; Misture, S.T.

    2001-01-01

    Order-disorder transitions in barium indate, Ba 2 In 2 O 5 , have been studied using in-situ X-ray and neutron diffraction. At room temperature, the crystal structure is an orthorhombic brownmillerite structure. At 706 C, the crystal structure is orthorhombic, possibly of the Imma or Ibm2 space groups. At 900 C, oxygen vacancies begin to disorder. The order-disorder transition occurs slowly in two steps over a temperature range of 900 - 925 C. Above this temperature range, the crystal structure is tetragonal, most likely belonging to the space group I 4/mcm. A second order-disorder transition begins at 1040 C, and proceeds over the temperature range 1040 - 1065 C. Above this temperature range, the crystal structure is a cubic, oxygen-deficient perovskite structure, with space group Pm3m. At an undetermined temperature above 1200 C, Ba 2 In 2 O 5 begins to decompose. (orig.)

  16. Investigation of a novel x-ray tube for the calibration of the x-ray crystal spectrometer in the KSTAR machine

    International Nuclear Information System (INIS)

    Bak, J.G.; Lee, S.G.

    2007-01-01

    A novel x-ray tube with a line filament has been developed for the in-situ calibration of the x-ray crystal spectrometer (XCS) in the KSTAR machine. The characteristics of the x-ray tube are investigated from the x-ray images obtained by using a pinhole and a CCD detector. It is found that the image has the width of about 0.1 mm, which is much improved as compared with the previous experimental results. In addition, there is a uniform region around the center of the image within its full length of 13.5 mm. This work may lead to the development of a novel x-ray tube with a line focus, which is required for the calibration of the XCS. Experimental results from the investigation of the x-ray tube are presented and the technical issues in a design of the in-situ calibration system using the x-ray tube for the KSTAR XCS are discussed. (author)

  17. An in situ synchrotron X-ray diffraction study of precipitation kinetics in a severely deformed Cu–Ni–Si alloy

    Energy Technology Data Exchange (ETDEWEB)

    Azzeddine, H.; Mehdi, B. [Faculty of Physics, USTHB, BP 32 El-Alia, Dar El Beida, Algiers (Algeria); Hennet, L. [Conditions Extrêmes et Matériaux: Haute Température et Irradiation, CNRS-CEMHTI, 1D Ave de la Recherche Scientifique, 45071 Orléans Cedex 2 (France); Thiaudière, D. [Synchrotron SOLEIL, L' Orme des Merisiers, Saint-Aubin, 91192 Gif-sur-Yvette Cedex (France); Alili, B. [Faculty of Physics, USTHB, BP 32 El-Alia, Dar El Beida, Algiers (Algeria); Kawasaki, M., E-mail: megumi@hanyang.ac.kr [Division of Materials Science and Engineering, Hanyang University, 17 Haengdang-dong, Seongdong-gu, Seoul 133-791 (Korea, Republic of); Departments of Aerospace and Mechanical Engineering and Materials Science, University of Southern California, Los Angeles, CA 90089-1453 (United States); Bradai, D. [Faculty of Physics, USTHB, BP 32 El-Alia, Dar El Beida, Algiers (Algeria); Langdon, T.G. [Departments of Aerospace and Mechanical Engineering and Materials Science, University of Southern California, Los Angeles, CA 90089-1453 (United States); Materials Research Group, Faculty of Engineering and the Environment, University of Southampton, Southampton SO17 1BJ (United Kingdom)

    2014-03-01

    In situ synchrotron X-ray diffraction was used to study the decomposition kinetics of a metastable Cu–2.5Ni–0.6Si (wt%) alloy after severe plastic deformation by equal-channel angular pressing (ECAP) and high-pressure torsion (HPT). The measurements were performed at room temperature and also at high temperatures of 723, 823 and 973 K in order to determine the ageing effect after processing. Two forms of precipitates, namely δ-Ni{sub 2}Si and γ-Ni{sub 5}Si{sub 2}, were identified and the sequence of their appearance was well established for ECAP processing and ageing. There was no detection of either a modulated structure resulting from spinodal decomposition or an ordered structure nucleated from the modulated structure. An X-ray hybrid pixel array detector (XPAD-S140 detector) permitted the detection of the nucleation stages of the δ-Ni{sub 2}Si phase that began soon after 24 s of ageing at 723 K. There was also no trace of any amorphization of the matrix phase.

  18. Thermal expansion and phase transformations of nitrogen-expanded austenite studied with in situ synchrotron X-ray diffraction

    DEFF Research Database (Denmark)

    Brink, Bastian; Ståhl, Kenny; Christiansen, Thomas Lundin

    2014-01-01

    Nitrogen-expanded austenite, _N, with high and low nitrogen contents was produced from AISI 316 grade stainless steel powder by gaseous nitriding in ammonia/hydrogen gas mixtures. In situ synchrotron X-ray diffraction was applied to investigate the thermal expansion and thermal stability...... as a fitting parameter. The stacking fault density is constant for temperatures up to 680 K, whereafter it decreases to nil. Surprisingly, a transition phase with composition M4N (M = Fe, Cr, Ni, Mo) appears for temperatures above 770 K. The linear coefficient of thermal expansion depends on the nitrogen...

  19. In situ X-ray diffraction study of crystallization process of GeSbTe thin films during heat treatment

    Energy Technology Data Exchange (ETDEWEB)

    Kato, Naohiko [Toyota Central R and D Labs., Inc., Nagakute, Aichi 480-1192 (Japan)]. E-mail: e0957@mosk.tytlabs.co.jp; Konomi, Ichiro [Toyota Central R and D Labs., Inc., Nagakute, Aichi 480-1192 (Japan); Seno, Yoshiki [Toyota Central R and D Labs., Inc., Nagakute, Aichi 480-1192 (Japan); Motohiro, Tomoyoshi [Toyota Central R and D Labs., Inc., Nagakute, Aichi 480-1192 (Japan)

    2005-05-15

    The crystallization processes of the Ge{sub 2}Sb{sub 2}Te{sub 5} thin film used for PD and DVD-RAM were studied in its realistic optical disk film configurations for the first time by X-ray diffraction using an intense X-ray beam of a synchrotron orbital radiation facility (SPring-8) and in situ quick detection with a Position-Sensitive-Proportional-Counter. The dependence of the amorphous-to-fcc phase-change temperature T{sub 1} on the rate of temperature elevation R{sub et} gave an activation energy E{sub a}: 0.93 eV much less than previously reported 2.2 eV obtained from a model sample 25-45 times thicker than in the real optical disks. The similar measurement on the Ge{sub 4}Sb{sub 1}Te{sub 5} film whose large reflectance change attains the readability by CD-ROM drives gave E{sub a}: 1.13 eV with larger T{sub 1} than Ge{sub 2}Sb{sub 2}Te{sub 5} thin films at any R{sub et} implying a lower sensitivity in erasing as well as a better data stability of the phase-change disk.

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

    International Nuclear Information System (INIS)

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

    2009-01-01

    In this paper we report an in situ X-ray microscopy study of a model metal electrochemistry system, incorporating faradaic reactivity: the anodic corrosion and cathodic electrodeposition of Ag in aqueous systems. The information at sub-μm scale about morpho-chemical evolution of the electrified interface, provided by this novel electroanalytical approach fosters fundamental understanding of important issues concerning material fabrication and stability, which are crucial in developing the next generation electrochemical technologies, such as fuel cells and biosensors. The key methodology challenge faced in this pilot electrochemical experiments is combining a three-electrode configuration and wet environment, which required metal electrodes suitable for transmitting soft X-rays and a sealed cell allowing working in high vacuum. This has been solved via lithographic fabrication route fabricating 75 nm thick Ag electrodes and using Si 3 N 4 membranes as X-ray windows and electrode support. Imaging in the STXM mode with phase contrast allowed us to monitor the corrosion morphologies and metal outgrowth features. Localised thickness variation and the build-up of reaction products of electron density different from that of the starting material have been detected with high sensitivity.

  1. In situ electrochemical high-energy X-ray diffraction using a capillary working electrode cell geometry

    Energy Technology Data Exchange (ETDEWEB)

    Young, Matthias J.; Bedford, Nicholas M.; Jiang, Naisheng; Lin, Deqing; Dai, Liming

    2017-05-26

    The ability to generate new electrochemically active materials for energy generation and storage with improved properties will likely be derived from an understanding of atomic-scale structure/function relationships during electrochemical events. Here, the design and implementation of a new capillary electrochemical cell designed specifically forin situhigh-energy X-ray diffraction measurements is described. By increasing the amount of electrochemically active material in the X-ray path while implementing low-Zcell materials with anisotropic scattering profiles, an order of magnitude enhancement in diffracted X-ray signal over traditional cell geometries for multiple electrochemically active materials is demonstrated. This signal improvement is crucial for high-energy X-ray diffraction measurements and subsequent Fourier transformation into atomic pair distribution functions for atomic-scale structural analysis. As an example, clear structural changes in LiCoO2under reductive and oxidative conditions using the capillary cell are demonstrated, which agree with prior studies. Accurate modeling of the LiCoO2diffraction data using reverse Monte Carlo simulations further verifies accurate background subtraction and strong signal from the electrochemically active material, enabled by the capillary working electrode geometry.

  2. Oxygen partial pressure control during in-situ high temperature X-ray diffraction on cerium dioxide

    International Nuclear Information System (INIS)

    Strach, M.; Belin, R.C.; Richaud, J-C.; Rogez, J.

    2014-01-01

    Cerium dioxide is widely used as a surrogate for plutonium dioxide in the studies of MOX type nuclear fuel. Thus, obtaining an accurate description of the structures present in this system in a range of temperatures is of importance to the development of fuel for the IV. generation of nuclear reactors. However, such a study requires appropriate scientific tools, in particular regarding the control and monitoring of the oxygen partial pressure (pO 2 ). Here we discuss several in-situ X-ray diffraction experiments performed to determine the phases present in the hypo-stoichiometric CeO 2-x region of the phase diagram and clearly demonstrate the need for controlling the pO 2 . (authors)

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

    Energy Technology Data Exchange (ETDEWEB)

    Zalkind, S., E-mail: shimonzl@nrcn.org.il; Rafailov, G.; Halevy, I.; Livneh, T.; Rubin, A.; Maimon, H.; Schweke, D.

    2017-03-15

    The oxidation kinetics of U-0.1 wt%Cr at oxygen pressures of 150 Torr and the temperature range of 90–150 °C was studied by means of in-situ X-ray diffraction (XRD). A “breakaway” in the oxidation kinetics is found at ∼0.25 μm, turning from a parabolic to a linear rate law. At the initial stage of oxidation the growth plane of UO{sub 2}(111) is the prominent one. As the oxide thickens, the growth rate of UO{sub 2}(220) plane increases and both planes grow concurrently. The activation energies obtained for the oxide growth are Q{sub parabolic} = 17.5 kcal/mol and Q{sub linear} = 19 kcal/mol. Enhanced oxidation around uranium carbide (UC) inclusions is clearly observed by scanning electron microscopy (SEM).

  4. Probing Stress States in Silicon Nanowires During Electrochemical Lithiation Using In Situ Synchrotron X-Ray Microdiffraction

    Directory of Open Access Journals (Sweden)

    Imran Ali

    2018-04-01

    Full Text Available Silicon is considered as a promising anode material for the next-generation lithium-ion battery (LIB due to its high capacity at nanoscale. However, silicon expands up to 300% during lithiation, which induces high stresses and leads to fractures. To design silicon nanostructures that could minimize fracture, it is important to understand and characterize stress states in the silicon nanostructures during lithiation. Synchrotron X-ray microdiffraction has proven to be effective in revealing insights of mechanical stress and other mechanics considerations in small-scale crystalline structures used in many important technological applications, such as microelectronics, nanotechnology, and energy systems. In the present study, an in situ synchrotron X-ray microdiffraction experiment was conducted to elucidate the mechanical stress states during the first electrochemical cycle of lithiation in single-crystalline silicon nanowires (SiNWs in an LIB test cell. Morphological changes in the SiNWs at different levels of lithiation were also studied using scanning electron microscope (SEM. It was found from SEM observation that lithiation commenced predominantly at the top surface of SiNWs followed by further progression toward the bottom of the SiNWs gradually. The hydrostatic stress of the crystalline core of the SiNWs at different levels of electrochemical lithiation was determined using the in situ synchrotron X-ray microdiffraction technique. We found that the crystalline core of the SiNWs became highly compressive (up to -325.5 MPa once lithiation started. This finding helps unravel insights about mechanical stress states in the SiNWs during the electrochemical lithiation, which could potentially pave the path toward the fracture-free design of silicon nanostructure anode materials in the next-generation LIB.

  5. Thin film growth studies using time-resolved x-ray scattering

    Science.gov (United States)

    Kowarik, Stefan

    2017-02-01

    Thin-film growth is important for novel functional materials and new generations of devices. The non-equilibrium growth physics involved is very challenging, because the energy landscape for atomic scale processes is determined by many parameters, such as the diffusion and Ehrlich-Schwoebel barriers. We review the in situ real-time techniques of x-ray diffraction (XRD), x-ray growth oscillations and diffuse x-ray scattering (GISAXS) for the determination of structure and morphology on length scales from Å to µm. We give examples of time resolved growth experiments mainly from molecular thin film growth, but also highlight growth of inorganic materials using molecular beam epitaxy (MBE) and electrochemical deposition from liquids. We discuss how scaling parameters of rate equation models and fundamental energy barriers in kinetic Monte Carlo methods can be determined from fits of the real-time x-ray data.

  6. In situ X-ray absorption fine structure studies on the structure of nickel phosphide catalyst supported on K-USY

    CERN Document Server

    Kawai, T; Suzuki, S

    2003-01-01

    Local structure around Ni in a nickel phosphide catalyst supported on K-USY was investigated by an situ X-ray absorption fine structure (XAFS) method during the reduction process of the catalyst and the hydrodesulfurization (HDS) reaction of thiophene. In the passivated sample, Ni phosphide was partially oxidized but after the reduction, 1.1 nm diameter Ni sub 2 P particles were formed with Ni-P and Ni-Ni distances at 0.218 and 0.261 nm, respectively, corresponding to those of bulk Ni sub 2 P. In situ XAFS cleary revealed that the Ni sub 2 P structure was stable under reaction conditions and was an active structure for the HDS process.

  7. In situ X-ray scattering studies of protein solution droplets drying on micro- and nanopatterned superhydrophobic PMMA surfaces.

    Science.gov (United States)

    Accardo, Angelo; Gentile, Francesco; Mecarini, Federico; De Angelis, Francesco; Burghammer, Manfred; Di Fabrizio, Enzo; Riekel, Christian

    2010-09-21

    Superhydrophobic poly(methyl methacrylate) surfaces with contact angles of ∼170° and high optical and X-ray transparencies have been fabricated through the use of optical lithography and plasma etching. The surfaces contain either a microscale pattern of micropillars or a random nanofibrillar pattern. Nanoscale asperities on top of the micropillars closely resemble Nelumbo nucifera lotus leaves. The evolution of the contact angle of water and lysozyme solution droplets during evaporation was studied on the micro- and nanopatterned surfaces, showing in particular contact-line pinning for the protein solution droplet on the nanopatterned surface. The microstructural evolution of lysozyme solution droplets was studied on both types of surfaces in situ under nearly contact-free conditions by synchrotron radiation microbeam wide-angle and small-angle X-ray scattering revealing the increasing protein concentration and the onset of precipitation. The solid residuals show hollow sphere morphologies. Rastermicrodiffraction of the detached residuals suggests about a 1/3 volume fraction of ≥17 nm lysozyme nanocrystalline domains and about a 2/3 short-range-order volume fraction. About 5-fold larger nanocrystalline domains were observed at the attachment points of the sphere to the substrates, which is attributed to particle growth in a shear flow. Such surfaces represent nearly contact-free sample supports for studies of inorganic and organic solution droplets, which find applications in biochips.

  8. Pyrophosphate-Inhibition of Apatite Formation Studied by In Situ X-Ray Diffraction

    Directory of Open Access Journals (Sweden)

    Casper Jon Steenberg Ibsen

    2018-02-01

    Full Text Available The pathways to crystals are still under debate, especially for materials relevant to biomineralization, such as calcium phosphate apatite known from bone and teeth. Pyrophosphate is widely used in biology to control apatite formation since it is a potent inhibitor of apatite crystallization. The impacts of pyrophosphate on apatite formation and crystallization kinetics are, however, not fully understood. Therefore, we studied apatite crystallization in water by synchrotron in situ X-ray diffraction. Crystallization was conducted from calcium chloride (0.2 M and sodium phosphate (0.12 M at pH 12 where hydrogen phosphate is the dominant phosphate species and at 60 °C to allow the synchrotron measurements to be conducted in a timely fashion. Following the formation of an initial amorphous phase, needle shaped crystals formed that had an octacalcium phosphate-like composition, but were too small to display the full 3D periodic structure of octacalcium phosphate. At later growth stages the crystals became apatitic, as revealed by changes in the lattice constant and calcium content. Pyrophosphate strongly inhibited nucleation of apatite and increased the onset of crystallization from minute to hour time scales. Pyrophosphate also reduced the rate of growth. Furthermore, when the pyrophosphate concentration exceeded ~1% of the calcium concentration, the resultant crystals had reduced size anisotropy suggesting that pyrophosphate interacts in a site-specific manner with the formation of apatite crystals.

  9. X-ray diffraction study of KTP (KTiOPO4) crystals under a static electric field

    International Nuclear Information System (INIS)

    Sebastian, M.T.; Klapper, H.; Bolt, R.J.

    1992-01-01

    X-ray diffraction studies are made on ion-conducting potassium titanyl phosphate (KTP) crystals with in situ DC electric field along different crystallographic directions. The X-ray rocking curves recorded with an electric field along the polar b axis (which is the direction of ion conduction) show a strong enhancement of the 040 reflection intensity (reflecting planes normal to the b axis) whereas the h0l reflections (reflecting planes parallel to the polar axis) do not show any intensity change. For an electric field normal to the polar axis no intensity change, either in 040 or in h0l reflections occurs. This observation is supplemented by X-ray topography. The 040 X-ray topographs recorded with in situ electric field along b exhibit strong extinction contrast in the form of striations parallel to the polar (ion-conduction) axis. The 040 intensity increase and the striation contrast are attributed to lattice deformation by the space-charge polarization due to the movement of the K + ions under the influence of the electric field. (orig.)

  10. Synchrotron radiation microbeam X-ray fluorescence analysis of zinc concentration in remineralized enamel in situ.

    Science.gov (United States)

    Matsunaga, Tsunenori; Ishizaki, Hidetaka; Tanabe, Shuji; Hayashi, Yoshihiko

    2009-05-01

    Remineralization is an indispensable phenomenon during the natural healing process of enamel decay. The incorporation of zinc (Zn) into enamel crystal could accelerate this remineralization. The present study was designed to investigate the concentration and distribution of Zn in remineralized enamel after gum chewing. The experiment was performed at the Photon Factory. Synchrotron radiation was monochromatized and X-rays were focused into a small beam spot. The X-ray fluorescence (XRF) from the sample was detected with a silicon (Si) (lithium (Li)) detector. X-ray beam energy was tuned to detect Zn. The examined samples were small enamel fragments remineralized after chewing calcium phosphate-containing gum in situ. The incorporation of Zn atom into hydroxyapatite (OHAP), the main component of enamel, was measured using Zn K-edge extended X-ray absorption fine structure (EXAFS) with fluorescence mode at the SPring-8. A high concentration of Zn was detected in a superficial area 10-microm deep of the sectioned enamel after gum chewing. This concentration increased over that in the intact enamel. The atomic distance between Zn and O in the enamel was calculated using the EXAFS data. The analyzed atomic distances between Zn and O in two sections were 0.237 and 0.240 nm. The present experiments suggest that Zn is effectively incorporated into remineralized enamel through the physiological processes of mineral deposition in the oral cavity through gum-chewing and that Zn substitution probably occurred at the calcium position in enamel hydroxyapatite.

  11. Radial Growth of Self-Catalyzed GaAs Nanowires and the Evolution of the Liquid Ga-Droplet Studied by Time-Resolved in Situ X-ray Diffraction.

    Science.gov (United States)

    Schroth, Philipp; Jakob, Julian; Feigl, Ludwig; Mostafavi Kashani, Seyed Mohammad; Vogel, Jonas; Strempfer, Jörg; Keller, Thomas F; Pietsch, Ullrich; Baumbach, Tilo

    2018-01-10

    We report on a growth study of self-catalyzed GaAs nanowires based on time-resolved in situ X-ray structure characterization during molecular-beam-epitaxy in combination with ex situ scanning-electron-microscopy. We reveal the evolution of nanowire radius and polytypism and distinguish radial growth processes responsible for tapering and side-wall growth. We interpret our results using a model for diameter self-stabilization processes during growth of self-catalyzed GaAs nanowires including the shape of the liquid Ga-droplet and its evolution during growth.

  12. Structural and microstructural changes during anion exchange of CoAl layered double hydroxides. An in situ X-ray powder diffraction study

    International Nuclear Information System (INIS)

    Johnsen, Rune E.; Krumeich, Frank; Norby, Poul

    2010-01-01

    Anion-exchange processes in cobalt-aluminium layered double hydroxides (LDHs) were studied by in situ synchrotron X-ray powder diffraction (XRPD). The processes investigated were CoAl-CO 3 →CoAl-Cl →CoAl-CO 3 , CoAl-Cl→CoAl-NO 3 and CoAl-CO 3 →CoAl-SO 4 . The XRPD data show that the CoAl-CO 3 →CoAl-Cl process is a two-phase transformation, where the amount of the CoAl-CO 3 phase decreases exponentially while that of the CoAl-Cl phase increases exponentially. Energy-dispersive X-ray spectroscopy (EDXS) studies of a partially chloride-exchanged CoAl-CO 3 LDH sample along with in situ XRPD data suggested that the individual particles in the CoAl-CO 3 sample are generally anion-exchanged with chloride one at a time. In contrast with the CoAl-CO 3 →CoAl-Cl transformation, the XRPD data show that the reverse CoAl-Cl→CoAl-CO 3 process is a one-phase transformation. Rietveld refinements indicate that the occupancy factors of the carbon and oxygen sites of the carbonate group increase, while that of the chloride site decreases. In the CoAl-Cl→CoAl-NO 3 anion-exchange reaction, the XRPD patterns reveal the existence of two intermediate phases in addition to the initial CoAl-Cl and final CoAl-NO 3 phases. The in situ data indicate that one of these intermediates is a mixed nitrate- and chloride-based LDH phase, where the disorder decreases as the nitrate content increases. The XRPD data of the partial CoAl-CO 3 →CoAl-SO 4 anion-exchange reaction show that the process is a two-phase transformation involving a sulfate-containing LDH with a 1H polytype structure. (orig.)

  13. In situ surface X-ray diffraction studies of the copper-electrolyte interface. Atomic structure and homoepitaxial grwoth

    Energy Technology Data Exchange (ETDEWEB)

    Golks, Frederik

    2011-05-19

    Copper electrodeposition is the predominantly used technique for on-chip wiring in the fabrication of ultra-large scale integrated (ULSI) microchips. In this 'damascene copper electroplating' process, multicomponent electrolytes containing organic additives realize void-free filling of trenches with high aspect ratio ('superconformal deposition'). Despite manifold studies, motivated by the continuous trend to shrink wiring dimensions and thus the demand of optimized plating baths, detailed knowledge on the growth mechanism - in presence and absence of additives - is still lacking. Using a recently developed hanging meniscus X-ray transmission cell, brilliant synchrotron x-rays and a fast, one-dimensional detector system, unique real-time in situ surface X-ray diffraction studies of copper electrodeposition were performed under realistic reaction conditions, approaching rates of technological relevance. Preparatory measurements of the electrochemical dissolution of Au(001) in chloride-containing electrolyte demonstrated the capability of this powerful technique, specifically the possibility to follow atomic-scale deposition or dissolution processes with a time resolution down to five milliseconds. The electrochemical as well as structural characterization of the Cu(001)- and Cu(111)-electrolyte interfaces provided detailed insight into the complex atomic-scale structures in presence of specifically adsorbed chloride on these surfaces. The interface of Cu(001) in chloride-containing electrolyte exhibits a continuous surface phase transition of a disordered Cl adlayer to a c(2 x 2) Cl adlayer with increasing potential. The latter was found to induce a small vertical corrugation of substrate atoms, which can be ascribed to lattice relaxations induced by the presence of coadsorbed water molecules and cations in the outer part of the electrochemical double layer. The study of the specific adsorption of chloride on Cu(111) from acidic aqueous

  14. In situ surface X-ray diffraction studies of the copper-electrolyte interface. Atomic structure and homoepitaxial grwoth

    Energy Technology Data Exchange (ETDEWEB)

    Golks, Frederik

    2011-05-19

    Copper electrodeposition is the predominantly used technique for on-chip wiring in the fabrication of ultra-large scale integrated (ULSI) microchips. In this 'damascene copper electroplating' process, multicomponent electrolytes containing organic additives realize void-free filling of trenches with high aspect ratio ('superconformal deposition'). Despite manifold studies, motivated by the continuous trend to shrink wiring dimensions and thus the demand of optimized plating baths, detailed knowledge on the growth mechanism - in presence and absence of additives - is still lacking. Using a recently developed hanging meniscus X-ray transmission cell, brilliant synchrotron x-rays and a fast, one-dimensional detector system, unique real-time in situ surface X-ray diffraction studies of copper electrodeposition were performed under realistic reaction conditions, approaching rates of technological relevance. Preparatory measurements of the electrochemical dissolution of Au(001) in chloride-containing electrolyte demonstrated the capability of this powerful technique, specifically the possibility to follow atomic-scale deposition or dissolution processes with a time resolution down to five milliseconds. The electrochemical as well as structural characterization of the Cu(001)- and Cu(111)-electrolyte interfaces provided detailed insight into the complex atomic-scale structures in presence of specifically adsorbed chloride on these surfaces. The interface of Cu(001) in chloride-containing electrolyte exhibits a continuous surface phase transition of a disordered Cl adlayer to a c(2 x 2) Cl adlayer with increasing potential. The latter was found to induce a small vertical corrugation of substrate atoms, which can be ascribed to lattice relaxations induced by the presence of coadsorbed water molecules and cations in the outer part of the electrochemical double layer. The study of the specific adsorption of chloride on Cu(111) from acidic aqueous electrolyte revealed a

  15. In situ multi-axial loading frame to probe elastomers using X-ray scattering.

    Science.gov (United States)

    Pannier, Yannick; Proudhon, Henry; Mocuta, Cristian; Thiaudière, Dominique; Cantournet, Sabine

    2011-11-01

    An in situ tensile-shear loading device has been designed to study elastomer crystallization using synchrotron X-ray scattering at the Synchrotron Soleil on the DiffAbs beamline. Elastomer tape specimens of thickness 2 mm can be elongated by up to 500% in the longitudinal direction and sheared by up to 200% in the transverse direction. The device is fully automated and plugged into the TANGO control system of the beamline allowing synchronization between acquisition and loading sequences. Experimental results revealing the evolution of crystallization peaks under load are presented for several tension/shear loading sequences.

  16. Beamline electrostatic levitator for in situ high energy x-ray diffraction studies of levitated solids and liquids

    Energy Technology Data Exchange (ETDEWEB)

    Gangopadhyay, A.K.; Lee, G.W.; Kelto, K.F.; Rogers, J.R.; Goldman, A.I.; Robinson, D.S.; Rathz, T.J.; Hyers, R.W. (WU); (UAB); (NASA); (UMASS, Amherst)

    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.

  17. On-line and in-situ x-ray diffraction analysis of the crystallisation of important pharmaceutical materials

    International Nuclear Information System (INIS)

    Hastings, S.

    1999-01-01

    Full text: The crystallisation process is an important unit operation for the separation and purification of many chemical products, particularly in the pharmaceutical industry. Variations in the conditions of crystallisation can lead to the formation of different polymorphic forms which are often meta-stable phases which results in phase conversion at different rates to the stable form. Our group, in collaboration with many industrial sponsors, have developed a number of online techniques which help to optimise the processing conditions of many of these specialty materials. In particular, on-line and in-situ X-ray diffraction (XRD) has been used to monitor the crystallisation of pharmaceutical materials. Several novel in-situ X-ray cells have been developed, in particular; a solution cell, which allows us to control and hence optimise crystallographic conditions such as temperature and pH whilst monitoring the crystal structure of the sample as it crystallises from solution. In conjunction with XRD data information on turbidity (% light transmittance) is taken to analyse solvent-mediated crystallisation. This technique gives information on the temperatures at which the system crystallises and dissolves. From this the meta-stable zone width (MSZW) can be calculated and then directly related to the crystal structure of the particles formed. The current system being studied is the crystallisation of stearic acid, a common pharmaceutical excipient, in various polar and non-polar solvents in order to ascertain the effect that the polarity of the solvent has on the polymorphic form crystallised. By combining such kinetic assessment with measurements of resulting particle structure the potential to optimise the process to produce optimal particle properties is obtainable. Copyright (1999) Australian X-ray Analytical Association Inc

  18. In situ analyses of Ag speciation in tissues of cucumber and wheat using synchrotron-based X-ray absorption spectroscopy

    Data.gov (United States)

    U.S. Environmental Protection Agency — In situ analyses of Ag speciation in tissues of cucumber and wheat using synchrotron-based X-ray absorption spectroscopy showing spectral fitting and linear...

  19. In situ observation of syntactic foams under hydrostatic pressure using X-ray tomography

    International Nuclear Information System (INIS)

    Lachambre, J.; Maire, E.; Adrien, J.; Choqueuse, D.

    2013-01-01

    Syntactic foams (hollow glass microspheres embedded in a polymeric matrix) are being used increasingly for the purpose of thermal insulation in ultradeep water. A better understanding of the damage mechanisms of these materials at the microsphere scale under such a hydrostatic loading condition is of prior importance in determining actual material limits, improving phenomenological modelling and developing novel formulations in the future. To achieve this goal, a study based on X-ray microtomography was performed on two syntactic foam materials (polypropylene and polyurethane matrix) and a standard foamed PP. A special set up has been designed in order to allow the X-ray microtomographic observation of the material during hydrostatic pressure loading using ethanol as the pressure fluid. Spatial resolution of (3.5 μm) 3 and in situ non-destructive scanning allowed a unique qualitative and quantitative analysis of the composite microstructure during stepwise isotropic compression by hydrostatic pressure up to 50 MPa. The collapse of weaker microspheres were observed during pressure increase and the damage parameters could be estimated. It is shown that the microspheres which are broken or the porosities which are close to the surface in the foamed PP are filled by a fluid (either the ethanol or the polymeric matrix itself). The hydrostatic pressure decreases the volume of the foam only slightly. In the PU matrix, ethanol diffusion is seen to induce swelling of the matrix, which is an unexpected phenomenon but reveals the high potential of X-ray microtomographic observation to improve diffusion analysis in complex media

  20. A geometrical approach for semi-automated crystal centering and in situ X-ray diffraction data collection

    International Nuclear Information System (INIS)

    Mohammad Yaser Heidari Khajepour; Ferrer, Jean-Luc; Lebrette, Hugo; Vernede, Xavier; Rogues, Pierrick

    2013-01-01

    High-throughput protein crystallography projects pushed forward the development of automated crystallization platforms that are now commonly used. This created an urgent need for adapted and automated equipment for crystal analysis. However, first these crystals have to be harvested, cryo-protected and flash-cooled, operations that can fail or negatively impact on the crystal. In situ X-ray diffraction analysis has become a valid alternative to these operations, and a growing number of users apply it for crystal screening and to solve structures. Nevertheless, even this shortcut may require a significant amount of beam time. In this in situ high-throughput approach, the centering of crystals relative to the beam represents the bottleneck in the analysis process. In this article, a new method to accelerate this process, by recording accurately the local geometry coordinates for each crystal in the crystallization plate, is presented. Subsequently, the crystallization plate can be presented to the X-ray beam by an automated plate-handling device, such as a six-axis robot arm, for an automated crystal centering in the beam, in situ screening or data collection. Here the preliminary results of such a semi-automated pipeline are reported for two distinct test proteins. (authors)

  1. An in situ near-ambient pressure X-ray Photoelectron Spectroscopy study of Mn polarised anodically in a cell with solid oxide electrolyte

    International Nuclear Information System (INIS)

    Bozzini, Benedetto; Amati, Matteo; Bocchetta, Patrizia; Dal Zilio, Simone; Knop-Gericke, Axel; Vesselli, Erik; Kiskinova, Maya

    2015-01-01

    This paper reports an in situ study of the anodic behavior of a model solid oxide electrolysis cell (SOEC) by means of near-ambient pressure X-ray Photoelectron Spectroscopy (XPS) combined with near edge X-ray absorption fine structure (NEXAFS) measurements. The focus is on the anodic surface chemistry of MnO x , a model anodic material already considered in cognate SOFC-related studies, during electrochemical operation in CO 2 , CO 2 /H 2 O and H 2 O ambients. The XPS and NEXAFS results we obtained, complemented by electrochemical measurements and SEM characterisation, reveal the chemical evolution of Mn under electrochemical control. MnO is the stable chemical form at open-circuit potential (OCP), while Mn 3 O 4 forms under anodic polarisation in all the investigated gas ambients. Carbon deposits are present on the Mn electrode at OCP, but they are readily oxidised under anodic conditions. Prolonged operation of the MnO x anode leads to pitting of the Mn films, damaging of the triple-phase boundary region and also to formation of discontinuities in the Mn patch. This is accompanied by chemical transformations of the electrolyte and formation of ZrC without impact on the surface chemistry of the Mn-based anode

  2. Reduction of variable-truncation artifacts from beam occlusion during in situ x-ray tomography

    Science.gov (United States)

    Borg, Leise; Jørgensen, Jakob S.; Frikel, Jürgen; Sporring, Jon

    2017-12-01

    Many in situ x-ray tomography studies require experimental rigs which may partially occlude the beam and cause parts of the projection data to be missing. In a study of fluid flow in porous chalk using a percolation cell with four metal bars drastic streak artifacts arise in the filtered backprojection (FBP) reconstruction at certain orientations. Projections with non-trivial variable truncation caused by the metal bars are the source of these variable-truncation artifacts. To understand the artifacts a mathematical model of variable-truncation data as a function of metal bar radius and distance to sample is derived and verified numerically and with experimental data. The model accurately describes the arising variable-truncation artifacts across simulated variations of the experimental setup. Three variable-truncation artifact-reduction methods are proposed, all aimed at addressing sinogram discontinuities that are shown to be the source of the streaks. The ‘reduction to limited angle’ (RLA) method simply keeps only non-truncated projections; the ‘detector-directed smoothing’ (DDS) method smooths the discontinuities; while the ‘reflexive boundary condition’ (RBC) method enforces a zero derivative at the discontinuities. Experimental results using both simulated and real data show that the proposed methods effectively reduce variable-truncation artifacts. The RBC method is found to provide the best artifact reduction and preservation of image features using both visual and quantitative assessment. The analysis and artifact-reduction methods are designed in context of FBP reconstruction motivated by computational efficiency practical for large, real synchrotron data. While a specific variable-truncation case is considered, the proposed methods can be applied to general data cut-offs arising in different in situ x-ray tomography experiments.

  3. Atoms in Action: Observing Atomic Motion with Dynamic in situ X-ray Diffraction

    Science.gov (United States)

    Cox, Jordan Michael

    Metal-organic framework (MOF) materials are rich in both structural diversity and application. These materials are comprised of metal atoms or clusters which are connected in a three-dimensional polymer-like network by bridging organic linker molecules. One of the major attractive features in MOFs is their permanent pore space which can potentially be used to adsorb or exchange foreign molecules from/with the surrounding environment. While MOFs are an active area of scientific interest, MOF materials are still relatively new, only 20 years old. As such, there is still much that needs to be understood about these materials before they can be effectively applied to widespread chemical problems like CO2 sequestration or low-pressure hydrogen fuel storage. One of the most important facets of MOF chemistry to understand in order to rationally design MOF materials with tailor-made properties is the relationship between the structural features in a MOF and the chemical and physical properties of that material. By examining in detail the atomic structure of a MOF with known properties under a variety of conditions, scientists can begin to unravel the guiding principles which govern these relationships. X-ray diffraction remains one of the most effective tools for determining the structure of a crystalline material with atomic resolution, and has been applied to the determination of MOF structures for years. Typically these experiments have been carried out using powder X-ray diffraction, but this technique lacks the high-resolution structural information found in single-crystal methods. Some studies have been reported which use specialized devices, sometimes called Environmental Control Cells, to study single crystalline MOFs under non-ambient chemical conditions in situ . However, these in situ studies are performed under static conditions. Even in cases where the ECC provides continued access to the local chemical environment during diffraction data collections, the

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

    Science.gov (United States)

    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.

  5. Texture evolution of orthorhombic α″ titanium alloy investigated by in situ X-ray diffraction

    Energy Technology Data Exchange (ETDEWEB)

    Elmay, W., E-mail: wafa.elmay@ensam.eu [Laboratoire d' Etude des Microstructures et de Mécanique des Matériaux LEM3 (UMR CNRS 7239), 4 rue Augustin Fresne, 57078 Metz (France); Berveiller, S.; Patoor, E. [Laboratoire d' Etude des Microstructures et de Mécanique des Matériaux LEM3 (UMR CNRS 7239), 4 rue Augustin Fresne, 57078 Metz (France); Gloriant, T. [Chimie-Métallurgie (UMR CNRS 6226), 20, Avenue des Buttes de Coesmes, F-35043 Rennes (France); Prima, F. [Laboratoire de Physico-Chimie des Surfaces (UMR CNRS 7045), 11 Rue Pierre et Marie Curie, F-75231 Paris (France); Laheurte, P. [Laboratoire d' Etude des Microstructures et de Mécanique des Matériaux LEM3 (UMR CNRS 7239), 4 rue Augustin Fresne, 57078 Metz (France)

    2017-01-02

    The present paper deals with an in-situ X-ray diffraction analysis during cyclic tensile tests of a fully martensitic Ti-24Nb alloy. Texture evolution of martensite α″ phase was followed during loading-unloading cycles. Preferential formation and reverse transformation of particular martensite variants have been observed based on pole figure analysis. The occurrence of the deformation mechanisms for the martensitic Ti-24Nb alloy was also commented by coupling microstructural observations during in-situ experiments and additional cyclic tests followed by heating after each unloading. Through the study of the evolution of the lattice strain, it was found that under loading conditions, the {020} planes exhibit a large tension lattice strain while the {200} planes are subjected to a compression solicitation, which causes the lattice parameters a and c to be shrunk, and b to be elongated.

  6. The effect of strain path change on subgrain volume fraction determined from in situ X-ray measurements

    DEFF Research Database (Denmark)

    Wejdemann, Christian; Poulsen, Henning Friis; Lienert, U.

    2009-01-01

    to additional 5% strain is performed in situ while mapping a selected X-ray reflection from one particular bulk grain with high angular resolution. The reciprocal space maps are analyzed with a recently developed fitting method, and a correlation is found between the evolution of the subgrain volume fraction...

  7. High Pressure In Situ X-ray Diffraction Study of MnO to 120 GPa and Comparison with Shock Compression Experiment

    Science.gov (United States)

    Yagi, Takehiko; Kondo, Tadashi; Syono, Yasuhiko

    1997-07-01

    In order to clarify the nature of the phase transformation in MnO observed at around 90 GPa by shock compression experiment (Syono et al., this symposium), high pressure in situ x-ray experiments were carried out up to 120 GPa. Powdered sample was directly compressed in Mao-Bell type diamond anvil and x-ray experiments were carried out using angle dispersive technique by combining synchrotron radiation and imaging plate detector. Distortion of the B1 structured phase into hexagonal unit cell was observed from 25-40 GPa, which continues to increase up to 90 GPa. At around 90 GPa, discontinuous change of the diffraction was observed. This new phase cannot be explained by a simple B2 structure and the analysis of this phase is in progress. This high pressure phase has metallic appearance, which reverses to transparent MnO on release of pressure.

  8. Formation and texture of palladium germanides studied by in situ X-ray diffraction and pole figure measurements

    Energy Technology Data Exchange (ETDEWEB)

    Geenen, F.A., E-mail: Filip.Geenen@UGent.be [Ghent University, Department of Solid-State Sciences, Krijgslaan 281 (S1), 9000 Gent (Belgium); Knaepen, W.; De Keyser, K. [Ghent University, Department of Solid-State Sciences, Krijgslaan 281 (S1), 9000 Gent (Belgium); Opsomer, K. [Interuniversitair Micro-Electronica Centrum (IMEC), Kapeldreef 75, 3001 Leuven (Belgium); Vanmeirhaeghe, R.L. [Ghent University, Department of Solid-State Sciences, Krijgslaan 281 (S1), 9000 Gent (Belgium); Jordan-Sweet, J.; Lavoie, C. [IBM T.J. Watson Research Center, Yorktown (United States); Detavernier, C. [Ghent University, Department of Solid-State Sciences, Krijgslaan 281 (S1), 9000 Gent (Belgium)

    2014-01-31

    The solid state reaction between 30 nm Pd films and various Ge substrates (Ge(100), Ge(111), polycrystalline Ge and amorphous Ge) was studied by means of in situ X-ray diffraction and in situ sheet resistance measurements. The reported phase sequence of Pd{sub 2}Ge followed by PdGe was verified on all substrates. The texture of the germanides was analysed by pole figure measurements on samples quenched in the Pd{sub 2}Ge and in the PdGe phase on both Ge(100) and (111) substrates. We report an epitaxial growth of Pd{sub 2}Ge on Ge(111) and on Ge(100). The formed PdGe has an axiotaxial alignment on Ge(111). On Ge(100), the axiotaxial texture is observed together with a fibre texture. The higher formation temperature of PdGe on Ge(111) could be related to the epitaxial alignment of the Pd{sub 2}Ge parent phase on Ge(111). - Highlights: • Solid-state reaction is studied on a Pd film with Ge substrates. • Pd2Ge grains have an epitaxial texture on both Ge 100 and Ge 111. • PdGe grains are found to grow with an axiotaxial texture. • Retarded PdGe formation on Ge111 is related with strong epitaxy of Pd2Ge.

  9. An in situ grazing incidence x-ray scattering study of block copolymer thin films during solvent vapor annealing

    Science.gov (United States)

    Gu, Xiaodan; Gunkel, Ilja; Hexemer, Alexander; Russell, Thomas

    2014-03-01

    Although solvent vapor annealing (SVA) has been widely applied to block copolymer (BCP) thin films to obtain well-ordered microdomains, the mechanism of enhancing lateral order is not well understood. Here, we used real time in situ grazing-incidence small-angle x-ray scattering (in situGISAXS) to study the self-assembly of PS-b-P2VP BCP BCPs with different molecular weights thin films in THF vapor, a near neutral solvent for both blocks. Both swelling and deswelling behavior of BCP thin films were examined. The extent of swellingand the solvent removal rate not only affect the domain spacing of BCPs but also dictate the extent of lateral ordering of the BCP microdomains. Larger grains were observed at higher values of the swelling ratio (close to disordering). To preserve the maximal lateral ordering of the microdomains in the swollen state, the fastest solvent removal rate is required to freeze in the ordered microdomain structure of the swollen BCP film. We thanks support from U.S. Department of Energy BES under contract BES-DE-FG02-96ER45612 and ALS doctoral fellowship.

  10. Nanocalorimeter platform for in situ specific heat measurements and x-ray diffraction at low temperature

    Science.gov (United States)

    Willa, K.; Diao, Z.; Campanini, D.; Welp, U.; Divan, R.; Hudl, M.; Islam, Z.; Kwok, W.-K.; Rydh, A.

    2017-12-01

    Recent advances in electronics and nanofabrication have enabled membrane-based nanocalorimetry for measurements of the specific heat of microgram-sized samples. We have integrated a nanocalorimeter platform into a 4.5 T split-pair vertical-field magnet to allow for the simultaneous measurement of the specific heat and x-ray scattering in magnetic fields and at temperatures as low as 4 K. This multi-modal approach empowers researchers to directly correlate scattering experiments with insights from thermodynamic properties including structural, electronic, orbital, and magnetic phase transitions. The use of a nanocalorimeter sample platform enables numerous technical advantages: precise measurement and control of the sample temperature, quantification of beam heating effects, fast and precise positioning of the sample in the x-ray beam, and fast acquisition of x-ray scans over a wide temperature range without the need for time-consuming re-centering and re-alignment. Furthermore, on an YBa2Cu3O7-δ crystal and a copper foil, we demonstrate a novel approach to x-ray absorption spectroscopy by monitoring the change in sample temperature as a function of incident photon energy. Finally, we illustrate the new insights that can be gained from in situ structural and thermodynamic measurements by investigating the superheated state occurring at the first-order magneto-elastic phase transition of Fe2P, a material that is of interest for magnetocaloric applications.

  11. In situ thermal residual stress evolution in ultrathin ZnO and Ag films studied by synchrotron x-ray diffraction

    Energy Technology Data Exchange (ETDEWEB)

    Renault, P.O., E-mail: Pierre.olivier.renault@univ-poitiers.fr [Institut P' , CNRS, Universite de Poitiers, UPR 3346, 86962 Futuroscope (France); Krauss, C.; Le Bourhis, E.; Geandier, G. [Institut P' , CNRS, Universite de Poitiers, UPR 3346, 86962 Futuroscope (France); Benedetto, A. [Saint-Gobain Recherche (SGR), 93303 Aubervilliers (France); Grachev, S.Y.; Barthel, E. [Lab. Surface du Verre et Interfaces (SVI), UMR-CNRS 125, 93303 Aubervilliers (France)

    2011-12-30

    Residual-stress evolution in sputtered encapsulated ZnO/Ag/ZnO stack has been studied in-situ by synchrotron x-ray diffraction when heat treated. The ZnO/Ag/ZnO stack encapsulated into Si{sub 3}N{sub 4} layers and deposited on (001) Si substrates was thermally heated from 25 Degree-Sign C to 600 Degree-Sign C and cooled down to 25 Degree-Sign C. X-ray diffraction 2D patterns captured continuously during the heat treatment allowed monitoring the diffraction peak shifts of both Ag (15 nm thick) and ZnO (10 nm and 50 nm thick) sublayers. Due to the mismatch between the coefficients of thermal expansion, the silicon substrate induced compressive thermal stresses in the films during heating. We first observed a linear increase of the compressive stress state in both Ag and ZnO films and then a more complex elastic-stress evolution starts to operate from about 100 Degree-Sign C for Ag and about 250 Degree-Sign C for ZnO. Thermal contraction upon cooling seems to dominate so that the initial compressive film stresses relax by about 300 and 700 MPa after thermal treatment for ZnO and Ag, respectively. The overall behavior is discussed in terms of structural changes induced by the heat treatment.

  12. Electrochemically adsorbed Pb on Ag (111) studied with grazing- incidence x-ray scattering

    International Nuclear Information System (INIS)

    Kortright, J.B.; Ross, P.N.; Melroy, O.R.; Toney, M.F.; Borges, G.L.; Samant, M.G.

    1989-04-01

    Grazing-incidence x-ray scattering studies of the evolution of electrochemically deposited layers of lead on silver (111) as a function of applied electrochemical potential are presented. Measurements were made with the adsorbed layers in contact with solution in a specially designed sample cell. The observed lead structures are a function of the applied potential and range from an incommensurate monolayer, resulting from underpotential deposition, to randomly oriented polycrystalline bulk lead, resulting from lower deposition potentials. These early experiments demonstrate the ability of in situ x-ray diffraction measurements to determine structures associated with electrochemical deposition. 6 refs., 4 figs

  13. Two methods for studying the X-ray variability

    NARCIS (Netherlands)

    Yan, Shu-Ping; Ji, Li; Méndez, Mariano; Wang, Na; Liu, Siming; Li, Xiang-Dong

    2016-01-01

    The X-ray aperiodic variability and quasi-periodic oscillation (QPO) are the important tools to study the structure of the accretion flow of X-ray binaries. However, the origin of the complex X-ray variability from X-ray binaries remains yet unsolved. We proposed two methods for studying the X-ray

  14. In-situ X-ray residual stress measurement on a peened alloy 600 weld metal at elevated temperature under tensile load

    International Nuclear Information System (INIS)

    Yunomura, Tomoaki; Maeguchi, Takaharu; Kurimura, Takayuki

    2014-01-01

    In order to verify stability of residual stress improvement effect of peeing for mitigation of stress corrosion cracking in components of PWR plant, relaxation behavior of residual stress induced by water jet peening (WJP) on surface of alloy 600 weld metal (alloy 132) was investigated by in-situ X-ray residual stress measurement under thermal aging and stress condition considered for actual plant operation. Surface residual stress change was observed at the early stage of thermal aging at 360°C, but no significant further stress relaxation was observed after that. Applied stress below yield stress does not significantly affect stress relaxation behavior of surface residual stress. For the X-ray residual stress measurement, X-ray stress constant at room temperature for alloy 600 was determined experimentally with several surface treatment and existence of applied strain. The X-ray stress constant at elevated temperatures were extrapolated theoretically based on the X-ray stress constant at room temperature for alloy 600. (author)

  15. Compact x-ray microradiograph for in situ imaging of solidification processes: Bringing in situ x-ray micro-imaging from the synchrotron to the laboratory

    Energy Technology Data Exchange (ETDEWEB)

    Rakete, C.; Baumbach, C.; Goldschmidt, A.; Samberg, D.; Schroer, C. G. [Institut fuer Strukturphysik, Technische Universitaet Dresden, D-01062 Dresden (Germany); Breede, F.; Stenzel, C. [Astrium-Space Transportation, Department: TO 611, Claude-Dornier-Strasse, D-88039 Friedrichshafen (Germany); Zimmermann, G.; Pickmann, C. [ACCESS e.V., Intzestrasse 5, D-52072 Aachen (Germany); Houltz, Y.; Lockowandt, C. [Science Services Division, SSC, Box 4207, SE-17104 Solna (Sweden); Svenonius, O.; Wiklund, P. [Scint-X AB, Torshamnsgatan 35, SE-164 40 Kista (Sweden); Mathiesen, R. H. [Inst. for Fysikk, NTNU, N-7491 Trondheim (Norway)

    2011-10-15

    A laboratory based high resolution x-ray radiograph was developed for the investigation of solidification dynamics in alloys. It is based on a low-power microfocus x-ray tube and is potentially appropriate for x-ray diagnostics in space. The x-ray microscope offers a high spatial resolution down to approximately 5 {mu}m. Dynamic processes can be resolved with a frequency of up to 6 Hz. In reference experiments, the setup was optimized to yield a high contrast for AlCu-alloys. With samples of about 150 {mu}m thickness, high quality image sequences of the solidification process were obtained with high resolution in time and space.

  16. Reflection-mode x-ray powder diffraction cell for in situ studies of electrochemical reactions

    International Nuclear Information System (INIS)

    Roberts, G.A.; Stewart, K.D.

    2004-01-01

    The design and operation of an electrochemical cell for reflection-mode powder x-ray diffraction experiments are discussed. The cell is designed for the study of electrodes that are used in rechargeable lithium batteries. It is designed for assembly in a glove box so that air-sensitive materials, such as lithium foil electrodes and carbonate-based electrolytes with lithium salts, can be used. The cell uses a beryllium window for x-ray transmission and electrical contact. A simple mechanism for compressing the electrodes is included in the design. Sample results for the cell are shown with a Cu Kα source and a position-sensitive detector

  17. In-situ x-ray characterization of wurtzite formation in GaAs nanowires

    Energy Technology Data Exchange (ETDEWEB)

    Krogstrup, Peter; Hannibal Madsen, Morten; Nygaard, Jesper; Feidenhans' l, Robert [Nano-Science Center, Niels Bohr Institute, University of Copenhagen, Copenhagen (Denmark); Hu Wen [Quantum Beam Science Directorate, Japan Atomic Energy Agency, 1-1-1 Koto, Sayo, Hyogo 679-5148 (Japan); Kozu, Miwa; Nakata, Yuka [University of Hyogo, 3-2-1 Koto, Kamigori, Hyogo 678-1297 (Japan); Takahasi, Masamitu [Quantum Beam Science Directorate, Japan Atomic Energy Agency, 1-1-1 Koto, Sayo, Hyogo 679-5148 (Japan); University of Hyogo, 3-2-1 Koto, Kamigori, Hyogo 678-1297 (Japan)

    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.

  18. Development of high-performance X-ray transparent crystallization plates for in situ protein crystal screening and analysis

    Energy Technology Data Exchange (ETDEWEB)

    Soliman, Ahmed S. M.; Warkentin, Matthew [Cornell University, Ithaca, New York (United States); Apker, Benjamin [MiTeGen LLC, Ithaca, New York (United States); Thorne, Robert E., E-mail: ret6@cornell.edu [Cornell University, Ithaca, New York (United States); MiTeGen LLC, Ithaca, New York (United States)

    2011-07-01

    An optically, UV and X-ray transparent crystallization plate suitable for in situ analysis has been developed. The plate uses contact line pinning rather than wells to confine the liquids. X-ray transparent crystallization plates based upon a novel drop-pinning technology provide a flexible, simple and inexpensive approach to protein crystallization and screening. The plates consist of open cells sealed top and bottom by thin optically, UV and X-ray transparent films. The plates do not need wells or depressions to contain liquids. Instead, protein drops and reservoir solution are held in place by rings with micrometre dimensions that are patterned onto the bottom film. These rings strongly pin the liquid contact lines, thereby improving drop shape and position uniformity, and thus crystallization reproducibility, and simplifying automated image analysis of drop contents. The same rings effectively pin solutions containing salts, proteins, cryoprotectants, oils, alcohols and detergents. Strong pinning by rings allows the plates to be rotated without liquid mixing to 90° for X-ray data collection or to be inverted for hanging-drop crystallization. The plates have the standard SBS format and are compatible with standard liquid-handling robots.

  19. Cell survival studies using ultrasoft x rays

    International Nuclear Information System (INIS)

    Schillaci, M.E.; Raju, M.R.; Carpenter, S.; Cornforth, M.; Wilder, M.

    1987-01-01

    Cell survival was studied for V79 hamster, 10T1/2 mouse, and human skin fibroblast cell lines, using carbon K (0.28 keV), copper K (8.0 keV), and 250 kVp x rays. Because of the rapid attenuation of the carbon x rays, cellular dimensions at the time of exposure were measured using optical and electron microscopy, and frequency distributions of mean dose absorbed by the cell nucleus were obtained. The results indicate that the differences in cell killing between ultra-soft and hard x rays may depend on the nuclear thickness of the cells. Studies of the effects of hypoxia on V79 and 10T1/2 cells using carbon K, aluminum K (1.5 keV), and copper K x rays show decreasing OER values with decreasing x-ray energy and no difference between the two cell lines. Age response studies with V79 cells show similar cell-cycle variation of survival for carbon K and aluminum K x rays as for hard x rays

  20. High pressure in-situ X-ray diffraction study on Zn-doped magnetite nanoparticles

    Science.gov (United States)

    Ferrari, S.; Bilovol, V.; Pampillo, L. G.; Grinblat, F.; Errandonea, D.

    2018-03-01

    We have performed high pressure synchrotron X-ray powder diffraction experiments on two different samples of Zn-doped magnetite nanoparticles (formula Fe(3-x)ZnxO4; x = 0.2, 0.5). The structural behavior of then a noparticles was studied up to 13.5 GPa for x = 0.2, and up to 17.4 GPa for x = 0.5. We have found that both systems remain in the cubic spinel structure as expected for this range of applied pressures. The analysis of the unit cell volume vs. pressure results in bulk modulus values lower than in both end-members, magnetite (Fe3O4) and zinc ferrite (ZnFe2O4), suggesting that chemical disorder may favor compressibility, which is expected to improve the increase of the Neel temperature under compression.

  1. In situ and ex situ electron microscopy and X-ray diffraction characterization of the evolution of a catalytic system - from synthesis to deactivation

    DEFF Research Database (Denmark)

    Gardini, Diego

    Heterogeneous catalysis represents a research field of undeniable importance for a multitude of technological and industrial processes. Supported catalysts are nowadays at the base of the large-scale production of most chemicals and are used for the removal of air pollutants from automotive engines...... the understanding of the structural properties and mechanisms at the origin of catalytic activity. This thesis presents the potential and uniqueness of ex situ and in situ transmission electron microscopy (TEM) and X-ray diffraction (XRD) techniques in the characterization of several supported material systems...... TEM (HRTEM) and electron energy loss spectroscopy (EELS) revealed the degradation of the supported carbide particles probably due to the formation of volatile molybdenum hydroxide species. The activity of silver nanoparticles as catalyst for soot oxidation was studied in operative conditions...

  2. Study of the thermal transformations of Co- and Fe-exchanged zeolites A and X by 'in situ' XRD under reducing atmosphere

    Energy Technology Data Exchange (ETDEWEB)

    Ronchetti, Silvia, E-mail: silvia.ronchetti@polito.it [Dipartimento di Scienza dei Materiali e Ingegneria Chimica, Politecnico di Torino, Corso Duca degli Abruzzi 24, 10129 Torino (Italy); Turcato, Elisa Aurelia; Delmastro, Alessandro [Dipartimento di Scienza dei Materiali e Ingegneria Chimica, Politecnico di Torino, Corso Duca degli Abruzzi 24, 10129 Torino (Italy); Esposito, Serena; Ferone, Claudio; Pansini, Michele [Laboratorio Materiali del Dipartimento di Meccanica, Strutture, Ambiente e Territorio, Facolta di Ingegneria dell' Universita di Cassino, Via G. Di Biasio 43, 03043 Cassino (Italy); Onida, Barbara; Mazza, Daniele [Dipartimento di Scienza dei Materiali e Ingegneria Chimica, Politecnico di Torino, Corso Duca degli Abruzzi 24, 10129 Torino (Italy)

    2010-06-15

    'In situ' high temperature X-ray diffraction under reducing atmosphere is used for the first time to study the thermal stability and transformations of Co- and Fe-exchanged A and X zeolites. TG-DTA and 'ex situ' XRD characterization were also carried out. The temperature of incipient crystallization of metallic phase was found to be 700 {sup o}C in Fe-zeolites and 800 {sup o}C in Co-zeolites. Moreover, ex situ X-ray experiments, after thermal treatment both under inert and reducing atmosphere, revealed the formation of ceramic phases upon the thermal collapse of the zeolitic framework. Metal nanoparticles were obtained by reduction and the size of metal clusters was found to range between 24 and 40 nm.

  3. X-ray irradiation induced reduction and nanoclustering of lead in borosilicate glass

    NARCIS (Netherlands)

    Stanley, H.B.; Banerjee, D.; Breemen, van L.C.A.; Ciston, J.; Liebscher, C.H.; Martis, V.; Merino, D.H.; Longo, A.; Pattison, P.; Peters, G.W.M.; Portale, G.; Sen, Sabyasachi; Bras, W.

    2014-01-01

    We have studied the formation of nanoparticles in lead sulfide (PbS)-doped borosilicate glass subjected to a two-step nucleation and growth heat treatment using in situ small-angle X-ray scattering (SAXS). The microstructure produced was subsequently characterized using X-ray powder diffraction

  4. Recent applications of hard x-ray photoelectron spectroscopy

    Energy Technology Data Exchange (ETDEWEB)

    Weiland, Conan; Woicik, Joseph C., E-mail: Joseph.Woicik@NIST.gov [National Institute of Standards and Technology, Gaithersburg, Maryland 20899 (United States); Rumaiz, Abdul K. [National Synchrotron Light Source II, Brookhaven National Laboratory, Upton, New York 11973 (United States); Pianetta, Piero [SLAC National Accelerator Laboratory, Menlo Park, California 94025 (United States)

    2016-05-15

    Recent applications of hard x-ray photoelectron spectroscopy (HAXPES) demonstrate its many capabilities in addition to several of its limitations. Examples are given, including measurement of buried interfaces and materials under in situ or in operando conditions, as well as measurements under x-ray standing-wave and resonant excitation. Physical considerations that differentiate HAXPES from photoemission measurements utilizing soft x-ray and ultraviolet photon sources are also presented.

  5. Molybdenum Cluster Chalcogenides: In Situ X-Ray Studies on the Formation of Cu xMo 6S 8 via Electron/Ion Transfer

    Science.gov (United States)

    Fischer, C.; Gocke, E.; Stege, U.; Schöllhorn, R.

    1993-01-01

    Systematic structural investigation have been performed on the formation of the ternary Chevrel phase system CuxMo6S8 by topotactic intercalation of copper into Mo6S8 via electron/ion transfer reactions. In high-temperature synthesis the homogeneity range of CuxMo6S8 formation corresponds to 1.8 ≤ x ≤ 3.66, while by galvanostatic or potentiostatic reduction of binary Mo6S8 at ambiet temperature in aqueous CuSO4 or aprotic CuCl/Ch3CN electrolyte the terminal rhombohedral phase Cu4Mo6S8 with the maximum number of electrons per Mo6 cluster can be obtained. The phase range 1 ≤ x ≤ 4 of CuxMo6S8 as obtained by galvanostatic reduction of Mo6S8 in aqueous CuSO4 electrolyte has been determined by in situ X-ray experiments. Warburg oxygen manometry has proved to be a new and powerful analytical tool for examination of the Cu content of ternary phase CuxMo6S8. Thermodiffractometry and 63 Cu NMR studies of Cu2Mo6S8 (high-temperature phase) reveal a phase-transition rhombohedral/triclinic in a broad temperature range between 285 and 200 K. Superconducting properties (temperature-dependent ac susceptibility) of high temperature and electrochemically prepared Cu phases are reported.

  6. Sulfur X-Ray Absorption Spectroscopy of Living Mammalian Cells: An Enabling Tool for Sulfur Metabolomics. in Situ Observation of Uptake of Taurine Into MDCK Cells

    Energy Technology Data Exchange (ETDEWEB)

    Gnida, M.; Sneeden, E.Yu; Whitin, J.C.; Prince, R.C.; Pickering, I.J.; Korbas, M.; George, G.N.

    2009-06-01

    Sulfur is essential for life, with important roles in biological structure and function. However, because of a lack of suitable biophysical techniques, in situ information about sulfur biochemistry is generally difficult to obtain. Here, we present an in situ sulfur X-ray absorption spectroscopy (S-XAS) study of living cell cultures of the mammalian renal epithelial MDCK cell line. A great deal of information is retrieved from a characteristic sulfonate feature in the X-ray absorption spectrum of the cell cultures, which can be related to the amino acid taurine. We followed the time and dose dependence of uptake of taurine into MDCK cell monolayers. The corresponding uptake curves showed a typical saturation behavior with considerable levels of taurine accumulation inside the cells (as much as 40% of total cellular sulfur). We also investigated the polarity of uptake of taurine into MDCK cells, and our results confirmed that uptake in situ is predominantly a function of the basolateral cell surface.

  7. Tuning of colossal dielectric constant in gold-polypyrrole composite nanotubes using in-situ x-ray diffraction techniques

    Energy Technology Data Exchange (ETDEWEB)

    Sarma, Abhisakh; Sanyal, Milan K., E-mail: milank.sanyal@saha.ac.in [Saha Institute of Nuclear Physics, 1/AF Bidhannagar, Kolkata 700 064 (India)

    2014-09-15

    In-situ x-ray diffraction technique has been used to study the growth process of gold incorporated polypyrrole nanotubes that exhibit colossal dielectric constant due to existence of quasi-one-dimensional charge density wave state. These composite nanotubes were formed within nanopores of a polycarbonate membrane by flowing pyrrole monomer from one side and mixture of ferric chloride and chloroauric acid from other side in a sample cell that allows collection of x-ray data during the reaction. The size of the gold nanoparticle embedded in the walls of the nanotubes was found to be dependent on chloroauric acid concentration for nanowires having diameter more than 100 nm. For lower diameter nanotubes the nanoparticle size become independent of chloroauric acid concentration and depends on the diameter of nanotubes only. The result of this study also shows that for 50 nm gold-polypyrrole composite nanotubes obtained with 5.3 mM chloroauric acid gives colossal dielectric constant of about 10{sup 7}. This value remain almost constant over a frequency range from 1Hz to 10{sup 6} Hz even at 80 K temperature.

  8. Tuning of colossal dielectric constant in gold-polypyrrole composite nanotubes using in-situ x-ray diffraction techniques

    Directory of Open Access Journals (Sweden)

    Abhisakh Sarma

    2014-09-01

    Full Text Available In-situ x-ray diffraction technique has been used to study the growth process of gold incorporated polypyrrole nanotubes that exhibit colossal dielectric constant due to existence of quasi-one-dimensional charge density wave state. These composite nanotubes were formed within nanopores of a polycarbonate membrane by flowing pyrrole monomer from one side and mixture of ferric chloride and chloroauric acid from other side in a sample cell that allows collection of x-ray data during the reaction. The size of the gold nanoparticle embedded in the walls of the nanotubes was found to be dependent on chloroauric acid concentration for nanowires having diameter more than 100 nm. For lower diameter nanotubes the nanoparticle size become independent of chloroauric acid concentration and depends on the diameter of nanotubes only. The result of this study also shows that for 50 nm gold-polypyrrole composite nanotubes obtained with 5.3 mM chloroauric acid gives colossal dielectric constant of about 107. This value remain almost constant over a frequency range from 1Hz to 106 Hz even at 80 K temperature.

  9. Hydrogen absorption in epitaxial W/Nb(001) and polycrystalline Fe/Nb(110) multilayers studied in-situ by X-ray/neutron scattering techniques and X-ray absorption spectroscopy

    International Nuclear Information System (INIS)

    Klose, F.; Rehm, C.; Fieber-Erdmann, M.; Holub-Krappe, E.; Bleif, H. J.; Sowers, H.; Goyette, R.; Troger, L.; Maletta, H.

    1999-01-01

    Hydrogen can be absorbed in large quantities by 100 A thin Nb layers embedded in epitaxial W/Nb and polycrystalline Fe/Nb multilayers. The solubility and the hydrogen-induced structural changes of the host lattice are explored in-situ by small-angle neutron/X-ray reflectometry and high-angle diffraction. These measurements reveal for both systems that the relative out-of-plane expansion of the Nb layers is considerably larger than the relative increase of the Nb interplanar spacing indicating two distinctly different mechanisms of hydrogen absorption. In Fe/Nb multilayers, hydrogen expands the Nb interplanar spacing in a continuous way as function of the external pressure. In contrast, the Nb lattice expansion is discontinuous in epitaxial W/Nb multilayers: A jump in the Nb(002) Bragg reflection position occurs at a critical hydrogen pressure of 1 mbar. In-situ EXAFS spectroscopy also exhibits an irreversible expansion of the Nb lattice in the film plane for p H2 > 1 mbar. This can be regarded as a structural phase transition from an exclusively out-of-plane to a three-dimensionally expanded state at low and high hydrogen pressures, respectively

  10. Mechanistic studies of chemical looping desulfurization of Mn-based oxides using in situ X-ray absorption spectroscopy

    International Nuclear Information System (INIS)

    König, C.F.J.; Nachtegaal, M.; Seemann, M.; Clemens, F.; Garderen, N. van; Biollaz, S.M.A.; Schildhauer, T.J.

    2014-01-01

    Highlights: • Mn sorbents remove H 2 S from hot syngas in chemical looping desulfurization process. • State of Mn followed by in situ X-ray absorption spectroscopy and mass spectrometry. • Two-step mechanism explains the formation of SO 2 under reducing conditions. - Abstract: Cleaning of producer gas from biomass gasification is required for further processing, e.g. to avoid catalyst poisoning in subsequent conversion steps. High-temperature gas cleaning, of which sulfur removal is an important part, is a promising way to improve the overall efficiency of biomass conversion. In a high temperature “chemical looping desulfurization” process, a sorbent material, here manganese oxide, is cycled between producer gas from the gasifier to remove sulfur species, and an oxidizing atmosphere, in which the sulfur species are released as SO 2 . Alternatively, the use of such material as reactive bed material could be integrated into an allothermal dual fluidized bed gasifier. In a laboratory reactor, we subjected manganese-based materials to a periodically changing gas atmosphere, simulating a “chemical looping desulfurization” reactor. The “fuel reactor” gas contained H 2 , CO, CH 4 and H 2 S, similar as in the producer gas, and the “oxidizing reactor” contained diluted O 2 . Mass spectrometry showed that most of the H 2 S is taken up by the sample in the “fuel reactor” part, while also some unwanted SO 2 is generated in the “fuel reactor” part. Most of the sulfur is released in the oxidizing reactor. Simultaneous in situ X-ray absorption spectroscopy (XAS) of the Mn materials during different stages of the chemical looping desulfurization process showed that the initial Mn 3 O 4 is transformed in the presence of H 2 S to MnS via a MnO intermediate in the fuel reactor. Oxygen from the reduction of Mn 3 O 4 oxidizes some H 2 S to the undesired SO 2 in the fuel reactor. Upon exposure to O 2 , MnS is again oxidized to Mn 3 O 4 via MnO, releasing SO

  11. Laboratory and In-Flight In-Situ X-ray Imaging and Scattering Facility for Materials, Biotechnology and Life Sciences

    Science.gov (United States)

    2003-01-01

    We propose a multifunctional X-ray facility for the Materials, Biotechnology and Life Sciences Programs to visualize formation and behavior dynamics of materials, biomaterials, and living organisms, tissues and cells. The facility will combine X-ray topography, phase micro-imaging and scattering capabilities with sample units installed on the goniometer. This should allow, for the first time, to monitor under well defined conditions, in situ, in real time: creation of imperfections during growth of semiconductors, metal, dielectric and biomacromolecular crystals and films, high-precision diffraction from crystals within a wide range of temperatures and vapor, melt, solution conditions, internal morphology and changes in living organisms, tissues and cells, diffraction on biominerals, nanotubes and particles, radiation damage, also under controlled formation/life conditions. The system will include an ultrabright X-ray source, X-ray mirror, monochromator, image-recording unit, detectors, and multipurpose diffractometer that fully accommodate and integrate furnaces and samples with other experimental environments. The easily adjustable laboratory and flight versions will allow monitoring processes under terrestrial and microgravity conditions. The flight version can be made available using a microsource combined with multilayer or capillary optics.

  12. In situ x-ray imaging of nanoparticle agglomeration in fluidized beds

    International Nuclear Information System (INIS)

    Jenneson, Paul Michael; Gundogdu, Ozcan

    2006-01-01

    A high spatial (down to 400 nm) and temporal resolution (down to 1 ms) x-ray imaging apparatus has been designed to study the agglomeration of arc plasma synthesized zinc oxide nanoparticles (average diameter of 50 nm) in fluidized beds under different gas flow velocities. The mean volume distribution of the nanoparticle agglomerates was determined with x-ray microtomography and found to correspond to a lognormal distribution with a mean value of 0.70x10 9 μm 3 and a variance of 3.6x10 21 (μm 3 ) 2 . The average density of the agglomerates was found to be 2.9 g cm -3 compared to 5.6 g cm -3 for the individual nanoparticles. The powder assembly was then dynamically imaged using an x-ray image intensifier coupled to a digital camera using a field of view of 24.20 mm by 32.25 mm and a temporal resolution of 40 ms. Sequential frames were captured into computer memory for a range of gas flow velocities from 0.026 ms -1 to 0.313 ms -1 . The breakup energy of the agglomerates was calculated to be approximately 2x10 -8 J using a combination of dynamic observations and physical properties of the agglomerate system extracted from the x-ray microtomographic data

  13. In Situ Solid-State Reactions Monitored by X-ray Absorption Spectroscopy: Temperature-Induced Proton Transfer Leads to Chemical Shifts.

    Science.gov (United States)

    Stevens, Joanna S; Walczak, Monika; Jaye, Cherno; Fischer, Daniel A

    2016-10-24

    The dramatic colour and phase alteration with the solid-state, temperature-dependent reaction between squaric acid and 4,4'-bipyridine has been probed in situ with X-ray absorption spectroscopy. The electronic and chemical sensitivity to the local atomic environment through chemical shifts in the near-edge X-ray absorption fine structure (NEXAFS) revealed proton transfer from the acid to the bipyridine base through the change in nitrogen protonation state in the high-temperature form. Direct detection of proton transfer coupled with structural analysis elucidates the nature of the solid-state process, with intermolecular proton transfer occurring along an acid-base chain followed by a domino effect to the subsequent acid-base chains, leading to the rapid migration along the length of the crystal. NEXAFS thereby conveys the ability to monitor the nature of solid-state chemical reactions in situ, without the need for a priori information or long-range order. © 2016 Wiley-VCH Verlag GmbH & Co. KGaA, Weinheim.

  14. High pressure in situ X-ray diffraction study of MnO to 137 GPa and comparison with shock compression experiment

    Science.gov (United States)

    Yagi, T.; Kondo, T.; Syono, Y.

    1998-07-01

    In order to clarify the nature of the phase transformation in MnO observed at around 90 GPa by shock compression experiment, high pressure in situ X-ray observations were carried out up to 137 GPa. Powdered sample was directly compressed in Mao-Bell type diamond anvil cell and X-ray experiments were carried out using angle dispersive technique by combining synchrotron radiation and imaging plate detector. Distortion of the B1 structured phase was observed above about 40 GPa, which continues to increase up to 90 GPa. Two discontinuous changes of the diffraction profiles were observed at around 90 GPa and 120 GPa. The nature of the intermediate phase between 90 GPa and 120 GPa is not clear yet. It is neither cesium chloride (B2) nor nickel arsenide (B8) structure. On the other hand, the diffraction profile above 120 GPa can be reasonably well explained by the B8 structure. High pressure phases above 90 GPa have metallic luster and all the transformations are reversible on release of pressure.

  15. X-ray chemical analyzer for field applications

    International Nuclear Information System (INIS)

    Gamba, O.O.M.

    1977-01-01

    A self-supporting portable field multichannel x-ray chemical analyzer system is claimed. It comprises a lightweight, flexibly connected, remotely locatable, radioisotope-excited sensing probe utilizing a cryogenically-cooled solid state semi-conductor crystal detector for fast in situ non-destructive, qualitative and quantitative analysis of elements in solid, powder, liquid or slurried form, utilizing an x-ray energy dispersive spectrometry technique

  16. Study on TV X-ray system characteristics

    International Nuclear Information System (INIS)

    Semenov, A.P.; Volkov, A.V.

    1978-01-01

    The results are presented of comparative investigations into the main characteristics of TV X-ray systems (TXS) and X-ray radiography when X-raying of the 1Kh18N9T steel. The following characteristics are considered: the threshold contrast sensitivity, the sensitivity to revealing standard defects, and the dose rate of X-radiation at the input of the X-ray converter. Practical recommendations are given on the use of TXS in flaw detection of various materials. It is remarked to use introscopes for testing of thick welded products articles, and X-ray vidicon systems for study of low-contrast images (in testing of welds made by point welding, and of thin-wall products)

  17. X-ray in-situ study of copper electrodeposition on UHV prepared GaAs(001) surfaces

    Energy Technology Data Exchange (ETDEWEB)

    Gruender, Yvonne

    2008-06-02

    For this work a unique setup for in-situ electrochemical studies was employed and improved. This setup permits UHV preparation of the GaAs(001) surface with a defined surface termination (arsenic-rich or gallium-rich) and its characterization by SXRD in UHV, under ambient pressure in inert gas and in electrolyte under potential control without passing through air. The GaAs(001) surfaces were capped by amorphous arsenic. This permitted to ship them through ambient air. Afterwards smooth well defined GaAs(001) surfaces could be recovered by thermal annealing in UHV. A first investigation of the arsenic capped sample was done by atomic force microscopy (AFM) and Surface X-Ray Diffraction (SXRD). The non bulk like termination of the arsenic buried GaAs(001) surface was revealed. For the electrochemical metal deposition, arsenic terminated (2 x 4) reconstructed and gallium terminated (4 x 2) reconstructed GaAs(001) surfaces were employed. These surfaces were characterized by STM, LEED and a first time by SXRD. The surfaces are smooth, however, a higher degree of disorder than for MBE prepared reconstructed GaAs(001) is found. After exposure of the sample to nitrogen, the surfaces were then again studied by SXRD. These two steps characterizing the bare GaAs(001) surfaces permitted us to get a better knowledge of the starting surface and its influence on the later electrodeposited copper. At ambient pressure both reconstructions are lifted, but the surface is not bulk-like terminated as can be deduced from the crystal truncation rods. Epitaxial copper clusters grow upon electrodeposition on the UHV prepared GaAs(001) surface. The copper lattice is rotated and inclined with respect to the GaAs substrate lattice, leading to eight symmetry equivalent domains. The influence of the surface termination as well as the nucleation potential on the structure of the electrodeposited copper were investigated. The tilt and rotation angles do not depend on the deposition potential but

  18. High-speed image converter x-ray studies

    International Nuclear Information System (INIS)

    Bryukhnevitch, G.I.; Kas'yanov, Yu.S.; Korobkin, V.V.; Prokhorov, A.M.; Stepanov, B.M.; Chevokin, V.K.; Schelev, M.Ya.

    1975-01-01

    Two X-ray high-speed image-converter cameras (ICC) have been developed. In the first one a soft X-ray radiation is converted into visible light with the aid of a 0.5ns response time, plastic scintillator. The second camera incorporates a photocathode which is sensitive to visible and X-ray radiation. Its calculated temporal resolution approaches 5 to 7ps. Both developed cameras were employed for studies of X-ray radiation emitted by laser plasma. For the smooth nanosecond excited laser pulses, a noticeable amplitude modulation was recorded in all laser pulses reflected by plasma as well as in each third pulse of X-ray plasma radiation. It was also observed that the duration of X-ray plasma radiation is 20 to 40% shorter than that of the incident nanosecond laser pulses and this duration being 3 to 6 times longer than that of the picosecond irradiating pulses. The half-width of the recorded X-ray plasma pulses was 30 to 60ps. (author)

  19. X-ray reflectivity and surface roughness

    International Nuclear Information System (INIS)

    Ocko, B.M.

    1988-01-01

    Since the advent of high brightness synchrotron radiation sources there has been a phenomenal growth in the use of x-rays as a probe of surface structure. The technique of x-ray reflectivity is particularly relevant to electrochemists since it is capable of probing the structure normal to an electrode surface in situ. In this paper the theoretical framework for x-ray reflectivity is reviewed and the results from previous non-electrochemistry measurements are summarized. These measurements are from the liquid/air interface (CCl 4 ), the metal crystal vacuum interface (Au(100)), and from the liquid/solid interface(liquid crystal/silicon). 34 refs., 5 figs

  20. In-situ X-ray Nanocharacterization of Defect Kinetics in Chalcogenide Solar Cell Materials

    Energy Technology Data Exchange (ETDEWEB)

    Bertoni, Mariana [Arizona State Univ., Tempe, AZ (United States); Lai, Barry [Argonne National Lab. (ANL), Argonne, IL (United States). Advanced Photon Source (APS); Masser, Jorg [Argonne National Lab. (ANL), Argonne, IL (United States). Advanced Photon Source (APS); Buonassisi, Tonio [Massachusetts Inst. of Technology (MIT), Cambridge, MA (United States)

    2016-09-21

    ) correlate positively, and In negatively with charge collection efficiency for cells with low Ga content, both at grain boundaries and in grain cores. For cells with high Ga content, the charge collection efficiency depends to much lesser extent on the elemental distribution. The objective is three folded: (1) develop an x-ray in-situ microscopy capability to simulate growth and processing conditions, (2) apply it to elucidate performance-governing defect kinetics in chalcogenide solar cell materials, and (3) to study approaches to engineer materials from the nanoscale up. The development of these capabilities will enable experimental characterization to take place under actual processing and operating conditions and it will have impact well beyond the proposed research, enabling future studies on a large variety of materials system where electronic properties depend on underlying structural or chemical inhomogeneities.

  1. Sample cell for studying liquid interfaces with an in situ electric field using X-ray reflectivity and application to clay particles at oil-oil interfaces.

    Science.gov (United States)

    Larsen, Simon R; Hansteen, Marie; Pacakova, Barbara; Theodor, Keld; Arnold, Thomas; Rennie, Adrian R; Helgesen, Geir; Knudsen, Kenneth D; Bordallo, Heloisa N; Fossum, Jon Otto; Cavalcanti, Leide P

    2018-05-01

    Commissioning results of a liquid sample cell for X-ray reflectivity studies with an in situ applied electrical field are presented. The cell consists of a Plexiglas container with lateral Kapton windows for air-liquid and liquid-liquid interface studies, and was constructed with grooves to accept plate electrodes on the walls parallel to the direction of the beam. Both copper and ITO plate electrodes have been used, the latter being useful for simultaneous optical studies. Commissioning tests were made at the I07 beamline of the Diamond Light Source. open access.

  2. Optical and X-ray studies of Compact X-ray Binaries in NGC 5904

    Science.gov (United States)

    Bhalotia, Vanshree; Beck-Winchatz, Bernhard

    2018-06-01

    Due to their high stellar densities, globular cluster systems trigger various dynamical interactions, such as the formation of compact X-ray binaries. Stellar collisional frequencies have been correlated to the number of X-ray sources detected in various clusters and we hope to measure this correlation for NGC 5904. Optical fluxes of sources from archival HST images of NGC 5904 have been measured using a DOLPHOT PSF photometry in the UV, optical and near-infrared. We developed a data analysis pipeline to process the fluxes of tens of thousands of objects using awk, python and DOLPHOT. We plot color magnitude diagrams in different photometric bands in order to identify outliers that could be X-ray binaries, since they do not evolve the same way as singular stars. Aligning previously measured astrometric data for X-ray sources in NGC 5904 from Chandra with archival astrometric data from HST will filter out the outlier objects that are not X-ray producing, and provide a sample of compact binary systems that are responsible for X-ray emission in NGC 5904. Furthermore, previously measured X-ray fluxes of NGC 5904 from Chandra have also been used to measure the X-ray to optical flux ratio and identify the types of compact X-ray binaries responsible for the X-ray emissions in NGC 5904. We gratefully acknowledge the support from the Illinois Space Grant Consortium.

  3. Ex-situ X-ray computed tomography data for a non-crimp fabric based glass fibre composite under fatigue loading

    DEFF Research Database (Denmark)

    Jespersen, Kristine Munk; Mikkelsen, Lars Pilgaard

    2017-01-01

    The data published with this article are high resolution X-ray computed tomography (CT) data obtained during an ex-situ fatigue test of a coupon test specimen made from a non-crimp fabric based glass fibre composite similar to those used for wind turbine blades. The fatigue test was interrupted...

  4. Static tensile deformation behavior of a lean duplex stainless steel studied by in situ neutron diffraction and synchrotron radiation white x-rays

    International Nuclear Information System (INIS)

    Tsuchida, Noriyuki; Kawahata, Taiji; Ishimaru, Eiichiro; Takahashi, Akihiko; Suzuki, Hiroshi; Shobu, Takahisa

    2013-01-01

    To investigate the tensile deformation behavior of a lean duplex stainless steel (S32101) from the viewpoints of plastic deformability among phases or grains, we performed static tensile tests, in situ neutron diffraction, and white x-ray diffraction experiments at room temperature. In the static tensile tests, the S32101 steel displayed a larger uniform elongation and a better tensile strength-uniform elongation balance than a commercial SUS329J4L duplex stainless steel. A larger uniform elongation of S32101 is associated with the macroscopic work hardening behavior that a work hardening rate higher than the flow stress can maintain up until high true strains. From the experimental results of synchrotron radiation white x-ray diffraction experiments, the hard phase of S32101 was changed from the ferrite (α) phase to austenite (γ) one during tensile deformation. This led to a larger stress partitioning between the phases at the latter stage of deformation. From the experimental results of in situ neutron diffraction, it was found that the stress partitioning of the γ phase in the S32101 was the largest among the present results. Therefore, the larger work hardening rate of S32101 can be explained by the large stress partitioning of the γ phase, that between γ and α phases and γ volume fraction. (author)

  5. Nanocalorimeter platform for in situ specific heat measurements and x-ray diffraction at low temperature

    Energy Technology Data Exchange (ETDEWEB)

    Willa, K. [Materials Science Division, Argonne National Laboratory, 9700 South Cass Avenue, Argonne, Illinois 60439, USA; Diao, Z. [Department of Physics, Stockholm University, SE-106 91 Stockholm, Sweden; Laboratory of Mathematics, Physics and Electrical Engineering, Halmstad University, P.O. Box 823, SE-301 18 Halmstad, Sweden; Campanini, D. [Department of Physics, Stockholm University, SE-106 91 Stockholm, Sweden; Welp, U. [Materials Science Division, Argonne National Laboratory, 9700 South Cass Avenue, Argonne, Illinois 60439, USA; Divan, R. [Center for Nanoscale Materials, Argonne National Laboratory, 9700 South Cass Avenue, Argonne, Illinois 60439, USA; Hudl, M. [Department of Physics, Stockholm University, SE-106 91 Stockholm, Sweden; Islam, Z. [X-ray Science Division, Argonne National Laboratory, 9700 South Cass Avenue, Argonne, Illinois 60439, USA; Kwok, W. -K. [Materials Science Division, Argonne National Laboratory, 9700 South Cass Avenue, Argonne, Illinois 60439, USA; Rydh, A. [Department of Physics, Stockholm University, SE-106 91 Stockholm, Sweden

    2017-12-01

    Recent advances in electronics and nanofabrication have enabled membrane-based nanocalorimetry for measurements of the specific heat of microgram-sized samples. We have integrated a nanocalorimeter platform into a 4.5 T split-pair vertical-field magnet to allow for the simultaneous measurement of the specific heat and x-ray scattering in magnetic fields and at temperatures as low as 4 K. This multi-modal approach empowers researchers to directly correlate scattering experiments with insights from thermodynamic properties including structural, electronic, orbital, and magnetic phase transitions. The use of a nanocalorimeter sample platform enables numerous technical advantages: precise measurement and control of the sample temperature, quantification of beam heating effects, fast and precise positioning of the sample in the x-ray beam, and fast acquisition of x-ray scans over a wide temperature range without the need for time-consuming re-centering and re-alignment. Furthermore, on an YBa2Cu3O7-delta crystal and a copper foil, we demonstrate a novel approach to x-ray absorption spectroscopy by monitoring the change in sample temperature as a function of incident photon energy. Finally, we illustrate the new insights that can be gained from in situ structural and thermodynamic measurements by investigating the superheated state occurring at the first-order magneto-elastic phase transition of Fe2P, a material that is of interest for magnetocaloric applications.

  6. In Situ X-ray Diffraction Study of Cesium Exchange in Synthetic Umbite

    International Nuclear Information System (INIS)

    Fewox, C.; Clearfield, A.; Celestian, A.

    2011-01-01

    The exchange of Cs + into H 1.22 K 0.84 ZrSi 3 O 9 · 2.16H 2 O (umbite-(HK)) was followed in situ using time-resolved X-ray diffraction at the National Synchrotron Light Source. The umbite framework (space group P2 1 /c with cell dimensions of a = 7.2814(3) (angstrom), b = 10.4201(4) (angstrom), c = 13.4529(7) (angstrom), and β = 90.53(1) o ) consists of wollastonite-like silicate chains linked by isolated zirconia octahedra. Within umbite-(HK) there are two unique ion exchange sites in the tunnels running parallel to the a-axis. Exchange Site 1 is marked by 8 member-ring (MR) windows in the bc-plane and contains K + cations. Exchange Site 2 is marked by a larger 8-MR channel parallel to [100], and contains H 2 O molecules. The occupancy of the Cs + cations through these channels was modeled by Rietveld structure refinements of the diffraction data and demonstrated that there is a two-step exchange process. The incoming Cs + ions populated the larger 8-MR channel (Exchange Site 2) first and then migrated into the smaller 8-MR channel. During the exchange process a structural change occurs, transforming the exchanger from monoclinic P2 1 /c to orthorhombic P2 1 2 1 2 1 . This structural change occurs when Cs + occupancy in the small cavity becomes greater than 0.50. The final in situ ion exchange diffraction pattern was refined to yield umbite-(CsK) with the molecular formula H 0.18 K 0.45 Cs 1.37 ZrSi 3 O 9 · 0.98H 2 O and possessing an orthorhombic unit cell with dimensions a = 10.6668(8) (angstrom), b = 13.5821(11) (angstrom), c = 7.3946(6) (angstrom). Solid state 133 Cs MAS NMR showed there is only a slight difference between the two cavities electronically. Valence bond sums for the completely occupied Exchange Site 1 demonstrate that Cs-O bonds of up to 3.8 (angstrom) contribute to the coordination of the Cs + cation.

  7. Soft x rays for radiobiological studies

    International Nuclear Information System (INIS)

    Ban, Sadayuki; Iida, Shozo; Shimba, Hachiro; Awa, A.A.; Hamilton, H.B.; Clifton, K.H.

    1986-04-01

    Lethal effects and chromosome aberrations induced in cells exposed to low energy (soft) X rays demonstrated that these relatively low energy X rays are just as effective as those of higher energy for radiobiological studies, and even more effective for irradiating cultured mammalian cells than laboratory animals. (author)

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

    DEFF Research Database (Denmark)

    Skou, Magda; Skou, Soren; Jensen, Thomas Glasdam

    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 sim...... in incidental sample purification. Hence, this versatile microfluidic device enables investigation of experimentally induced structural changes under dynamically controllable sample conditions. (C) 2014 International Union of Crystallography......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...

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

    Energy Technology Data Exchange (ETDEWEB)

    Maddox, B. R., E-mail: maddox3@llnl.gov; Akin, M. C., E-mail: akin1@llnl.gov; Teruya, A.; Hunt, D.; Hahn, D.; Cradick, J. [Lawrence Livermore National Laboratory, Livermore, California 94550 (United States); Morgan, D. V. [National Security Technologies LLC, Los Alamos, New Mexico 87544 (United States)

    2016-08-15

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

  10. Thermal expansion behavior of empressite, AgTe: A structural study by means of in situ high-temperature single-crystal X-ray diffraction

    International Nuclear Information System (INIS)

    Bindi, Luca

    2009-01-01

    The crystal structure of empressite, AgTe, a rare silver telluride, has been investigated by in situ X-ray single-crystal diffraction methods within the temperature range 298-463 K. AgTe remains orthorhombic, space group Pmnb (Pnma as standard), and shows only normal thermal expansion over the entire temperature range. The unit-cell parameters show a gradual increase with the increase of temperature. Slight adjustments in the geometry of Ag-tetrahedra and in the crystal-chemical environment of tellurium atoms occur in a continuous way without abrupt structural changes. The coefficients of thermal expansion along various axes are: α a = 1.5 x 10 -5 K -1 , α b = 3.0 x 10 -5 K -1 , α c = 2.2 x 10 -5 K -1 , and the bulk thermal expansion coefficient α V is 5.4 x 10 -5 K -1 for the temperature range 298-463 K

  11. Measurement of ZnO/Al2O3 Heterojunction Band Offsets by in situ X-Ray Photoelectron Spectroscopy

    International Nuclear Information System (INIS)

    Lei Hong-Wen; Zhang Hong; Wang Xue-Min; Zhao Yan; Yan Da-Wei; Jiang Zhong-Qian; Yao Gang; Zeng Ti-Xian; Wu Wei-Dong

    2013-01-01

    ZnO films are grown on c-sapphire substrates by laser molecular beam epitaxy. The band offsets of the ZnO/Al 2 O 3 heterojunction are studied by in situ x-ray photoelectron spectroscopy. The valence band of Al 2 O 3 is found to be 3.59±0.05eV below that of ZnO. Together with the resulting conduction band offset of 2.04±0.05eV, this indicates that a type-I staggered band line exists at the ZnO/Al 2 O 3 heterojunction

  12. In situ X-ray analysis of MoO3 reduction

    International Nuclear Information System (INIS)

    Leisegang, T.; Levin, A.A.; Meyer, D.C.; Walter, J.

    2005-01-01

    The reduction of MoO 3 to MoO 2 under hydrogen/argon atmosphere (5 vol. % H 2 /95 vol. % Ar) in the temperature range 323 K..623 K was studied in situ by means of wide-angle X-ray scattering. It has been found that the starting material, MoO 3 , consists of two different orthorhombic MoO 3 phases A and B with nearly the same structure parameters. The phase A (fraction of 37.1 wt%) describes the larger crystallites whereas the phase B (fraction of 62.9 wt.%) describes the smaller crystallites. Under the reduction to monoclinic MoO 2 phase during the heating, the thermal evolution of the phase fractions is different. A conclusion is drawn that MoO 2 is formed preferably in big crystallites. About 10 wt. % of MoO 2 has been found to form at 623 K resulting in about 69 wt. % after cooling to room temperature followed by holding in Ar/H 2 atmosphere about 24 h. Additionally, about 4.4 wt. % of the Mo 4 O 11 oxide probably formed in large crystallites was detected in the reduced powder after the cooling. (copyright 2005 WILEY-VCH Verlag GmbH and Co. KGaA, Weinheim) (orig.)

  13. Radiation chemistry of polymeric X-ray resists; Zur Strahlenchemie polymerer Roentgenresists

    Energy Technology Data Exchange (ETDEWEB)

    Wollersheim, O.

    1995-03-01

    In this study, the radiation chemical reactions in poly(methyl-methacrylate) (PMMA) and homo- and copolymers of lactide and glycollide during X-ray exposure with synchrotron radiation from the Bonn ELSA electron storage ring are quantitatively analyzed. In situ studies of the irradiated PMMA and lactide/glycollide polymers with mass spectroscopy, infrared spectroscopy and ESR spectroscopy combined with ex situ methods as size exclusion chromatography and titration lead to a complete and quantitative understanding of the radiation chemical reactions in both polymer classes. The implications for the application of the polymers in the X-ray deep etch lithography, which is the appropriate process for the production of microsystem components, are discussed. (orig.)

  14. In-situ observation of deuteride formation in palladium electrochemical cathode by X-ray diffraction method

    International Nuclear Information System (INIS)

    Yamamoto, Takao; Oka, Takashi; Taniguchi, Ryoichi

    1990-01-01

    In-situ X-ray diffraction observation of palladium foil cathode (10 μm) was carried out during electrolysis of 0.1N-LiOD heavy water solution in order to estimate the deuterium content in palladium during the detection of charged particles in our previous work. A complete transformation into β-palladium deuteride phase was observed, and its maximum lattice constant 4.06 A was evaluated as corresponding to D/Pd = 0.73. The deuterium concentration in the previous work was estimated as higher than this considering the difference in cell conditions. (author)

  15. A neutron-X-ray, NMR and calorimetric study of glassy Probucol synthesized using containerless techniques

    International Nuclear Information System (INIS)

    Weber, J.K.R.; Benmore, C.J.; Tailor, A.N.; Tumber, S.K.; Neuefeind, J.; Cherry, B.; Yarger, J.L.; Mou, Q.; Weber, W.; Byrn, S.R.

    2013-01-01

    Highlights: • Acoustic levitation was used to make phase-pure glassy forms of pharmaceutical compounds. • Neutrons, X-rays and NMR were used to characterize the glasses. • The glass comprised of slightly distorted molecules packed in a random network. • Potential for new drug synthesis routes is discussed. - Abstract: Acoustic levitation was used to trap 1–3 mm diameter drops of Probucol and other pharmaceutical materials in containerless conditions. Samples were studied in situ using X-ray diffraction and ex situ using neutron diffraction, NMR and DSC techniques. The materials were brought into non-equilibrium states by supersaturating solutions or by supercooling melts. The glass transition and crystallization temperatures of glassy Probucol were 29 ± 1 and 71 ± 1 °C respectively. The glassy form was stable with a shelf life of at least 8 months. A neutron/X-ray difference function of the glass showed that while molecular sub-groups remain rigid, many of the hydrogen correlations observed in the crystal become smeared out in the disordered material. The glass is principally comprised of slightly distorted Form I Probucol molecules with disordered packing rather than large changes in the individual molecular structure. Avoiding surface contact-induced nucleation provided access to highly non-equilibrium phases and enabled synthesis of phase-pure glasses

  16. A neutron-X-ray, NMR and calorimetric study of glassy Probucol synthesized using containerless techniques

    Energy Technology Data Exchange (ETDEWEB)

    Weber, J.K.R., E-mail: rweber@anl.gov [Materials Development, Inc., Arlington Heights, IL 60004 (United States); Argonne National Laboratory, Argonne, IL 60439 (United States); Benmore, C.J. [Argonne National Laboratory, Argonne, IL 60439 (United States); Department of Physics, Arizona State University, AZ 85287 (United States); Tailor, A.N.; Tumber, S.K. [Materials Development, Inc., Arlington Heights, IL 60004 (United States); Neuefeind, J. [Oak Ridge National Laboratory, Oak Ridge, TN 37831 (United States); Cherry, B. [Magnetic Resonance Research Center, Arizona State University, AZ 85287 (United States); Department of Chemistry and Biochemistry, Arizona State University, AZ 85287 (United States); Yarger, J.L. [Department of Physics, Arizona State University, AZ 85287 (United States); Magnetic Resonance Research Center, Arizona State University, AZ 85287 (United States); Department of Chemistry and Biochemistry, Arizona State University, AZ 85287 (United States); Mou, Q. [Magnetic Resonance Research Center, Arizona State University, AZ 85287 (United States); Department of Chemistry and Biochemistry, Arizona State University, AZ 85287 (United States); Weber, W. [Department of Physics, Arizona State University, AZ 85287 (United States); Department of Chemistry and Biochemistry, Arizona State University, AZ 85287 (United States); Byrn, S.R. [Department of Industrial and Physical Pharmacy, Purdue University, IN 47907 (United States)

    2013-10-16

    Highlights: • Acoustic levitation was used to make phase-pure glassy forms of pharmaceutical compounds. • Neutrons, X-rays and NMR were used to characterize the glasses. • The glass comprised of slightly distorted molecules packed in a random network. • Potential for new drug synthesis routes is discussed. - Abstract: Acoustic levitation was used to trap 1–3 mm diameter drops of Probucol and other pharmaceutical materials in containerless conditions. Samples were studied in situ using X-ray diffraction and ex situ using neutron diffraction, NMR and DSC techniques. The materials were brought into non-equilibrium states by supersaturating solutions or by supercooling melts. The glass transition and crystallization temperatures of glassy Probucol were 29 ± 1 and 71 ± 1 °C respectively. The glassy form was stable with a shelf life of at least 8 months. A neutron/X-ray difference function of the glass showed that while molecular sub-groups remain rigid, many of the hydrogen correlations observed in the crystal become smeared out in the disordered material. The glass is principally comprised of slightly distorted Form I Probucol molecules with disordered packing rather than large changes in the individual molecular structure. Avoiding surface contact-induced nucleation provided access to highly non-equilibrium phases and enabled synthesis of phase-pure glasses.

  17. Development of a combined portable x-ray fluorescence and Raman spectrometer for in situ analysis.

    Science.gov (United States)

    Guerra, M; Longelin, S; Pessanha, S; Manso, M; Carvalho, M L

    2014-06-01

    In this work, we have built a portable X-ray fluorescence (XRF) spectrometer in a planar configuration coupled to a Raman head and a digital optical microscope, for in situ analysis. Several geometries for the XRF apparatus and digital microscope are possible in order to overcome spatial constraints and provide better measurement conditions. With this combined spectrometer, we are now able to perform XRF and Raman measurements in the same point without the need for sample collection, which can be crucial when dealing with cultural heritage objects, as well as forensic analysis. We show the capabilities of the spectrometer by measuring several standard reference materials, as well as other samples usually encountered in cultural heritage, geological, as well as biomedical studies.

  18. In situ X-ray polymerization: from swollen lamellae to polymer-surfactant complexes.

    Science.gov (United States)

    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.

  19. X-ray initiated polymerization of wood impregnants

    Energy Technology Data Exchange (ETDEWEB)

    Cleland, Marshall R.; Galloway, Richard A. [IBA Industrial, Inc., Edgewood, NY (United States); Berejka, Anthony J. [Ionicorp, Huntington, NY 11743 (United States)], E-mail: berejka@msn.com; Montoney, Daniel [Strathmore Products, Syracuse, NY (United States); Driscoll, Mark; Smith, Leonard; Scott Larsen, L. [State University of New York, SUNY-ESF, Syracuse, NY (United States)

    2009-07-15

    X-rays, derived from a high energy, high-current electron beam (EB), initiated in-situ polymerization of a unique class of monomers that were found to penetrate the cell walls of wood. X-rays initiated an auto-catalytic acrylic polymerization and penetrated through thick pieces of wood. The final cured product having the polymerizate, a polymer, both in the wood cell lumens and in the cell walls is called wood impregnated with a wood-polymer penetrant (WPP). The controlled lower dose rate of X-rays overcame disproportionation encountered when using higher dose-rate electron beam initiation. With X-rays, the in-situ polymerization took place in one exposure of modest dose. With EB, multiple passes were needed to avoid excessive heat build-up and monomer volatilization. Having entered the cell walls of the wood and then being polymerized within the cell walls, these radiation-cured unique monomers imparted outstanding dimensional stability upon exposure of the impregnated wood to humidity cycling. The preferred monomer system was also chemically modified prior to impregnation with agents that would remain in the wood and prevent the growth of fungi and other microbials. This technique differs from historic uses of monomers that merely filled the lumens of the wood (historic wood-polymer composites), which are only suitable for indoor use. The WPP impregnated wood that was either X-ray cured or EB cured demonstrated enhanced structural properties, dimensional stability, and decay resistance.

  20. X-ray initiated polymerization of wood impregnants

    International Nuclear Information System (INIS)

    Cleland, Marshall R.; Galloway, Richard A.; Berejka, Anthony J.; Montoney, Daniel; Driscoll, Mark; Smith, Leonard; Scott Larsen, L.

    2009-01-01

    X-rays, derived from a high energy, high-current electron beam (EB), initiated in-situ polymerization of a unique class of monomers that were found to penetrate the cell walls of wood. X-rays initiated an auto-catalytic acrylic polymerization and penetrated through thick pieces of wood. The final cured product having the polymerizate, a polymer, both in the wood cell lumens and in the cell walls is called wood impregnated with a wood-polymer penetrant (WPP). The controlled lower dose rate of X-rays overcame disproportionation encountered when using higher dose-rate electron beam initiation. With X-rays, the in-situ polymerization took place in one exposure of modest dose. With EB, multiple passes were needed to avoid excessive heat build-up and monomer volatilization. Having entered the cell walls of the wood and then being polymerized within the cell walls, these radiation-cured unique monomers imparted outstanding dimensional stability upon exposure of the impregnated wood to humidity cycling. The preferred monomer system was also chemically modified prior to impregnation with agents that would remain in the wood and prevent the growth of fungi and other microbials. This technique differs from historic uses of monomers that merely filled the lumens of the wood (historic wood-polymer composites), which are only suitable for indoor use. The WPP impregnated wood that was either X-ray cured or EB cured demonstrated enhanced structural properties, dimensional stability, and decay resistance.

  1. In situ X-ray study of the structural evolution of gold nano-domains by spray deposition on thin conductive P3HT films.

    Science.gov (United States)

    Al-Hussein, M; Schindler, M; Ruderer, M A; Perlich, J; Schwartzkopf, M; Herzog, G; Heidmann, B; Buffet, A; Roth, S V; Müller-Buschbaum, P

    2013-02-26

    Gold (Au) nanoparticles are deposited from aqueous solution onto one of the most used conductive polymers, namely poly(3-hexylthiophene) (P3HT), using airbrush deposition. We report on the structure formation and packing of the Au nanoparticles after a 5 s spray cycle. In situ grazing incidence small-angle X-ray scattering (GISAXS) measurements with 20 ms time resolution allow a real-time observation of the emergence and evolution of the microstructure during a spray cycle and subsequent solvent evaporation. The results reveal multistage nanoscale ordering of the Au nanoparticles during the spray cycle. Further ex situ atomic force microscopy measurements of the sprayed films showed the formation of Au monolayer islands on top of the polymer film. Our study suggests that the solvent-substrate interaction as well as solvent evaporation kinetics are important factors that need to be taken into consideration in order to grow a compact uniform monolayer film for the fabrication of ultrathin films using airbrush deposition.

  2. X-ray reflectivity measurements of liquid/solid interfaces under high hydrostatic pressure conditions.

    Science.gov (United States)

    Wirkert, Florian J; Paulus, Michael; Nase, Julia; Möller, Johannes; Kujawski, Simon; Sternemann, Christian; Tolan, Metin

    2014-01-01

    A high-pressure cell for in situ X-ray reflectivity measurements of liquid/solid interfaces at hydrostatic pressures up to 500 MPa (5 kbar), a pressure regime that is particularly important for the study of protein unfolding, is presented. The original set-up of this hydrostatic high-pressure cell is discussed and its unique properties are demonstrated by the investigation of pressure-induced adsorption of the protein lysozyme onto hydrophobic silicon wafers. The presented results emphasize the enormous potential of X-ray reflectivity studies under high hydrostatic pressure conditions for the in situ investigation of adsorption phenomena in biological systems.

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

    Energy Technology Data Exchange (ETDEWEB)

    Cinbiz, Mahmut N., E-mail: cinbizmn@ornl.gov [Department of Mechanical and Nuclear Engineering, Pennsylvania State University, University Park, PA, 16802 (United States); Koss, Donald A., E-mail: koss@ems.psu.edu [Department of Materials Science and Engineering, Pennsylvania State University, University Park, PA, 16802 (United States); Motta, Arthur T., E-mail: atm2@psu.edu [Department of Mechanical and Nuclear Engineering, Pennsylvania State University, University Park, PA, 16802 (United States); Department of Materials Science and Engineering, Pennsylvania State University, University Park, PA, 16802 (United States); Park, Jun-Sang, E-mail: parkjs@aps.anl.gov [Advanced Photon Source, Argonne National Laboratory, Argonne, IL, 60439 (United States); Almer, Jonathan D., E-mail: almer@aps.anl.gov [Advanced Photon Source, Argonne National Laboratory, Argonne, IL, 60439 (United States)

    2017-04-15

    The d-spacing evolution of both in-plane and out-of-plane hydrides has been studied using in situ synchrotron radiation X-ray diffraction during thermo-mechanical cycling of cold-worked stress-relieved Zircaloy-4. The structure of the hydride precipitates is such that the δ{111} d-spacing of the planes aligned with the hydride platelet face is greater than the d-spacing of the 111 planes aligned with the platelet edges. Upon heating from room temperature, the δ{111} planes aligned with hydride plate edges exhibit bi-linear thermally-induced expansion. In contrast, the d-spacing of the (111) plane aligned with the hydride plate face initially contracts upon heating. These experimental results can be understood in terms of a reversal of stress state associated with precipitating or dissolving hydride platelets within the α-zirconium matrix. - Highlights: •The δ{111} d-spacings aligned with the hydride plate edges exhibit a bi-linear thermal expansion. •Stress state reversal is predicted with the onset of hydride dissolution. •During dissolution, the δ{111} planes oriented parallel to the hydride plate face initially contract upon heating. •Hydride d-spacings indicate that both in-plane (circumferential) and out-of-plane (radial) hydrides are in the same strain-state and likely in the same stress state as well.

  4. X-ray spectrometry with synchrotron radiation; Roentgenspektrometrie mit Synchrotronstrahlung

    Energy Technology Data Exchange (ETDEWEB)

    Mueller, Matthias [Physikalisch-Technische Bundesanstalt (PTB), Berlin (Germany). Arbeitsgruppe ' Roentgen- und IR-Spektrometrie' ; Gerlach, Martin; Holfelder, Ina; Hoenicke, Philipp; Lubeck, Janin; Nutsch, Andreas; Pollakowski, Beatrix; Streeck, Cornelia; Unterumsberger, Rainer; Weser, Jan; Beckhoff, Burkhard

    2014-12-15

    The X-ray spectrometry of the PTB at the BESSY II storage ring with radiation in the range from 78 eV to 10.5 keV is described. After a description of the instrumentation development reference-sample free X-ray fluorescence analysis, the determination of fundamental atomic parameters, X-ray fluorescence analysis under glance-angle incidence, highly-resolving absorption spectrometry, and emission spectrometry are considered. Finally liquid cells and in-situ measurement techniques are described. (HSI)

  5. Thermal expansion behavior of empressite, AgTe: A structural study by means of in situ high-temperature single-crystal X-ray diffraction

    Energy Technology Data Exchange (ETDEWEB)

    Bindi, Luca [Museo di Storia Naturale, sez. di Mineralogia, Universita di Firenze, Via La Pira 4, I-50121 Firenze (Italy)], E-mail: luca.bindi@unifi.it

    2009-04-03

    The crystal structure of empressite, AgTe, a rare silver telluride, has been investigated by in situ X-ray single-crystal diffraction methods within the temperature range 298-463 K. AgTe remains orthorhombic, space group Pmnb (Pnma as standard), and shows only normal thermal expansion over the entire temperature range. The unit-cell parameters show a gradual increase with the increase of temperature. Slight adjustments in the geometry of Ag-tetrahedra and in the crystal-chemical environment of tellurium atoms occur in a continuous way without abrupt structural changes. The coefficients of thermal expansion along various axes are: {alpha}{sub a} = 1.5 x 10{sup -5} K{sup -1}, {alpha}{sub b} = 3.0 x 10{sup -5} K{sup -1}, {alpha}{sub c} = 2.2 x 10{sup -5} K{sup -1}, and the bulk thermal expansion coefficient {alpha}{sub V} is 5.4 x 10{sup -5} K{sup -1} for the temperature range 298-463 K.

  6. Speckle-based at-wavelength metrology of x-ray optics at Diamond Light Source

    Science.gov (United States)

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

    2017-08-01

    To achieve high resolution and sensitivity on the nanometer scale, further development of X-ray optics is required. Although ex-situ metrology provides valuable information about X-ray optics, the ultimate performance of X-ray optics is critically dependent on the exact nature of the working conditions. Therefore, it is equally important to perform in-situ metrology at the optics' operating wavelength (`at-wavelength' metrology) to optimize the performance of X-ray optics and correct and minimize the collective distortions of the upstream beamline optics, e.g. monochromator, windows, etc. Speckle-based technique has been implemented and further improved at Diamond Light Source. We have demonstrated that the angular sensitivity for measuring the slope error of an optical surface can reach an accuracy of two nanoradians. The recent development of the speckle-based at-wavelength metrology techniques will be presented. Representative examples of the applications of the speckle-based technique will also be given - including optimization of X-ray mirrors and characterization of compound refraction lenses. Such a high-precision metrology technique will be extremely beneficial for the manufacture and in-situ alignment/optimization of X-ray mirrors for next-generation synchrotron beamlines.

  7. Revealing fatigue damage evolution in unidirectional composites for wind turbine blades using x-ray computed tomography

    DEFF Research Database (Denmark)

    Mikkelsen, Lars Pilgaard

    ’. Thereby, it will be possible to lower the cost of energy for wind energy based electricity. In the presented work, a lab-source x-ray computed tomography equipment (Zeiss Xradia 520 Versa) has been used in connection with ex-situ fatigue testing of uni-directional composites in order to identify fibre...... to other comparable x-ray studies) have been used in order to ensure a representative test volume during the ex-situ fatigue testing. Using the ability of the x-ray computed tomography to zoom into regions of interest, non-destructive, the fatigue damage evolution in a repeating ex-situ fatigue loaded test...... improving the fatigue resistance of non-crimp fabric used in the wind turbine industry can be made....

  8. Picosecond x-ray streak camera studies

    International Nuclear Information System (INIS)

    Kasyanov, Yu.S.; Malyutin, A.A.; Richardson, M.C.; Chevokin, V.K.

    1975-01-01

    Some initial results of direct measurement of picosecond x-ray emission from laser-produced plasmas are presented. A PIM-UMI 93 image converter tube, incorporating an x-ray sensitive photocathode, linear deflection, and three stages of image amplification was used to analyse the x-ray radiation emanating from plasmas produced from solid Ti targets by single high-intensity picosecond laser pulses. From such plasmas, the x-ray emission typically persisted for times of 60psec. However, it is shown that this detection system should be capable of resolving x-ray phenomena of much shorter duration. (author)

  9. High pressure X-ray studies

    International Nuclear Information System (INIS)

    Sikka, S.K.

    1981-01-01

    High pressure research has already led to new insights in the physical properties of materials and at times to the synthesis of new ones. In all this, X-ray diffraction has been a valuable diagnostic experimental tool. In particular, X-rays in high pressure field have been used (a) for crystallographic identification of high pressure polymorphs and (b) for study of the effect of pressure on lattice parameters and volume under isothermal conditions. The results in the area (a) are reviewed. The techniques of applying high pressures are described. These include both static and dynamic shockwave X-ray apparatus. To illustrate the effect of pressure, some of the pressure induced phase transitions in pure metals are described. It has been found that there is a clear trend for elements in any group of the periodic table to adopt similar structures at high pressures. These studies have enabled to construct generalized phase diagrams for many groups. In the case of alloys, the high pressure work done on Ti-V alloys is presented. (author)

  10. Selective molecular annealing: in situ small angle X-ray scattering study of microwave-assisted annealing of block copolymers.

    Science.gov (United States)

    Toolan, Daniel T W; Adlington, Kevin; Isakova, Anna; Kalamiotis, Alexis; Mokarian-Tabari, Parvaneh; Dimitrakis, Georgios; Dodds, Christopher; Arnold, Thomas; Terrill, Nick J; Bras, Wim; Hermida Merino, Daniel; Topham, Paul D; Irvine, Derek J; Howse, Jonathan R

    2017-08-09

    Microwave annealing has emerged as an alternative to traditional thermal annealing approaches for optimising block copolymer self-assembly. A novel sample environment enabling small angle X-ray scattering to be performed in situ during microwave annealing is demonstrated, which has enabled, for the first time, the direct study of the effects of microwave annealing upon the self-assembly behavior of a model, commercial triblock copolymer system [polystyrene-block-poly(ethylene-co-butylene)-block-polystyrene]. Results show that the block copolymer is a poor microwave absorber, resulting in no change in the block copolymer morphology upon application of microwave energy. The block copolymer species may only indirectly interact with the microwave energy when a small molecule microwave-interactive species [diethylene glycol dibenzoate (DEGDB)] is incorporated directly into the polymer matrix. Then significant morphological development is observed at DEGDB loadings ≥6 wt%. Through spatial localisation of the microwave-interactive species, we demonstrate targeted annealing of specific regions of a multi-component system, opening routes for the development of "smart" manufacturing methodologies.

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

    Science.gov (United States)

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

    2015-06-01

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

  12. X-ray excited optical luminescence, photoluminescence, photostimulated luminescence and x-ray photoemission spectroscopy studies on BaFBr:Eu

    CERN Document Server

    Subramanian, N; Govinda-Rajan, K; Mohammad-Yousuf; Santanu-Bera; Narasimhan, S V

    1997-01-01

    The results of x-ray excited optical luminescence (XEOL), photoluminescence (PL), photostimulated luminescence (PSL) and x-ray photoemission spectroscopy (XPS) studies on the x-ray storage phosphor BaFBr:Eu are presented in this paper. Analyses of XEOL, PL and PSL spectra reveal features corresponding to the transitions from 4f sup 6 td sup 1 to 4f sup 7 configurations in different site symmetries of Eu sup 2 sup +. Increasing x-ray dose is seen to lead to a red shift in the maximum of the PL excitation spectrum for the 391 nm emission. The XEOL and XPS spectra do not show any signature of Eu sup 3 sup + in the samples studied by us, directly raising doubts about the model of Takahashi et al in which Eu sup 2 sup + is expected to ionize to Eu sup 3 sup + upon x-ray irradiation and remain stable until photostimulation. XEOL and PSL experiments with simultaneous x-ray irradiation and He - Ne laser excitation as well as those with sequential x-ray irradiation and laser stimulation bring out the competition betwe...

  13. An x-ray detector for time-resolved studies

    International Nuclear Information System (INIS)

    Rodricks, B.; Brizard, C.; Clarke, R.; Lowe, W.

    1992-01-01

    The development of ultrahigh-brightness x-ray sources makes time-resolved x-ray studies more and more feasible. Improvements in x-ray optics components are also critical for obtaining the appropriate beam for a particular type of experiment. Moreover, fast parallel detectors will be essential in order to exploit the combination of high intensity x-ray sources and novel optics for time-resolved experiments. A CCD detector with a time resolution of microseconds has been developed at the Advanced Photon Source (APS). This detector is fully programmable using CAMAC electronics and a Micro Vax computer. The techniques of time-resolved x-ray studies, which include scattering, microradiography, microtomography, stroboscopy, etc., can be applied to a range of phenomena (including rapid thermal annealing, surface ordering, crystallization, and the kinetics of phase transition) in order to understand these time-dependent microscopic processes. Some of these applications will be illustrated by recent results performed at synchrotrons. New powerful x-ray sources now under construction offer the opportunity to apply innovative approaches in time-resolved work

  14. In situ surface X-ray diffraction study of ultrathin epitaxial Co films on Au(111) in alkaline solution

    International Nuclear Information System (INIS)

    Reikowski, Finn; Maroun, Fouad; Di, Nan; Allongue, Philippe; Ruge, Martin; Stettner, Jochim; Magnussen, Olaf M.

    2016-01-01

    The oxidation behavior of ultrathin electrodeposited Co films on Au(111) in alkaline electrolyte was studied using in situ surface X-ray scattering techniques employing synchrotron radiation and complementary optical reflectivity and electrochemical measurements. The films are formed at pH 4 and consist of (001)-oriented hcp Co crystallites that are several nm high, a few ten nm in diameter, and remain largely unchanged after electrolyte exchange to pH 12 solution. In the pre-oxidation peak only minor changes were observed in the diffraction studies, excluding the formation of Co(OH)_2 layers. In the potential regime of Co hydroxide formation a rapid reduction of the amount of Co is observed, while the characteristic height of the islands decreases only slightly. On longer times scales, growth of 3D crystals of Co(OH)_2 occurs as well as irreversible Co dissolution into the electrolyte is found. On the basis of the structural observations oxidation of the Co film is proposed to proceed via fast formation of an ultrathin passivating layer, followed by nucleation and growth of 3D hydroxide crystals at the grain boundaries in the Co deposit.

  15. Real-time x-ray scattering study of the initial growth of organic crystals on polymer brushes

    Energy Technology Data Exchange (ETDEWEB)

    An, Sung Yup; Ahn, Kwangseok; Kim, Doris Yangsoo; Lee, Dong Ryeol, E-mail: drlee@ssu.ac.kr [Department of Physics, Soongsil University, Seoul 156-743 (Korea, Republic of); Lee, Hyun-Hwi [Pohang Accelerator Laboratory, Pohang University of Science and Technology, Pohang 790-784 (Korea, Republic of); Cho, Jeong Ho, E-mail: jhcho94@skku.edu [Department of Chemical Engineering, SKKU Advanced Institute of Nanotechnology (SAINT) and Center for Human Interface Nano Technology (HINT), Sungkyunkwan University, Suwon 440-476 (Korea, Republic of)

    2014-04-21

    We studied the early-stage growth structures of pentacene organic crystals grown on polymer brushes using real-time x-ray scattering techniques. In situ x-ray reflectivity and atomic force microscopy analyses revealed that at temperatures close to the glass transition temperature of polymer brush, the pentacene overlayer on a polymer brush film showed incomplete condensation and 3D island structures from the first monolayer. A growth model based on these observations was used to quantitatively analyze the real-time anti-Bragg x-ray scattering intensities measured during pentacene growth to obtain the time-dependent layer coverage of the individual pentacene monolayers. The extracted total coverage confirmed significant desorption and incomplete condensation in the pentacene films deposited on the polymer brushes. These effects are ascribed to the change in the surface viscoelasticity of the polymer brushes around the glass transition temperature.

  16. An X-ray and optical study of the ultracompact X-ray binary A 1246-58

    NARCIS (Netherlands)

    in 't Zand, J.J.M.; Bassa, C.G.; Jonker, P.G.; Keek, L.; Verbunt, F.W.M.; Méndez, M.; Markwardt, C.B.

    2008-01-01

    Results are discussed of an X-ray and optical observation campaign of the low-mass X-ray binary A 1246-58 performed with instruments on Satellite per Astronomia X ("BeppoSAX"), the Rossi X-ray Timing Explorer (RXTE), the X-ray Multi-mirror Mission ("XMM-Newton"), the Swift mission, and the Very

  17. In-situ X-ray absorption spectroscopy analysis of capacity fade in nanoscale-LiCoO2

    International Nuclear Information System (INIS)

    Patridge, Christopher J.; Love, Corey T.; Swider-Lyons, Karen E.; Twigg, Mark E.; Ramaker, David E.

    2013-01-01

    The local structure of nanoscale (∼10–40 nm) LiCoO 2 is monitored during electrochemical cycling utilizing in-situ X-ray absorption spectroscopy (XAS). The high surface area of the LiCoO 2 nanoparticles not only enhances capacity fade, but also provides a large signal from the particle surface relative to the bulk. Changes in the nanoscale LiCoO 2 metal-oxide bond lengths, structural disorder, and chemical state are tracked during cycling by adapting the delta mu (Δμ) technique in complement with comprehensive extended X-ray absorption fine structure (EXAFS) modeling. For the first time, we use a Δμ EXAFS method, and by comparison of the difference EXAFS spectra, extrapolate significant coordination changes and reduction of cobalt species with cycling. This combined approach suggests Li–Co site exchange at the surface of the nanoscale LiCoO 2 as a likely factor in the capacity fade and irreversible losses in practical, microscale LiCoO 2 . - Graphical abstract: Electrochemical cycling of Li-ion batteries has strong impact on the structure and integrity of the cathode active material particularly near the surface/electrolyte interface. In developing a new method, we have used in-situ X-ray absorption spectroscopy during electrochemical cycling of nanoscale LiCoO 2 to track changes during charge and discharge and between subsequent cycles. Using difference spectra, several small changes in Co-O bond length, Co-O and Co-Co coordination, and site exchange between Co and Li sites can be tracked. These methods show promise as a new technique to better understand processes which lead to capacity fade and loss in Li-ion batteries. - Highlights: • A new method is developed to understand capacity fade in Li-ion battery cathodes. • Structural changes are tracked during Li intercalation/deintercalation of LiCoO 2 . • Surface structural changes are emphasized using nanoscale-LiCoO 2 and difference spectra. • Full multiple scattering calculations are used to

  18. Fatigue History and in-situ Loading Studies of the overload Effect Using High Resolution X-ray Strain Profiling

    International Nuclear Information System (INIS)

    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 max ) -p (ΔK) p ] γ 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. Arsenic speciation in solids using X-ray absorption spectroscopy

    Science.gov (United States)

    Foster, Andrea L.; Kim, Chris S.

    2014-01-01

    Synchrotron-based X-ray absorption spectroscopy (XAS) is an in situ, minimally-destructive, element-specific, molecular-scale structural probe that has been employed to study the chemical forms (species) of arsenic (As) in solid and aqueous phases (including rocks, soils, sediment, synthetic compounds, and numerous types of biota including humans) for more than 20 years. Although several excellent reviews of As geochemistry and As speciation in the environment have been published previously (including recent contributions in this volume), the explosion of As-XAS studies over the past decade (especially studies employing microfocused X-ray beams) warrants this new review of the literature and of data analysis methods.

  20. Applications of x ray absorption fine structure to the in situ study of the effect of cobalt in nickel hydrous oxide electrodes for fuel cells and rechargeable batteries

    Science.gov (United States)

    Kim, Sunghyun; Tryk, Donald A.; Scherson, Daniel A.; Antonio, Mark R.

    1993-01-01

    Electronic and structural aspects of composite nickel-cobalt hydrous oxides have been examined in alkaline solutions using in situ X-ray absorption fine structure (XAFS). The results obtained have indicated that cobalt in this material is present as cobaltic ions regardless of the oxidation state of nickel in the lattice. Furthermore, careful analysis of the Co K-edge Extended X-ray absorption fine structure data reveals that the co-electrodeposition procedure generates a single phase, mixed metal hydrous oxide, in which cobaltic ions occupy nickel sites in the NiO2 sheet-like layers and not two intermixed phases each consisting of a single metal hydrous oxide.

  1. Extended X-ray absorption fine structure and X-ray diffraction studies on supported Ni catalysts

    International Nuclear Information System (INIS)

    Aldea, N.; Marginean, P.; Yaning, Xie; Tiandou, Hu; Tao, Liu; Wu, Zhongua; ZhenYa, Dai

    1999-01-01

    In the first part of this paper, we present a study based on EXAFS spectroscopy. This method can yield structural information about the local environment around a specific atomic constituent in the amorphous materials, the location and chemical state of any catalytic atom on any support or point defect structures, in alloys and composites. EXAFS is a specific technique of the scattering of X-ray on materials. The present study is aimed toward elucidation of the local structure of Ni atoms and their interaction with oxide support. The second goal of the paper consists in X-ray diffraction on the same samples. X-ray diffraction method that is capable to determine average particle size, microstrains, probability of faults as well as particle size distribution function of supported Ni catalysts is presented. The method is based on the Fourier analysis of a single X-Ray diffraction profile. The results obtained on supported nickel catalysts, which are used in H/D isotopic exchange reactions are reported. The global structure is obtained with a new fitting method based on the Generalised Fermi Function facilities for approximation and Fourier transform of the experimental X-Ray line profiles. Both types of measurements were performed on Beijing Synchrotron Radiation Facilities (BSRF). (authors)

  2. X-ray microscopy and spectromicroscopy - tools for environmental studies

    International Nuclear Information System (INIS)

    Thieme, J.

    2002-01-01

    Full text: X-ray microscopy achieves a much higher resolution than light microscopy. This is due to the much shorter wavelength of X-rays compared to visible light. The smallest structures that can be seen in an X-ray microscope at present are about 20 nm in size. X-ray microscopy is also capable of imaging specimens directly in aqueous media. By choosing the wavelength of the X-radiation appropriately, it is possible to perform spectromicroscopy studies. Comprising, it is a tool very well suited to study colloidal structures in the environment. X-ray microscopy can be performed with two types of instruments. An X-ray microscope quickly takes high-resolution images of objects to be studied, whereas a scanning X-ray microscope is an analytical instrument for spectromicroscopy. Here, an object can be imaged using energies above and below the absorption edge of an element. Dividing both images gives rise to a map of the distribution of this element in the sample. Using near-edge resonances it is possible to conduct NEXAFS studies. As the X-ray energy is raised to match the absorption edge resonances are found, that reflect the chemical bonding state of the element. Therefore, it is possible with X-ray microscopy to combine high spatial resolution with high spectral resolution for studies of colloidal structures. The Institute of X-ray physics builds up an X-ray microscopy beamline at the electron storage ring BESSY II with both, an X-ray microscope and a scanning X-ray microscope. The status of this beamline will be presented in this talk. Colloidal structures play an important role in the environment. Due to their surface activity they are involved in various processes. Substances can be bound and immobilized or transported, colloids can attach to microorganisms building up microhabitats, and organic substances as humics can flocculate due the interaction with metals. A great variety of colloidal structures from the environment have been studied using X-ray

  3. Synchrotron x-ray methods in studies of thin organic film structure

    International Nuclear Information System (INIS)

    Gentle, I.

    2002-01-01

    Full text: In recent years, the study of the structures of organic films as thin as a single monolayer has been revolutionized by methods that take advantage of the characteristics of synchrotron radiation. In particular, the methods of grazing incidence X-ray diffraction (GIXD) and X-ray reflectivity have led to a number of valuable insights into structural aspects of thin films at molecular resolution. Our group has been studying films formed at the air/water interface as insoluble monolayers and subsequently transferred to solid substrates using either the vertical (Langmuir-Blodgett) or horizontal (Langmuir-Schaeffer) methods. The main aim of these experiments is to exert control over film structure in the direction parallel to the substrate surface. This is highly desirable in order to design devices that exploit the optical and electrooptical properties of functional materials, but is difficult to do. By varying the chemical structure of the film materials and controlling deposition conditions a degree of control is possible, but only using synchrotron methods can it be easily verified. We have also developed a novel method of rapidly collecting data from GIXD measurements by the application of area detection (imaging plates), which has made possible measurements of dynamic processes such as in-situ annealing. Such measurements are not possible using traditional scanning methods. One area of current interest is films composed of porphyrins as functional materials, either alone or as mixed films with fatty acids. We have been investigating ways of assembling porphyrins in such a way as to overcome the tendency to aggregate, and to produce patterning and ordered structures in the plane of the interface. Examples will be given of how film composition and deposition method affects the final structure, and of how X-ray methods can be used to elucidate both the structures and the mechanisms. Copyright (2002) Australian X-ray Analytical Association Inc

  4. A Versatile System for High-Throughput In Situ X-ray Screening and Data Collection of Soluble and Membrane-Protein Crystals

    Energy Technology Data Exchange (ETDEWEB)

    Broecker, Jana; Klingel, Viviane; Ou, Wei-Lin; Balo, Aidin R.; Kissick, David J.; Ogata, Craig M.; Kuo, Anling; Ernst, Oliver P.

    2016-10-12

    In recent years, in situ data collection has been a major focus of progress in protein crystallography. Here, we introduce the Mylar in situ method using Mylar-based sandwich plates that are inexpensive, easy to make and handle, and show significantly less background scattering than other setups. A variety of cognate holders for patches of Mylar in situ sandwich films corresponding to one or more wells makes the method robust and versatile, allows for storage and shipping of entire wells, and enables automated crystal imaging, screening, and goniometerbased X-ray diffraction data-collection at room temperature and under cryogenic conditions for soluble and membrane-protein crystals grown in or transferred to these plates. We validated the Mylar in situ method using crystals of the water-soluble proteins hen egg-white lysozyme and sperm whale myoglobin as well as the 7-transmembrane protein bacteriorhodopsin from Haloquadratum walsbyi. In conjunction with current developments at synchrotrons, this approach promises high-resolution structural studies of membrane proteins to become faster and more routine.

  5. In situ X-ray synchrotron study of organic semiconductor ultra-thin films growth

    International Nuclear Information System (INIS)

    Moulin, J.-F.; Dinelli, F.; Massi, M.; Albonetti, C.; Kshirsagar, R.; Biscarini, F.

    2006-01-01

    In this work we present an X-ray diffraction study of the early stages of growth of an organic semiconductor (sexithiophene, T 6 ) thin film prepared by high vacuum sublimation. Specular reflectometry and grazing incidence X-ray diffraction were used to monitor the formation of T 6 films on silicon oxide. Our results show that T 6 grows as a crystalline layer from the beginning of the evaporation. The reflectometry analysis suggests that, in the range of rates and temperatures studied, the growth is never layer by layer but rather 3D in nature. In-plane GIXD has allowed us to observe for the first time a thin film phase of T 6 formed of molecules standing normal to the substrate and arranged in a compressed unit cell with respect to the bulk, i.e. the unit cell parameters b and c are relatively smaller. We have followed the dynamics of formation of this new phase and identified the threshold of appearance of the bulk phase, which occurs above ∼5-6 monolayers. These results are relevant to the problem of organic thin film transistors, for which we have previously demonstrated experimentally that only the first two monolayers of T 6 films are involved in the electrical transport. The layers above the second one do not effectively contribute to charge mobility, either because they are more 'disordered' or because of a screening of the gate field

  6. Optical and x-ray alignment approaches for off-plane reflection gratings

    Science.gov (United States)

    Allured, Ryan; Donovan, Benjamin D.; DeRoo, Casey T.; Marlowe, Hannah R.; McEntaffer, Randall L.; Tutt, James H.; Cheimets, Peter N.; Hertz, Edward; Smith, Randall K.; Burwitz, Vadim; Hartner, Gisela; Menz, Benedikt

    2015-09-01

    Off-plane reflection gratings offer the potential for high-resolution, high-throughput X-ray spectroscopy on future missions. Typically, the gratings are placed in the path of a converging beam from an X-ray telescope. In the off-plane reflection grating case, these gratings must be co-aligned such that their diffracted spectra overlap at the focal plane. Misalignments degrade spectral resolution and effective area. In-situ X-ray alignment of a pair of off-plane reflection gratings in the path of a silicon pore optics module has been performed at the MPE PANTER beamline in Germany. However, in-situ X-ray alignment may not be feasible when assembling all of the gratings required for a satellite mission. In that event, optical methods must be developed to achieve spectral alignment. We have developed an alignment approach utilizing a Shack-Hartmann wavefront sensor and diffraction of an ultraviolet laser. We are fabricating the necessary hardware, and will be taking a prototype grating module to an X-ray beamline for performance testing following assembly and alignment.

  7. Frequencies of X-ray and fast neutron induced chromosome translocations in human peripheral blood lymphocytes as detected by in situ hybridization using chromosome specific DNA libraries

    International Nuclear Information System (INIS)

    Natarajan, A.T.; Darroudi, F.; Vermeulen, S.; Wiegant, J.

    1992-01-01

    DNA libraries of six human chromosomes were used to detect translocations in human lymphocytes induced by different doses of X-rays and fast neutrons. Results show that with X-rays, one can detect about 1.5 to 2.0 fold more translocations in comparison to dicentrics, whereas following fast neutron irradiation, the difference between these two classes of aberrations are significantly different at high doses. In addition, triple fluorescent in situ hybridization technique was used to study the frequencies of radiation-induced translocations involving a specific chromosome. Chromosome number 1 was found to be involved in translocations more frequently than chromosomes number 2, 3, 4, 8 and X. (author). 10 refs., 1 fig., 2 tabs

  8. Characteristics of a molybdenum X-pinch X-ray source as a probe source for X-ray diffraction studies

    International Nuclear Information System (INIS)

    Zucchini, F.; Chauvin, C.; Combes, P.; Sol, D.; Loyen, A.; Roques, B.; Grunenwald, J.; Bland, S. N.

    2015-01-01

    X-ray emission from a molybdenum X-pinch has been investigated as a potential probe for the high pressure states made in dynamic compression experiments. Studies were performed on a novel 300 kA, 400 ns generator which coupled the load directly to a low inductance capacitor and switch combination. The X-pinch load consisted of 4 crossed molybdenum wires of 13 μm diameter, crossed at an angle of 62°. The load height was 10 mm. An initial x-ray burst generated at the wire crossing point, radiated in the soft x-ray range (hυ < 10 keV). This was followed, 2–5 ns later, by at least one harder x-ray burst (hυ > 10 keV) whose power ranged from 1 to 7 MW. Time integrated spectral measurements showed that the harder bursts were dominated by K-alpha emission; though, a lower level, wide band continuum up to at least 30 keV was also present. Initial tests demonstrated that the source was capable of driving Laue diffraction experiments, probing uncompressed samples of LiF and aluminium

  9. In-situ X-ray diffraction activation study on an Fe/TiO2 pre-catalyst.

    Science.gov (United States)

    Rayner, Matthew K; Billing, David G; Coville, Neil J

    2014-06-01

    This study focuses on the use of in situ powder X-ray diffraction (PXRD) and quantitative phase analysis using the Rietveld method to monitor the structural properties of a titania-supported iron (10% Fe/TiO2) pre-catalyst during calcination (oxidation) and activation (reduction) in the temperature range 25-900°C. The TiO2 oxidation study revealed an increase in anatase particle size before the anatase to rutile phase transformation, lending credibility to the bridging mechanism proposed by Kim et al. [(2007), Mater. Sci. Forum, 534-536, 65-68]. Pre-catalyst oxidation experiments allowed for the determination of a suitable calcination temperature (450°C) of the pre-catalyst in terms of maximum hematite concentration and appropriate particle size. These experiments also confirmed that the anatase to rutile phase transformation occurred at higher temperatures after Fe addition and that anatase was the sole donor of Ti(4+) ions, which are known to migrate into hematite (Gennari et al., 1998), during the formation of pseudobrookite (Fe2TiO5) at temperatures above 690°C. Using the results from the oxidation experiments, two pre-catalyst samples were calcined at different temperatures; one to represent the preferred case and one to represent a case where the pre-catalyst had been excessively heated. Samples of the excessively heated catalysts were exposed to different reducing gas atmospheres (5, 10 and 100% H2/N2) and heated in the in situ PXRD reactor, so that diffraction data could be collected during the activation process. The results show that reduction with gases containing low concentrations of H2 (5 and 10%) led to the formation of ilmenite (FeTiO3) and we were able to show that both anatase and rutile are consumed in the reaction. Higher concentrations of H2 led to the formation of magnetite (Fe3O4) and metallic iron (Fe(0)). We also noted a decrease in the anatase to rutile transformation temperature under reducing atmospheres when compared with the pre

  10. MapX: An In Situ, Full-Frame X-Ray Spectroscopic Imager for the Biogenic Elements

    Science.gov (United States)

    Blake, David; Sarrazin, Philippe; Thompson, Kathy; Bristow, Thomas

    2016-01-01

    Microbial life exploits microscale disequilibria at boundaries where valence, chemical potential, pH, Eh, etc. vary on a length scale commensurate with the organisms themselves - tens to hundreds of micrometers. These disequilibria can exist within cracks or veins in rocks and ice, at inter- or intra-crystalline boundaries, at sediment/water or sediment/atmosphere interfaces, or even within fluid inclusions trapped inside minerals. The detection of accumulations of the biogenic elements C,N,O,P,S at appropriate concentrations on or in a mineral/ice substrate would constitute permissive evidence of extant life, but context is also required. Does the putative biosignature exist in a habitable environment? Under what conditions of P, T, and chemical potential was the host mineralogy formed? MapX is an arm-deployed contact instrument that directly images the biogenic elements C, N, O, P, S, as well as the cations of the rock-forming minerals (Na, Mg, Al, Si, K, Ca, Ti, Cr, Mn, Fe) and important anions such as Cl, Fl. The instrument provides element images having =100 micron lateral spatial resolution over a 2.5 cm X 2.5 cm area, as well as quantitative XRF spectra from ground-selected or instrument-selected Regions of Interest (ROI) on the sample. Quantitative XRF spectra from ROI can be translated into mineralogies using ground- or instrument-based algorithms. Either an X-ray tube source (X-ray fluorescence) or a radioisotope source such as 244-Cm (alpha-particle and gamma-ray fluorescence) can be used, and characteristic X-rays emitted from the sample are imaged onto an X-ray sensitive CCD through an X-ray MicroPore Optic (MPO). As a fluorescent source, 244-Cm is highly desirable in a MapX instrument intended for life detection since high-energy alpha-particles are unrivaled in fluorescence yield for the low-Z elements. The MapX design as well as baseline performance requirements for a MapX instrument intended for life detection/identification of habitable

  11. Room temperature redox reaction by oxide ion migration at carbon/Gd-doped CeO2 heterointerface probed by an in situ hard x-ray photoemission and soft x-ray absorption spectroscopies

    Directory of Open Access Journals (Sweden)

    Takashi Tsuchiya, Shogo Miyoshi, Yoshiyuki Yamashita, Hideki Yoshikawa, Kazuya Terabe, Keisuke Kobayashi and Shu Yamaguchi

    2013-01-01

    Full Text Available In situ hard x-ray photoemission spectroscopy (HX-PES and soft x-ray absorption spectroscopy (SX-XAS have been employed to investigate a local redox reaction at the carbon/Gd-doped CeO2 (GDC thin film heterointerface under applied dc bias. In HX-PES, Ce3d and O1s core levels show a parallel chemical shift as large as 3.2 eV, corresponding to the redox window where ionic conductivity is predominant. The window width is equal to the energy gap between donor and acceptor levels of the GDC electrolyte. The Ce M-edge SX-XAS spectra also show a considerable increase of Ce3+ satellite peak intensity, corresponding to electrochemical reduction by oxide ion migration. In addition to the reversible redox reaction, two distinct phenomena by the electrochemical transport of oxide ions are observed as an irreversible reduction of the entire oxide film by O2 evolution from the GDC film to the gas phase, as well as a vigorous precipitation of oxygen gas at the bottom electrode to lift off the GDC film. These in situ spectroscopic observations describe well the electrochemical polarization behavior of a metal/GDC/metal capacitor-like two-electrode cell at room temperature.

  12. Investigation of the internal electric field distribution under in situ x-ray irradiation and under low temperature conditions by the means of the Pockels effect

    International Nuclear Information System (INIS)

    Prekas, G; Sellin, P J; Veeramani, P; Davies, A W; Lohstroh, A; Oezsan, M E; Veale, M C

    2010-01-01

    The internal electric field distribution in cadmium zinc telluride (CdZnTe) x-ray and γ-ray detectors strongly affects their performance in terms of charge transport and charge collection properties. In CdZnTe detectors the electric field distribution is sensitively dependent on not only the nature of the metal contacts but also on the working conditions of the devices such as the temperature and the rate of external irradiation. Here we present direct measurements of the electric field profiles in CdZnTe detectors obtained using the Pockels electo-optic effect whilst under in situ x-ray irradiation. These data are also compared with alpha particle induced current pulses obtained by the transient current technique, and we discuss the influence of both low temperature and x-ray irradiation on the electric field evolution. Results from these studies reveal strong distortion of the electric field consistent with the build-up of space charge at temperatures below 250 K, even in the absence of external irradiation. Also, in the presence of x-ray irradiation levels a significant distortion in the electric field is observed even at room temperature which matches well the predicted theoretical model.

  13. Experimental studies on pulse soft X-ray generator

    International Nuclear Information System (INIS)

    Li Chengrong; Yang Qinchi; Luo Chengmu; Han Min

    1990-01-01

    Emission sources of soft x rays (2 keV < hv < 6 keV) from hot plasmas have been studied in a small gas-puff Z-pinch. The emission sources are a group of uncontinuous hot spots. The output of soft x rays from the hot spots have been measured and the effect of the initial gas density on the yield of soft x rays has been investigated

  14. Feasibility study on X-ray source with pinhole imaging method

    International Nuclear Information System (INIS)

    Qiu Rui; Li Junli

    2007-01-01

    In order to verify the feasibility of study on X-ray source with pinhole imaging method, and optimize the design of X-ray pinhole imaging system, an X-ray pinhole imaging equipment was set up. The change of image due to the change of the position and intensity of X-ray source was estimated with mathematical method and validated with experiment. The results show that the change of the spot position and gray of the spot is linearly related with the change of the position and intensity of X-ray source, so it is feasible to study X-ray source with pinhole imaging method in this application. The results provide some references for the design of X-ray pinhole imaging system. (authors)

  15. Comparative study of radiation dose between digital panoramic X-ray unit and general panoramic X-ray unit

    International Nuclear Information System (INIS)

    Li Qingshan; Duan Tao; Wang Xiaoyun; Zhao Li; Dong Jian; Wei Lei

    2010-01-01

    Objective: To compare the actual dose of patients who receive the same medical practice by either digital panoramic X-ray unit and general panoramic X-ray unit and give evidence for better selection of oral X-ray examination method. Methods: Round sheet lithium fluoride (LiF) thermoluminescent dosimeters (TLD) were used. The experiment was divided into natural background contrast group, general panoramic X-ray children group, general panoramic X-ray adults group, digital panoramic X-ray children group and digital panoramic X-ray adults group. The dosimeter of natural background radiation was placed at the office of the doctor, the dosimeters of general panoramic X-ray children group and general panoramic X-ray adults group were irradiated by different conditions according to the clinical application of panoramic X-ray to children and adults, the dosimeters of digital panoramic X-ray children group and digital panoramic X-ray adults group were irradiated by different conditions according to the clinical application of digital panoramic X-ray to children and adults. The thermoluminescent dosimeter was used to count and calculate the exposure doses in various groups. Results: The dose of children exposed in general panoramic X-ray unit was 1.28 times of that in digital panoramic X-ray unit, there was significant difference (t=6.904, P<0.01). The dose of adults exposed in general panoramic X-ray unit was 1.55 times of that in the digital panoramic X-ray unit, there also was significant difference (t=-11.514. P< 0.01). Conclusion: The digital panoramic X-ray unit can reduce the dose of patients, so the digital panoramic X-ray unit should be used as far as possible. (authors)

  16. Resonant inelastic x-ray scattering studies of elementary excitations

    NARCIS (Netherlands)

    Ament, Lucas Johannes Peter (Luuk)

    2010-01-01

    Resonant Inelastic X-ray Scattering (RIXS) is an X-ray in, X-ray out technique that enables one to study the dispersion of excitations in solids. In this thesis, we investigated how various elementary excitations of transition metal oxides show up in RIXS spectra.

  17. On-axis microscopes for the inelastic x-ray scattering beamline at NSLS-II

    Energy Technology Data Exchange (ETDEWEB)

    Gofron, K. J., E-mail: kgofron@bnl.gov; Cai, Y. Q.; Coburn, D. S.; Antonelli, S.; Suvorov, A. [National Synchrotron Light Source II, Brookhaven National Laboratory, Upton, NY 11973 (United States); Flores, J. [Department of Physics and Astronomy, Stony Brook University, NY 11794 (United States)

    2016-07-27

    A novel on-axis X-ray microscope with 3 µm resolution, 3x magnification, and a working distance of 600 mm for in-situ sample alignment and X-ray beam visualization for the Inelastic X-ray Scattering (IXS) beamline at NSLS-II is presented. The microscope uses reflective optics, which minimizes dispersion, and allows imaging from Ultraviolet (UV) to Infrared (IR) with specifically chosen objective components (coatings, etc.). Additionally, a portable high resolution X-ray microscope for KB mirror alignment and X-ray beam characterization was developed.

  18. Ion-induced nanopatterns on semiconductor surfaces investigated by grazing incidence x-ray scattering techniques

    Energy Technology Data Exchange (ETDEWEB)

    Carbone, D; Metzger, T H [ID01, ESRF, 6 rue Jules Horowitz, F-38043 Grenoble Cedex (France); Biermanns, A; Pietsch, U [Festkoerperphysik, Universitaet Siegen, D-57068 Siegen (Germany); Ziberi, B; Frost, F [Leibniz-Institut fuer Oberflaechenmodifizierung e.V., D-04318 Leipzig (Germany); Plantevin, O [Universite Paris-Sud, Centre de Spectrometrie Nucleaire et de Spectrometrie de Masse, UMR 8609, F-91405 Orsay (France)], E-mail: gcarbone@esrf.fr

    2009-06-03

    In this review we cover and describe the application of grazing incidence x-ray scattering techniques to study and characterize nanopattern formation on semiconductor surfaces by ion beam erosion under various conditions. It is demonstrated that x-rays under grazing incidence are especially well suited to characterize (sub)surface structures on the nanoscale with high spatial and statistical accuracy. The corresponding theory and data evaluation is described in the distorted wave Born approximation. Both ex situ and in situ studies are presented, performed with the use of a specially designed sputtering chamber which allows us to follow the temporal evolution of the nanostructure formation. Corresponding results show a general stabilization of the ordering wavelength and the extension of the ordering as a function of the ion energy and fluence as predicted by theory. The in situ measurements are especially suited to study the early stages of pattern formation, which in some cases reveal a transition from dot to ripple formation. For the case of medium energy ions crystalline ripples are formed buried under a semi-amorphous thick layer with a ripple structure at the surface being conformal with the crystalline/amorphous interface. Here, the x-ray techniques are especially advantageous since they are non-destructive and bulk-sensitive by their very nature. In addition, the GI x-ray techniques described in this review are a unique tool to study the evolving strain, a topic which remains to be explored both experimentally and theoretically.

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

    Science.gov (United States)

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

    2016-11-01

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

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

    International Nuclear Information System (INIS)

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

    2016-01-01

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

  1. In situ alkali-silica reaction observed by x-ray microscopy

    International Nuclear Information System (INIS)

    Kurtis, K.E.; Monteiro, P.J.M.; Brown, J.T.; Meyer-Ilse, W.

    1997-01-01

    In concrete, alkali metal ions and hydroxyl ions contributed by the cement and reactive silicates present in aggregate can participate in a destructive alkali-silica reaction (ASR). This reaction of the alkalis with the silicates produces a gel that tends to imbibe water found in the concrete pores, leading to swelling of the gel and eventual cracking of the affected concrete member. Over 104 cases of alkali-aggregate reaction in dams and spillways have been reported around the world. At present, no method exists to arrest the expansive chemical reaction which generates significant distress in the affected structures. Most existing techniques available for the examination of concrete microstructure, including ASR products, demand that samples be dried and exposed to high pressure during the observation period. These sample preparation requirements present a major disadvantage for the study of alkali-silica reaction. Given the nature of the reaction and the affect of water on its products, it is likely that the removal of water will affect the morphology, creating artifacts in the sample. The purpose of this research is to observe and characterize the alkali-silica reaction, including each of the specific reactions identified previously, in situ without introducing sample artifacts. For observation of unconditioned samples, x-ray microscopy offers an opportunity for such an examination of the alkali-silica reaction. Currently, this investigation is focusing on the effect of calcium ions on the alkali-silica reaction

  2. In situ alkali-silica reaction observed by x-ray microscopy

    Energy Technology Data Exchange (ETDEWEB)

    Kurtis, K.E.; Monteiro, P.J.M. [Univ. of California, Berkeley, CA (United States); Brown, J.T.; Meyer-Ilse, W. [Ernest Orlando Lawrence Berkeley National Lab., CA (United States)

    1997-04-01

    In concrete, alkali metal ions and hydroxyl ions contributed by the cement and reactive silicates present in aggregate can participate in a destructive alkali-silica reaction (ASR). This reaction of the alkalis with the silicates produces a gel that tends to imbibe water found in the concrete pores, leading to swelling of the gel and eventual cracking of the affected concrete member. Over 104 cases of alkali-aggregate reaction in dams and spillways have been reported around the world. At present, no method exists to arrest the expansive chemical reaction which generates significant distress in the affected structures. Most existing techniques available for the examination of concrete microstructure, including ASR products, demand that samples be dried and exposed to high pressure during the observation period. These sample preparation requirements present a major disadvantage for the study of alkali-silica reaction. Given the nature of the reaction and the affect of water on its products, it is likely that the removal of water will affect the morphology, creating artifacts in the sample. The purpose of this research is to observe and characterize the alkali-silica reaction, including each of the specific reactions identified previously, in situ without introducing sample artifacts. For observation of unconditioned samples, x-ray microscopy offers an opportunity for such an examination of the alkali-silica reaction. Currently, this investigation is focusing on the effect of calcium ions on the alkali-silica reaction.

  3. Multiscale structural study using scanning X-ray microscope

    International Nuclear Information System (INIS)

    Ohsumi, Hiroyuki; Arima, Taka-hisa

    2016-01-01

    Correspondence between structures at the atomic- and meso-scales can be given by scanning X-ray microscopy integrated with polarized X-ray diffractometry. Symmetry is the common structural feature available across multiple hierarchies. This article introduces a symmetry evaluation technique based on polarized X-ray diffractometry and describes two embodiments: chirality domain observation and antiferromagnetic domain observation. Multiscale structural studies would play an important role in uncovering universality of hierarchical structure. (author)

  4. The application of in-situ 3D X-ray diffraction in annealing experiments: First interpretation of substructure development in deformed NaCl

    DEFF Research Database (Denmark)

    Borthwick, Verity; Schmidt, Søren; Piazolo, Sandra

    2012-01-01

    In-situ 3D X-ray diffraction (3DXRD) annealing experiments were conducted at the ID-11 beamline at the European Synchrotron Radiation Facility in Grenoble. This allowed us to nondestructively document and subsequently analyse the development of substructures during heating, without the influence...... subgrain boundary formation. These results demonstrate that 3DXRD coupled with in-situ heating is a successful non-destructive technique for examining real-time postdeformational annealing in strongly deformed crystalline materials with complicated microstructures. © (2012) Trans Tech Publications...

  5. X-ray diffraction studies on single and mixed confectionery fats using synchrotron radiation

    International Nuclear Information System (INIS)

    MacMillan, S.C.; Roberts, K.J.; Wells, M.; Polgreen, M.; Smith, I.

    1999-01-01

    Full text: Understanding and refining the molecular-scale processes involved in the manufacture of structured materials such as long-chain hydrocarbon compounds is important in many commercial areas such as the petrochemical, biochemical, food, pharmaceutical and soap industries. In such processes crystallisation is an important separation, purification and preparation technique. Despite this our knowledge of the crystallisation process itself is surprisingly limited. In order to improve the crystallisation of confectionery fats, the crystallisation of it's main component, cocoa butter fat, must be properly understood. Cocoa butter fat can exhibit up to 6 polymorphic forms of different crystallographic structures with melting points varying from 17.3 deg C to 36.3 deg C. During the production of chocolate it is essential to control the polymorphic form of fats present, in order to produce a final product with the correct physical and rheological properties. Both shear rate and temperature are thought to play a crucial role in this process. The most widely used method for studying polymorphism is X-ray diffraction. Typical X-ray diffraction patterns of fats exhibit two groups of diffraction lines corresponding to the long and short spacings. The long spacings correspond to the planes formed by the methyl end groups and are dependent on the chain length and the angle of tilt of the component fatty acids of the glyceride molecules. The short spacings refer to the cross sectional packing of the hydrocarbon chain and are independent of the chain length. The relationship between crystallisation rate, polymorphic form, shear and the fat composition has for the first time been quantified, which will enable more accurate control of the polymorhic form in chocolate production. This has been achieved by developing an improved in-situ cell for X-ray studies. The X-ray studies are necessary for the examination of on-line studies under well controlled conditions of temperature

  6. X-ray diffraction studies on single and mixed confectionery fats using synchrotron radiation

    Energy Technology Data Exchange (ETDEWEB)

    MacMillan, S.C.; Roberts, K.J.; Wells, M.; Polgreen, M.; Smith, I. [Heriot-Watt University, Edinburgh, (United Kingdom). Department of Mechanical and Chemical Engineering, Centre for Molecular and Interface Engineering

    1999-12-01

    Full text: Understanding and refining the molecular-scale processes involved in the manufacture of structured materials such as long-chain hydrocarbon compounds is important in many commercial areas such as the petrochemical, biochemical, food, pharmaceutical and soap industries. In such processes crystallisation is an important separation, purification and preparation technique. Despite this our knowledge of the crystallisation process itself is surprisingly limited. In order to improve the crystallisation of confectionery fats, the crystallisation of it`s main component, cocoa butter fat, must be properly understood. Cocoa butter fat can exhibit up to 6 polymorphic forms of different crystallographic structures with melting points varying from 17.3 deg C to 36.3 deg C. During the production of chocolate it is essential to control the polymorphic form of fats present, in order to produce a final product with the correct physical and rheological properties. Both shear rate and temperature are thought to play a crucial role in this process. The most widely used method for studying polymorphism is X-ray diffraction. Typical X-ray diffraction patterns of fats exhibit two groups of diffraction lines corresponding to the long and short spacings. The long spacings correspond to the planes formed by the methyl end groups and are dependent on the chain length and the angle of tilt of the component fatty acids of the glyceride molecules. The short spacings refer to the cross sectional packing of the hydrocarbon chain and are independent of the chain length. The relationship between crystallisation rate, polymorphic form, shear and the fat composition has for the first time been quantified, which will enable more accurate control of the polymorhic form in chocolate production. This has been achieved by developing an improved in-situ cell for X-ray studies. The X-ray studies are necessary for the examination of on-line studies under well controlled conditions of temperature

  7. Real-time growth study of plasma assisted atomic layer epitaxy of InN films by synchrotron x-ray methods

    Energy Technology Data Exchange (ETDEWEB)

    Nepal, Neeraj [U.S. Naval Research Laboratory, 4555 Overlook Avenue SW, Washington, DC 20375; Anderson, Virginia R. [American Society for Engineering Education, 1818 N Street NW, Washington, DC 20036; Johnson, Scooter D. [U.S. Naval Research Laboratory, 4555 Overlook Avenue SW, Washington, DC 20375; Downey, Brian P. [U.S. Naval Research Laboratory, 4555 Overlook Avenue SW, Washington, DC 20375; Meyer, David J. [U.S. Naval Research Laboratory, 4555 Overlook Avenue SW, Washington, DC 20375; DeMasi, Alexander [Physics Department, Boston University, 590 Commonwealth Avenue, Boston, Massachusetts 02215; Robinson, Zachary R. [Department of Physics, SUNY College at Brockport, 350 New Campus Dr, Brockport, New York 14420; Ludwig, Karl F. [Physics Department, Boston University, 590 Commonwealth Avenue, Boston, Massachusetts 02215; Eddy, Charles R. [U.S. Naval Research Laboratory, 4555 Overlook Avenue SW, Washington, DC 20375

    2017-03-13

    The temporal evolution of high quality indium nitride (InN) growth by plasma-assisted atomic layer epitaxy (ALEp) on a-plane sapphire at 200 and 248 °C was probed by synchrotron x-ray methods. The growth was carried out in a thin film growth facility installed at beamline X21 of the National Synchrotron Light Source at Brookhaven National Laboratory and at beamline G3 of the Cornell High Energy Synchrotron Source, Cornell University. Measurements of grazing incidence small angle x-ray scattering (GISAXS) during the initial cycles of growth revealed a broadening and scattering near the diffuse specular rod and the development of scattering intensities due to half unit cell thick nucleation islands in the Yoneda wing with correlation length scale of 7.1 and 8.2 nm, at growth temperatures (Tg) of 200 and 248 °C, respectively. At about 1.1 nm (two unit cells) of growth thickness nucleation islands coarsen, grow, and the intensity of correlated scattering peak increased at the correlation length scale of 8.0 and 8.7 nm for Tg = 200 and 248 °C, respectively. The correlated peaks at both growth temperatures can be fitted with a single peak Lorentzian function, which support single mode growth. Post-growth in situ x-ray reflectivity measurements indicate a growth rate of ~0.36 Å/cycle consistent with the growth rate previously reported for self-limited InN growth in a commercial ALEp reactor. Consistent with the in situ GISAXS study, ex situ atomic force microscopy power spectral density measurements also indicate single mode growth. Electrical characterization of the resulting film revealed an electron mobility of 50 cm2/V s for a 5.6 nm thick InN film on a-plane sapphire, which is higher than the previously reported mobility of much thicker InN films grown at higher temperature by molecular beam epitaxy directly on sapphire. These early results indicated that in situ synchrotron x-ray study of the epitaxial growth kinetics of InN films is a very powerful method to

  8. X-ray spectroscopy and X-ray crystallography of metalloenzymes at XFELs

    International Nuclear Information System (INIS)

    Yano, Junko

    2016-01-01

    The ultra-bright femtosecond X-ray pulses provided by X-ray Free Electron Lasers (XFELs) open capabilities for studying the structure and dynamics of a wide variety of biological and inorganic systems beyond what is possible at synchrotron sources. Although the structure and chemistry at the catalytic sites have been studied intensively in both biological and inorganic systems, a full understanding of the atomic-scale chemistry requires new approaches beyond the steady state X-ray crystallography and X-ray spectroscopy at cryogenic temperatures. Following the dynamic changes in the geometric and electronic structure at ambient conditions, while overcoming X-ray damage to the redox active catalytic center, is key for deriving reaction mechanisms. Such studies become possible by using the intense and ultra-short femtosecond X-ray pulses from an XFEL, where sample is probed before it is damaged. We have developed methodology for simultaneously collecting crystallography data and X-ray emission spectra, using an energy dispersive spectrometer at ambient conditions. In addition, we have developed a way to collect metal L-edge data of dilute samples using soft X-rays at XFELs. The advantages and challenges of these methods will be described in this review. (author)

  9. X-Ray Radiographic Observation of Directional Solidification Under Microgravity: XRMON-GF Experiments on MASER12 Sounding Rocket Mission

    Science.gov (United States)

    Reinhart, G.; NguyenThi, H.; Bogno, A.; Billia, B.; Houltz, Y.; Loth, K.; Voss, D.; Verga, A.; dePascale, F.; Mathiesen, R. H.; hide

    2012-01-01

    The European Space Agency (ESA) - Microgravity Application Promotion (MAP) programme entitled XRMON (In situ X-Ray MONitoring of advanced metallurgical processes under microgravity and terrestrial conditions) aims to develop and perform in situ X-ray radiography observations of metallurgical processes in microgravity and terrestrial environments. The use of X-ray imaging methods makes it possible to study alloy solidification processes with spatio-temporal resolutions at the scales of relevance for microstructure formation. XRMON has been selected for MASER 12 sounding rocket experiment, scheduled in autumn 2011. Although the microgravity duration is typically six minutes, this short time is sufficient to investigate a solidification experiment with X-ray radiography. This communication will report on the preliminary results obtained with the experimental set-up developed by SSC (Swedish Space Corporation). Presented results dealing with directional solidification of Al-Cu confirm the great interest of performing in situ characterization to analyse dynamical phenomena during solidification processes.

  10. Planetary X-ray studies: past, present and future

    Science.gov (United States)

    Branduardi-Raymont, Graziella

    2016-07-01

    Our solar system is a fascinating physics laboratory and X-ray observations are now firmly established as a powerful diagnostic tool of the multiple processes taking place in it. The science that X-rays reveal encompasses solar, space plasma and planetary physics, and the response of bodies in the solar system to the impact of the Sun's activity. This talk will review what we know from past observations and what we expect to learn in the short, medium and long term. Observations with Chandra and XMM-Newton have demonstrated that the origin of Jupiter's bright soft X-ray aurorae lies in the Charge eXchange (CX) process, likely to involve the interaction with atmospheric neutrals of local magnetospheric ions, as well as those carried in the solar wind. At higher energies electron bremsstrahlung is thought to be the X-ray emitting mechanism, while the whole planetary disk acts as a mirror for the solar X-ray flux via Thomson and fluorescent scattering. This 'X-ray mirror' phenomenon is all that is observed from Saturn's disk, which otherwise lacks X-ray auroral features. The Earth's X-ray aurora is bright and variable and mostly due to electron bremsstrahlung and line emission from atmospheric species. Un-magnetised planets, Venus and Mars, do not show X-ray aurorae but display the interesting combination of mirroring the solar X-ray flux and producing X-rays by Solar Wind Charge eXchange (SWCX) in their exospheres. These processes respond to different solar stimulation (photons and solar wind plasma respectively) hence their relative contributions are seen to vary according to the Sun's output. Present and future of planetary X-ray studies are very bright. We are preparing for the arrival of the Juno mission at Jupiter this summer and for coordinated observations with Chandra and XMM-Newton on the approach and later during Juno's orbital phase. These will allow direct correlation of the local plasma conditions with the X-ray emissions and the establishment of the

  11. Design studies for ITER x-ray diagnostics

    International Nuclear Information System (INIS)

    Hill, K.W.; Bitter, M.; von Goeler, S.; Hsuan, H.

    1995-01-01

    Concepts for adapting conventional tokamak x-ray diagnostics to the harsh radiation environment of ITER include use of grazing-incidence (GI) x-ray mirrors or man-made Bragg multilayer (ML) elements to remove the x-ray beam from the neutron beam, or use of bundles of glass-capillary x-ray ''light pipes'' embedded in radiation shields to reduce the neutron/gamma-ray fluxes onto the detectors while maintaining usable x-ray throughput. The x-ray optical element with the broadest bandwidth and highest throughput, the GI mirror, can provide adequate lateral deflection (10 cm for a deflected-path length of 8 m) at x-ray energies up to 12, 22, or 30 keV for one, two, or three deflections, respectively. This element can be used with the broad band, high intensity x-ray imaging system (XIS), the pulseheight analysis (PHA) survey spectrometer, or the high resolution Johann x-ray crystal spectrometer (XCS), which is used for ion-temperature measurement. The ML mirrors can isolate the detector from the neutron beam with a single deflection for energies up to 50 keV, but have much narrower bandwidth and lower x-ray power throughput than do the GI mirrors; they are unsuitable for use with the XIS or PHA, but they could be used with the XCS; in particular, these deflectors could be used between ITER and the biological shield to avoid direct plasma neutron streaming through the biological shield. Graded-d ML mirrors have good reflectivity from 20 to 70 keV, but still at grazing angles (<3 mrad). The efficiency at 70 keV for double reflection (10 percent), as required for adequate separation of the x-ray and neutron beams, is high enough for PHA requirements, but not for the XIS. Further optimization may be possible

  12. X-ray diffraction and X-ray standing-wave study of the lead stearate film structure

    Energy Technology Data Exchange (ETDEWEB)

    Blagov, A. E.; Dyakova, Yu. A.; Kovalchuk, M. V.; Kohn, V. G.; Marchenkova, M. A.; Pisarevskiy, Yu. V.; Prosekov, P. A., E-mail: prosekov@crys.ras.ru [Russian Academy of Sciences, Shubnikov Institute of Crystallography (Russian Federation)

    2016-05-15

    A new approach to the study of the structural quality of crystals is proposed. It is based on the use of X-ray standing-wave method without measuring secondary processes and considers the multiwave interaction of diffraction reflections corresponding to different harmonics of the same crystallographic reflection. A theory of multiwave X-ray diffraction is developed to calculate the rocking curves in the X-ray diffraction scheme under consideration for a long-period quasi-one-dimensional crystal. This phase-sensitive method is used to study the structure of a multilayer lead stearate film on a silicon substrate. Some specific structural features are revealed for the surface layer of the thin film, which are most likely due to the tilt of the upper layer molecules with respect to the external normal to the film surface.

  13. Visualizing and measuring flow in shale matrix using in situ synchrotron X-ray microtomography

    Science.gov (United States)

    Kohli, A. H.; Kiss, A. M.; Kovscek, A. R.; Bargar, J.

    2017-12-01

    Natural gas production via hydraulic fracturing of shale has proliferated on a global scale, yet recovery factors remain low because production strategies are not based on the physics of flow in shale reservoirs. In particular, the physical mechanisms and time scales of depletion from the matrix into the simulated fracture network are not well understood, limiting the potential to optimize operations and reduce environmental impacts. Studying matrix flow is challenging because shale is heterogeneous and has porosity from the μm- to nm-scale. Characterizing nm-scale flow paths requires electron microscopy but the limited field of view does not capture the connectivity and heterogeneity observed at the mm-scale. Therefore, pore-scale models must link to larger volumes to simulate flow on the reservoir-scale. Upscaled models must honor the physics of flow, but at present there is a gap between cm-scale experiments and μm-scale simulations based on ex situ image data. To address this gap, we developed a synchrotron X-ray microscope with an in situ cell to simultaneously visualize and measure flow. We perform coupled flow and microtomography experiments on mm-scale samples from the Barnett, Eagle Ford and Marcellus reservoirs. We measure permeability at various pressures via the pulse-decay method to quantify effective stress dependence and the relative contributions of advective and diffusive mechanisms. Images at each pressure step document how microfractures, interparticle pores, and organic matter change with effective stress. Linking changes in the pore network to flow measurements motivates a physical model for depletion. To directly visualize flow, we measure imbibition rates using inert, high atomic number gases and image periodically with monochromatic beam. By imaging above/below X-ray adsorption edges, we magnify the signal of gas saturation in μm-scale porosity and nm-scale, sub-voxel features. Comparing vacuumed and saturated states yields image

  14. Hydrogen Absorption in Metal Thin Films and Heterostructures Investigated in Situ with Neutron and X-ray Scattering

    Directory of Open Access Journals (Sweden)

    Sara J. Callori

    2016-05-01

    Full Text Available Due to hydrogen possessing a relatively large neutron scattering length, hydrogen absorption and desorption behaviors in metal thin films can straightforwardly be investigated by neutron reflectometry. However, to further elucidate the chemical structure of the hydrogen absorbing materials, complementary techniques such as high resolution X-ray reflectometry and diffraction remain important too. Examples of work on such systems include Nb- and Pd-based multilayers, where Nb and Pd both have strong affinity to hydrogen. W/Nb and Fe/Nb multilayers were measured in situ with unpolarized and polarized neutron reflectometry under hydrogen gas charging conditions. The gas-pressure/hydrogen-concentration dependence, the hydrogen-induced macroscopic film swelling as well as the increase in crystal lattice plane distances of the films were determined. Ferromagnetic-Co/Pd multilayers were studied with polarized neutron reflectometry and in situ ferromagnetic resonance measurements to understand the effect of hydrogen absorption on the magnetic properties of the system. This electronic effect enables a novel approach for hydrogen sensing using a magnetic readout scheme.

  15. Bismuth X-ray absorber studies for TES microcalorimeters

    International Nuclear Information System (INIS)

    Sadleir, J.E.; Bandler, S.R.; Brekosky, R.P.; Chervenak, J.; Figueroa-Feliciano, E.; Finkbeiner, F.; Iyomoto, N.; Kelley, R.L.; Kilbourne, C.A.; King, J.M.; Porter, F.S.; Robinson, I.K.; Saab, T.; Talley, D.J.

    2006-01-01

    Bismuth's large atomic number and low carrier density makes it an attractive X-ray absorber material for microcalorimeters. Bismuth's long Fermi wavelength and long mean free paths have motivated much interest in the fabrication of high quality bismuth films to study quantum size effects. Despite such incentives, fabrication of high quality bismuth films has proven difficult, and measured properties of such films are highly variable in the literature. Implementing a bismuth deposition process for TES (superconducting Transition Edge Sensor) device fabrication presents additional challenges particularly at interfaces due to the inherent granularity and surface roughness of its films, its low melting point, and its tendency to diffuse and form undesired intermetallic phases. We report observations of Bi-Cu and Bi-Au diffusion in our devices correlating with large shifts in T c (superconducting transition temperature). Using SEM and in situ R vs T annealing experiments we have been able to study these diffusion processes and identify their activation temperatures

  16. In-situ X-ray absorption spectroscopy analysis of capacity fade in nanoscale-LiCoO{sub 2}

    Energy Technology Data Exchange (ETDEWEB)

    Patridge, Christopher J. [NRC/NRL Cooperative Research Associate, U.S. Naval Research Laboratory, Washington, DC 20375 (United States); Love, Corey T., E-mail: corey.love@nrl.navy.mil [Chemistry Division, Code 6113, U.S. Naval Research Laboratory, Washington, DC 20375 (United States); Swider-Lyons, Karen E. [Chemistry Division, Code 6113, U.S. Naval Research Laboratory, Washington, DC 20375 (United States); Twigg, Mark E. [Electronics Science and Technology Division, Code 6812, U.S. Naval Research Laboratory, Washington, DC 20375 (United States); Ramaker, David E. [Chemistry Division, Code 6189, U.S. Naval Research laboratory, Washington, DC 20375 (United States)

    2013-07-15

    The local structure of nanoscale (∼10–40 nm) LiCoO{sub 2} is monitored during electrochemical cycling utilizing in-situ X-ray absorption spectroscopy (XAS). The high surface area of the LiCoO{sub 2} nanoparticles not only enhances capacity fade, but also provides a large signal from the particle surface relative to the bulk. Changes in the nanoscale LiCoO{sub 2} metal-oxide bond lengths, structural disorder, and chemical state are tracked during cycling by adapting the delta mu (Δμ) technique in complement with comprehensive extended X-ray absorption fine structure (EXAFS) modeling. For the first time, we use a Δμ EXAFS method, and by comparison of the difference EXAFS spectra, extrapolate significant coordination changes and reduction of cobalt species with cycling. This combined approach suggests Li–Co site exchange at the surface of the nanoscale LiCoO{sub 2} as a likely factor in the capacity fade and irreversible losses in practical, microscale LiCoO{sub 2}. - Graphical abstract: Electrochemical cycling of Li-ion batteries has strong impact on the structure and integrity of the cathode active material particularly near the surface/electrolyte interface. In developing a new method, we have used in-situ X-ray absorption spectroscopy during electrochemical cycling of nanoscale LiCoO{sub 2} to track changes during charge and discharge and between subsequent cycles. Using difference spectra, several small changes in Co-O bond length, Co-O and Co-Co coordination, and site exchange between Co and Li sites can be tracked. These methods show promise as a new technique to better understand processes which lead to capacity fade and loss in Li-ion batteries. - Highlights: • A new method is developed to understand capacity fade in Li-ion battery cathodes. • Structural changes are tracked during Li intercalation/deintercalation of LiCoO{sub 2}. • Surface structural changes are emphasized using nanoscale-LiCoO{sub 2} and difference spectra. • Full multiple

  17. X-ray optics and X-ray microscopes: new challenges

    International Nuclear Information System (INIS)

    Susini, J.

    2004-01-01

    main fields of applications are driven by the unique attributes of X-ray microscopy in the multi-keV energy range: i) access to K-absorption edges and fluorescence emission lines of medium-light elements and L,M - edges of heavy materials for micro-spectroscopy (e.g. XANES), chemical or trace element mapping ii) higher penetration depths compared to soft X-rays allowing imaging of thicker samples, iii) favorable wavelengths for diffraction studies and iv) generally large focal lengths and depths of focus which are advantageous for the use of specific sample environments (high pressure, controlled temperatures....). Typical experiments can be broadly divided into two categories: i) morphological studies which require high spatial resolution and are therefore well adapted to 2D or 3D transmission full-field microscopy. ii) studies dealing with co-localization and/or speciation of trace elements in heterogeneous matrices at the micron scale. Following a brief account on the basic principles and methods, strengths and weaknesses of X-ray microscopy and spectro-microscopy techniques in the 1 - 30 keV range will be discussed and illustrated by examples of applications. The main technical developments, involving new focusing lenses or novel phase contrast geometry, will be presented. (author)

  18. At-wavelength metrology of x-ray optics at Diamond Light Source

    Science.gov (United States)

    Wang, Hongchang; Berujon, Sebastien; Sutter, John; Alcock, Simon G.; Sawhney, Kawal

    2014-09-01

    Modern, third-generation synchrotron radiation sources provide coherent and extremely bright beams of X-ray radiation. The successful exploitation of such beams depends to a significant extent on imperfections and misalignment of the optics employed on the beamlines. This issue becomes even more critical with the increasing use of active optics, and the desire to achieve diffraction-limited and coherence-preserving X-ray beams. In recent years, significant progress has been made to improve optic testing and optimization techniques, especially those using X-rays for so-called atwavelength metrology. These in-situ and at-wavelength metrology methods can be used not only to optimize the performance of X-ray optics, but also to correct and minimize the collective distortions of upstream beamline optics, including monochromators, and transmission windows. An overview of at-wavelength metrology techniques implemented at Diamond Light Source is presented, including grating interferometry and X-ray near-field speckle based techniques. Representative examples of the application of these techniques are also given, including in-situ and atwavelength calibration and optimization of: active, piezo bimorph mirrors; Kirkpatrick-Baez (KB) mirrors; and refractive optics such as compound refractive lenses.

  19. X-ray astronomy

    International Nuclear Information System (INIS)

    Culhane, J.L.; Sanford, P.W.

    1981-01-01

    X-ray astronomy has been established as a powerful means of observing matter in its most extreme form. The energy liberated by sources discovered in our Galaxy has confirmed that collapsed stars of great density, and with intense gravitational fields, can be studied by making observations in the X-ray part of the electromagnetic spectrum. The astronomical objects which emit detectable X-rays include our own Sun and extend to quasars at the edge of the Universe. This book describes the history, techniques and results obtained in the first twenty-five years of exploration. Space rockets and satellites are essential for carrying the instruments above the Earth's atmosphere where it becomes possible to view the X-rays from stars and nebulae. The subject is covered in chapters, entitled: the birth of X-ray astronomy; the nature of X-radiation; X-rays from the Sun; solar-flare X-rays; X-rays from beyond the solar system; supernovae and their remnants; X-rays from binary stars; white dwarfs and neutron stars; black holes; X-rays from galaxies and quasars; clusters of galaxies; the observatories of the future. (author)

  20. 2 and 3 dimensional systems studied using x-ray crystallographic techniques

    International Nuclear Information System (INIS)

    Schultz, T. M.

    1998-01-01

    Dodecanethiol is known to self assemble on pure Au(111) surfaces. Grazing incidence X-ray diffraction (GIXD) experiments have been performed on this surface under true equilibrium conditions, using an in-situ cell. In addition an extended ex-situ data set of dodecanethiol on gold has been collected. Finally the structure of the cleaved (OOι) surface of benzamide is presented, based on GIXD measurements. Structural models for tetramethylammonium tetrafluoroborate based on rigid body TLX refinements are presented. A comparison between three different data collection methods is carried out and the appearance of a twinned structure at the 158 K phase transition is discussed. The critical temperature of the phase transition is determined. (au)

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

    Science.gov (United States)

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

    2013-03-15

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

  2. 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.

    Science.gov (United States)

    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 (film formation processes. The high-energy synchrotron-radiation based x-rays result in small scattering angles (industry-relevant processes. We openly encourage the materials research community to contact us for collaborative opportunities using this unique and versatile scientific instrument.

  3. Phase transformation in sol-gel prepared zirconia using in-situ high temperature X-ray diffraction

    International Nuclear Information System (INIS)

    Srinivasan, R.; Davis, B.H.; Hubbard, C.R.; Cavin, O.B.; Porter, W.D.

    1991-01-01

    Zirconia was precipitated at a pH of 10.5 by admixing a solution of ZrCl 4 and NH 4 OH both rapidly (∼ 1 min) and slowly (∼ 8 hr). The precipitate was calcined at 500C for 5 hours and then furnace cooled. The former exhibited monoclinic phase while the latter yielded tetragonal phase. The pathway from amorphous to crystalline form was followed by in-situ high temperature X-ray diffraction in flowing air and in He. The data showed the evolution of the tetragonal crystalline phase on heating. On rapid cooling the tetragonal phase is retained at R.T., and on slow cooling the transformation to monoclinic phase occurs in air

  4. In situ x-ray scattering studies of the Au(111)/electrolyte interface

    International Nuclear Information System (INIS)

    Wang, Jia; Ocko, B.M.; Davenport, A.J.; Isaacs, H.S.

    1991-01-01

    The adsorption of anions at the Au(111) electrode and the subsequent effect on the gold surface structure have been investigated using x-ray specular reflectivity and grazing incident angle diffraction techniques. The top layer of gold atoms undergoes a reversible phase transition between the (1x1) bulk termination and a (23x√ bar 3) reconstructed phase on changing the potential. The shifts of the phase transition potential in NaCland NaBr solutions from the one in NaF can be understood by the anion adsorption induced charge effect. The reconstruction formation rate increases in chloride and bromide solutions due to an increase in the surface mobility with anion adsorption. Adsorbed chloride and bromide monolayers can be monitored during a potential scan by the specular reflectivity

  5. Characterization of Polycrystalline Materials Using Synchrotron X-ray Imaging and Diffraction Techniques

    DEFF Research Database (Denmark)

    Ludwig, Wolfgang; King, A.; Herbig, M.

    2010-01-01

    The combination of synchrotron radiation x-ray imaging and diffraction techniques offers new possibilities for in-situ observation of deformation and damage mechanisms in the bulk of polycrystalline materials. Minute changes in electron density (i.e., cracks, porosities) can be detected using...... propagation based phase contrast imaging, a 3-D imaging mode exploiting the coherence properties of third generation synchrotron beams. Furthermore, for some classes of polycrystalline materials, one may use a 3-D variant of x-ray diffraction imaging, termed x-ray diffraction contrast tomography. X-ray...

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

    Energy Technology Data Exchange (ETDEWEB)

    Weber, J. K. R.; Alderman, O. L. G. [Materials Development, Inc., Arlington Heights, Illinois 60004 (United States); Advanced Photon Source, Argonne National Laboratory, Argonne, Illinois 60439 (United States); Tamalonis, A.; Sendelbach, S. [Materials Development, Inc., Arlington Heights, Illinois 60004 (United States); Benmore, C. J. [Advanced Photon Source, Argonne National Laboratory, Argonne, Illinois 60439 (United States); Hebden, A.; Williamson, M. A. [Nuclear Engineering Division, Argonne National Laboratory, Argonne, Illinois 60439 (United States)

    2016-07-15

    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.

  7. X-ray imaging with compound refractive lens and microfocus X-ray tube

    OpenAIRE

    Pina, Ladislav; Dudchik, Yury; Jelinek, Vaclav; Sveda, Libor; Marsik, Jiri; Horvath, Martin; Petr, Ondrej

    2008-01-01

    Compound refractive lenses (CRL), consisting of a lot number in-line concave microlenses made of low-Z material were studied. Lenses with focal length 109 mm and 41 mm for 8-keV X-rays, microfocus X-ray tube and X-ray CCD camera were used in experiments. Obtained images show intensity distribution of magnified microfocus X-ray source focal spot. Within the experiments, one lens was also used as an objective lens of the X-ray microscope, where the copper anode X-ray microfocus tube served as a...

  8. In situ synchrotron X-ray powder diffraction study of the early hydration of α-tricalcium phosphate/tricalcium silicate composite bone cement

    Energy Technology Data Exchange (ETDEWEB)

    Morejon-Alonso, Loreley; Correa, Jose Raul, E-mail: lmorejon@fq.uh.cu [Departamento de Quimica General, Facultad de Quimica, Universidad de La Habana, UH (Cuba); Motisuke, Mariana [Universidade Federal de Sao Paulo (UNIFESP), Sao Jose dos Campos, SP (Brazil); Carrodeguas, Raul Garcia [Universidade Federal de Campina Grande (UFCG), Campina Grande, PB (Brazil). Laboratorio de Avaliacao e Desenvolvimento de Biomateriais do Nordeste; Santos, Luis Alberto dos [Universidade Federal do Rio Grande do Sul (UFRGS), Porto Alegre, RS (Brazil). Escola de Engenharia. Departamento de Materiais

    2015-01-15

    Bioactivity, osteogenicity and mechanical properties of α-tricalcium phosphate (α-TCP) based phosphates cements can be improved by adding tricalcium silicate (C{sub 3}S); however, the addition of C{sub 3}S delays the precipitation and growth of calcium deficient hydroxyapatite (CDHA). Thus, the aim of this work was the study of in situ setting reaction of α-TCP/C{sub 3}S composite bone cement under high energy X-ray generated by a synchrotron source within the first 72h. The results showed that the addition of C{sub 3}S induces the precipitation of nanosized CDHA at early times depending on the added content. Calculated crystallite sizes showed that the higher the content of C{sub 3}S, the smaller the crystal size at the beginning of the precipitation. These results are different from those obtained by conventional XRD method, suggesting that the proposed technique is a powerful tool in determining the composition and extent of reaction of CPCs surfaces in real time. (author)

  9. Growth and structure of water on SiO2 films on Si investigated byKelvin probe microscopy and in situ X-ray Spectroscopies

    Energy Technology Data Exchange (ETDEWEB)

    Verdaguer, A.; Weis, C.; Oncins, G.; Ketteler, G.; Bluhm, H.; Salmeron, M.

    2007-06-14

    The growth of water on thin SiO{sub 2} films on Si wafers at vapor pressures between 1.5 and 4 torr and temperatures between -10 and 21 C has been studied in situ using Kelvin Probe Microscopy and X-ray photoemission and absorption spectroscopies. From 0 to 75% relative humidity (RH) water adsorbs forming a uniform film 4-5 layers thick. The surface potential increases in that RH range by about 400 mV and remains constant upon further increase of the RH. Above 75% RH the water film grows rapidly, reaching 6-7 monolayers at around 90% RH and forming a macroscopic drop near 100%. The O K-edge near-edge X-ray absorption spectrum around 75% RH is similar to that of liquid water (imperfect H-bonding coordination) at temperatures above 0 C and ice-like below 0 C.

  10. X-Ray Diffraction for In-Situ Mineralogical Analysis of Planetesimals.

    Science.gov (United States)

    Sarrazin, P.; Blake, D. F.; Dera, P.; Downs, R. T.; Taylor, J.

    2017-12-01

    X-ray diffraction (XRD) is a general purpose technique for definitive, quantitative mineralogical analysis. When combined with XRF data for sample chemistry, XRD analyses yield as complete a characterization as is possible by any spacecraft-capable techniques. The MSL CheMin instrument, the first XRD instrument flown in space, has been used to establish the quantitative mineralogy of the Mars global soil, to discover the first habitable environment on another planet, and to provide the first in-situ evidence of silicic volcanism on Mars. CheMin is now used to characterize the depositional and diagenetic environments associated with the mudstone sediments of lower strata of Mt. Sharp. Conventional powder XRD requires samples comprised of small grains presented in random orientations. In CheMin, sample cells are vibrated to cause loose powder to flow within the cell, driven by granular convection, which relaxes the requirement for fine grained samples. Nevertheless, CheMin still requires mechanisms to collect, crush, sieve and deliver samples before analysis. XTRA (Extraterrestrial Regolith Analyzer) is an evolution of CheMin intended to analyze fines in as-delivered surface regolith, without sample preparation. Fine-grained regolith coats the surfaces of most airless bodies in the solar system, and because this fraction is typically comminuted from the rocky regolith, it can often be used as a proxy for the surface as a whole. HXRD (Hybrid-XRD) is concept under development to analyze rocks or soils without sample preparation. Like in CheMin, the diffracted signal is collected with direct illumination CCD's. If the material is sufficiently fine-grained, a powder XRD pattern of the characteristic X-ray tube emission is obtained, similar to CheMin or XTRA. With coarse grained crystals, the white bremsstrahlung radiation of the tube is diffracted into Laue patterns. Unlike typical Laue applications, HXRD uses the CCD's capability to distinguish energy and analyze the

  11. X-Ray Optics at NASA Marshall Space Flight Center

    Science.gov (United States)

    O'Dell, Stephen L.; Atkins, Carolyn; Broadway, David M.; Elsner, Ronald F.; Gaskin, Jessica A.; Gubarev, Mikhail V.; Kilaru, Kiranmayee; Kolodziejczak, Jeffery J.; Ramsey, Brian D.; Roche, Jacqueline M.; hide

    2015-01-01

    NASA's Marshall Space Flight Center (MSFC) engages in research, development, design, fabrication, coating, assembly, and testing of grazing-incidence optics (primarily) for x-ray telescope systems. Over the past two decades, MSFC has refined processes for electroformed-nickel replication of grazing-incidence optics, in order to produce high-strength, thin-walled, full-cylinder x-ray mirrors. In recent years, MSFC has used this technology to fabricate numerous x-ray mirror assemblies for several flight (balloon, rocket, and satellite) programs. Additionally, MSFC has demonstrated the suitability of this technology for ground-based laboratory applications-namely, x-ray microscopes and cold-neutron microscopes and concentrators. This mature technology enables the production, at moderately low cost, of reasonably lightweight x-ray telescopes with good (15-30 arcsecond) angular resolution. However, achieving arcsecond imaging for a lightweight x-ray telescope likely requires development of other technologies. Accordingly, MSFC is conducting a multi-faceted research program toward enabling cost-effective production of lightweight high-resolution x-ray mirror assemblies. Relevant research topics currently under investigation include differential deposition for post-fabrication figure correction, in-situ monitoring and control of coating stress, and direct fabrication of thin-walled full-cylinder grazing-incidence mirrors.

  12. a Synoptic Study of AN X-Ray Nova in Outburst

    Science.gov (United States)

    McClintock, Jeffrey

    Optical studies of X-ray novae in quiescence have yielded compelling evidence for black holes in binary systems. However, X-ray studies in quiescence are severely constrained by the near absence of high energy emission. Thus, further observational advances in black hole astrophysics require a substantial commitment to observe X-ray novae in outburst in just that spectral range accessible to XTE. We propose an agressive campaign of X-ray observations of the next non-pulsing X-ray nova that rises above 3 Crab at 2-10 keV. We further propose a coordinated and intensive campaign of optical and radio observations covering both hemispheres. The observations will provide a full temporal and spectral view of the outburst cycle.

  13. High-resolution X-ray diffraction studies of multilayers

    DEFF Research Database (Denmark)

    Christensen, Finn Erland; Hornstrup, Allan; Schnopper, H. W.

    1988-01-01

    High-resolution X-ray diffraction studies of the perfection of state-of-the-art multilayers are presented. Data were obtained using a triple-axis perfect-crystal X-ray diffractometer. Measurements reveal large-scale figure errors in the substrate. A high-resolution triple-axis set up is required...

  14. X-ray filter for x-ray powder diffraction

    Science.gov (United States)

    Sinsheimer, John Jay; Conley, Raymond P.; Bouet, Nathalie C. D.; Dooryhee, Eric; Ghose, Sanjit

    2018-01-23

    Technologies are described for apparatus, methods and systems effective for filtering. The filters may comprise a first plate. The first plate may include an x-ray absorbing material and walls defining first slits. The first slits may include arc shaped openings through the first plate. The walls of the first plate may be configured to absorb at least some of first x-rays when the first x-rays are incident on the x-ray absorbing material, and to output second x-rays. The filters may comprise a second plate spaced from the first plate. The second plate may include the x-ray absorbing material and walls defining second slits. The second slits may include arc shaped openings through the second plate. The walls of the second plate may be configured to absorb at least some of second x-rays and to output third x-rays.

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

    Energy Technology Data Exchange (ETDEWEB)

    Weekes, H.E. [Department of Materials, Royal School of Mines, Imperial College London, Prince Consort Road, London SW7 2BP (United Kingdom); Jones, N.G. [Department of Materials Science and Metallurgy, University of Cambridge, 27 Charles Babbage Road, Cambridge CB3 0FS (United Kingdom); Lindley, T.C. [Department of Materials, Royal School of Mines, Imperial College London, Prince Consort Road, London SW7 2BP (United Kingdom); Dye, D., E-mail: david.dye@imperial.ac.uk [Department of Materials, Royal School of Mines, Imperial College London, Prince Consort Road, London SW7 2BP (United Kingdom)

    2016-09-15

    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 (TSS{sub D,H}) and precipitation (TSS{sub P,H}).

  16. Novel X-ray telescopes for wide-field X-ray monitoring

    International Nuclear Information System (INIS)

    Hudec, R.; Inneman, A.; Pina, L.; Sveda, L.

    2005-01-01

    We report on fully innovative very wide-field of view X-ray telescopes with high sensitivity as well as large field of view. The prototypes are very promising, allowing the proposals for space projects with very wide-field Lobster-eye X-ray optics to be considered. The novel telescopes will monitor the sky with unprecedented sensitivity and angular resolution of order of 1 arcmin. They are expected to contribute essentially to study and to understand various astrophysical objects such as AGN, SNe, Gamma-ray bursts (GRBs), X-ray flashes (XRFs), galactic binary sources, stars, CVs, X-ray novae, various transient sources, etc. The Lobster optics based X-ray All Sky Monitor is capable to detect around 20 GRBs and 8 XRFs yearly and this will surely significantly contribute to the related science

  17. Optical studies of massive X-ray binaries

    International Nuclear Information System (INIS)

    Zuiderwijk, E.J.

    1979-01-01

    Photometric and spectroscopic studies of several optical counterparts of massive X-ray binaries are presented. Subjects of study were the binary systems:HD77581/4U0900-40 (Vela X-1), HD153919/4U1700-37, Wray 977/4U1223-62 and Sk160/4U0115-74 (=SMC X-1). (Auth.)

  18. X-ray fluorescence imaging with polycapillary X-ray optics

    International Nuclear Information System (INIS)

    Yonehara, Tasuku; Yamaguchi, Makoto; Tsuji, Kouichi

    2010-01-01

    X-ray fluorescence spectrometry imaging is a powerful tool to provide information about the chemical composition and elemental distribution of a specimen. X-ray fluorescence spectrometry images were conventionally obtained by using a μ-X-ray fluorescence spectrometry spectrometer, which requires scanning a sample. Faster X-ray fluorescence spectrometry imaging would be achieved by eliminating the process of sample scanning. Thus, we developed an X-ray fluorescence spectrometry imaging instrument without sample scanning by using polycapillary X-ray optics, which had energy filter characteristics caused by the energy dependence of the total reflection phenomenon. In the present paper, we show that two independent straight polycapillary X-ray optics could be used as an energy filter of X-rays for X-ray fluorescence. Only low energy X-rays were detected when the angle between the two optical axes was increased slightly. Energy-selective X-ray fluorescence spectrometry images with projection mode were taken by using an X-ray CCD camera equipped with two polycapillary optics. It was shown that Fe Kα (6.40 keV) and Cu Kα (8.04 keV) could be discriminated for Fe and Cu foils.

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

    International Nuclear Information System (INIS)

    Dimasi, E.; Gower, L.B.

    2000-01-01

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

  20. Dehydrogenation kinetics of pure and nickel-doped magnesium hydride investigated by in situ time-resolved powder X-ray diffraction

    DEFF Research Database (Denmark)

    Jensen, T.R.; Andreasen, A.; Vegge, Tejs

    2006-01-01

    The dehydrogenation kinetics of pure and nickel (Ni)-doped (2w/w%) magnesium hydride (MgH2) have been investigated by in situ time-resolved powder X-ray diffraction (PXD). Deactivated samples, i.e. air exposed, are investigated in order to focus on the effect of magnesium oxide (MgO) surface layers......, which might be unavoidable for magnesium (Mg)-based storage media for mobile applications. A curved position-sensitive detector covering 120 degrees in 20 and a rotating anode X-ray source provide a time resolution of 45 s and up to 90 powder pattems collected during an experiment under isothermal...... by the Johnson-Mehi-Avrami formalism in order to derive rate constants at different temperatures. The apparent activation energies for dehydrogenation of pure and Ni-doped magnesium hydride were E-A approximate to 300 and 250 kJ/mol, respectively. Differential scanning calorimetry gave, E-A = 270 k...

  1. X-ray diffraction study of lithium hydrazinium sulfate and lithium ammonium sulfate crystals under a static electric field

    International Nuclear Information System (INIS)

    Sebastian, M.T.; Becker, R.A.; Klapper, H.

    1991-01-01

    X-ray diffraction studies are made on proton-conducting polar lithium hydrazinium sulfate and ferroelectric lithium ammonium sulfate. The X-ray rocking curves recorded with in situ electric field along the polar b axis of lithium hydrazinium sulfate (direction of proton conductivity) show a strong enhancement of the 0k0 diffraction intensity. The corresponding 0k0 X-ray topographs reveal extinction contrast consisting of striations parallel to the polar axis. They disappear when the electric field is switched off. The effect is very strong in 0k0 but invisible in h0l reflections. It is present only if the electric field is parallel to the polar axis b. This unusual X-ray topographic contrast is correlated with the proton conduction. It is supposed that, under electric field, an inhomogeneous charge distribution develops, distorting the crystal lattice. Similar experiments on lithium ammonium sulfate also show contrast variations, but of quite different behaviour than before. In this case they result from changes of the ferroelectric domain configuration under electric field. (orig.)

  2. An in-situ X-ray absorption spectroelectrochemical study of the electroreduction of uranium ions in HCl, HNO{sub 3}, and Na{sub 2}CO{sub 3} solutions

    Energy Technology Data Exchange (ETDEWEB)

    Uehara, Akihiro; Fujii, Toshiyuki; Yamana, Hajimu [Kyoto Univ., Osaka (Japan). Div. of Nuclear Engineering Science; Okamoto, Yoshihiro [Japan Atomic Energy Agency, Ibaraki (Japan). Quantum Beam Science Directorate

    2016-04-01

    A spectroelectrochemical cell was fabricated for in-situ X-ray absorption spectroscopy (in-situ XAS). The XAS spectra of the uranium L{sub III} edge were monitored in electrolyte solutions during the electrochemical reduction. Tetravalent uranium, U{sup 4+}, in 1 mol dm{sup -3} (M) hydrochloric acid (HCl) was electrochemically prepared from hexavalent uranium, UO{sub 2}{sup 2+}, by constant current electrolysis, and the extended X-ray absorption fine structure (EXAFS) was analyzed. The concentration ratio of UO{sub 2}{sup 2+} and U{sup 4+}, which were formed via the disproportionation of pentavalent uranium, UO{sub 2}{sup +}, during the electrolysis, were calculated based on the intensity of the signal for the two axial oxygen atoms in the linear UO{sub 2}{sup 2+} unit, the U-O{sub ax}, bond that had a radial structural function. The apparent redox potential of the UO{sub 2}{sup 2+}/U{sup 4+} couple in 1 M HCl was determined based on the Nernst equation using the concentrations of UO{sub 2}{sup 2+} and U{sup 4+}. The electrode potential was shown to be close to the formal potential of the UO{sub 2}{sup 2+}/UO{sub 2}{sup +} couple as reported previously. This result indicates that the UO{sub 2}{sup +} that was formed electrochemically at the electrode disproportionated to form UO{sub 2}{sup 2+} and U{sup 4+} in the bulk solution. The in-situ XAS of UO{sub 2}{sup 2+} in 0.1 M nitric acid was also performed. The U{sup 4+} that formed was partially re-oxidized to UO{sub 2}{sup 2+} by the NO{sub 3}{sup -} present in the solution. The formation of the UO{sub 2}{sup +} carbonato complex was observed by in-situ XAS in a 1 M sodium carbonate solution during the bulk electrolysis. The edge jump of the X-ray absorption near edge structure (XANES) spectrum shifted from 17.164 to 17.163 keV, and the bond distances of U-O{sub ax} and U-O for CO{sub 3}{sup 2-} increased from 1.78 to 1.88 Aa and from 2.42 to 2.53 Aa, respectively, because of the reduction of the UO{sub 2}{sup 2

  3. X-ray studies of microstructures in semiconductors and superconducting materials

    International Nuclear Information System (INIS)

    Kao, Y.H.

    1991-01-01

    Several different experimental investigations were carried out during the present report period. These include x-ray studies of semiconductors, high-T c superconductors, and various thin films using synchrotron radiation (especially soft x-ray experiments by means of our new detector) and measurements of some fundamental properties of new superconducting materials made in our laboratory at Buffalo. We have made the first systematic study of electronic structure in the high-T c superconductors La 2-x Sr x CuO 4 with x ranging from 0 to 0.15 by x-ray absorption spectroscopy (XAS)

  4. M. I. T. studies of transient X-ray phenomena

    Energy Technology Data Exchange (ETDEWEB)

    Canizares, C R [Massachusetts Inst. of Tech., Cambridge (USA). Dept. of Physics

    1976-06-01

    A variety of transient X-ray phenomena have been studied by the M.I.T. X-ray Astronomy Group. Data from the OSO-7 satellite reveal both long and short time-scale transients. Extensive observations have been made of the Lupus X-ray Nova (3U1543-47) and of GX339-4 (MX1658-48) which may represent a very different type of transient source. A unique, intense X-ray flare lasting ten minutes was also recorded, and the X-ray emission from the active galaxy Cen A was found to vary significantly over a period of several days. In a recent balloon flight the Crab pulsar, NP0532, was observed to exhibit a transient pulsed component distinct from the usual main pulse and interpulse. A sounding-rocket experiment detected an ultrasoft transient X-ray source tentatively associated with SS Cygni, and preliminary results from SAS-3 show a very hard spectrum for the new source A0535+26. On the other hand, extensive OSO-7 null observations of both Type I and II supernovae and of the flaring radio star Algol make it unlikely that these types of objects are potent transient X-ray emitters.

  5. In-Situ Synchrotron Radiation Study of Formation and Growth of Crystalline CexZr1-xO2 Nanoparticles Synthesized in Supercritical Water

    DEFF Research Database (Denmark)

    Tyrsted, Christoffer; Becker-Christensen, Jacob; Hald, Peter

    2010-01-01

    -zirconia system, the growth of ceria and zirconia nanoparticles is fundamentally different under supercritical water conditions. For comparison, ex situ synthesis has also been performed using an in-house supercritical flow reactor. The resulting samples were analyzed using PXRD, small-angle X-ray scattering......In situ synchrotron powder X-ray diffraction (PXRD) measurements have been conducted to follow the nucleation and growth of crystalline CexZr1-xO2 nanoparticles synthesized in supercritical water with a full substitution variation (x = 0, 0.2, 0.5, 0.8, and 1.0). Direction-dependent growth curves...... are determined and described using reaction kinetic models. A distinct change in growth kinetics is observed with increasing cerium content. For x = 0.8 and 1.0 (high cerium content), the growth is initially limited by the surface reaction kinetics; however, at a size of ∼6 nm, the growth changes and becomes...

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

    Science.gov (United States)

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

    2016-11-01

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

  7. X-ray holography: X-ray interactions and their effects

    International Nuclear Information System (INIS)

    London, R.A.; Trebes, J.E.; Rosen, M.D.

    1988-01-01

    The authors summarize a theoretical study of the interactions of x-rays with a biological sample during the creation of a hologram. The choice of an optimal wavelength for x-ray holography is discussed, based on a description of scattering by objects within an aqueous environment. The problem of the motion resulting from the absorption of x-rays during a short exposure is described. The possibility of using very short exposures in order to capture the image before motion can compromise the resolution is explored. The impact of these calculation on the question of the feasibility of using an x-ray laser for holography of biological structures is discussed. 12 refs., 2 figs

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

    Science.gov (United States)

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

    2018-05-01

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

  9. In-situ Raman and X-ray photoelectron spectroscopic studies on the pitting corrosion of modified 9Cr-1Mo steel in neutral chloride solution

    Science.gov (United States)

    Ramya, S.; Nanda Gopala Krishna, D.; Mudali, U. Kamachi

    2018-01-01

    In-situ Raman and X-ray photoelectron spectroscopic studies were performed for the identification of native and corroded surface oxide layers of modified 9Cr-1Mo steel. The Raman data obtained for native oxide layer of modified 9Cr-1Mo steel revealed that it was mainly composed of oxides of Fe and Cr. The presence of alloying element Mo was found to be less significant in the native oxide film. The oxides of Cr were dominant at the surface and were found to be decreasing closer to metal/oxide layer interface. The changes in the chemical composition of the native films upon in-situ pitting during potentiostatic polarization experiment were characterized by in-situ Raman analysis. The corrosion products of potentiostatically polarized modified 9Cr-1Mo steel was composed of dominant Fe (III) phases viz., γ- Fe2O3, α and γ - FeOOH along with the oxides of chromium. The results from Raman analysis were corroborated with the XPS experiments on as received and pitted samples of modified 9Cr-1Mo steel specimens. It was observed that the oxides of Cr and Mo contributed for the stability of the surface layer by forming Cr2O3 and MoO3. Also, the study attempted to find out the intermediate corrosion products inside the metastable pits to account for the pseudo passive behavior of modified 9Cr-1Mo steel in 0.1 M NaCl solution.

  10. Synchrotron x-ray diffraction study of liquid surfaces

    DEFF Research Database (Denmark)

    Als-Nielsen, Jens Aage; Pershan, P.S.

    1983-01-01

    A spectrometer for X-ray diffraction and refraction studies of horizontal, free surfaces of liquids is described. As an illustration smetic-A layering at the surface of a liquid crystal is presented.......A spectrometer for X-ray diffraction and refraction studies of horizontal, free surfaces of liquids is described. As an illustration smetic-A layering at the surface of a liquid crystal is presented....

  11. Multiscale 3D characterization with dark-field x-ray microscopy

    DEFF Research Database (Denmark)

    Simons, Hugh; Jakobsen, Anders Clemen; Ahl, Sonja Rosenlund

    2016-01-01

    Dark-field x-ray microscopy is a new way to three-dimensionally map lattice strain and orientation in crystalline matter. It is analogous to dark-field electron microscopy in that an objective lens magnifies diffracting features of the sample; however, the use of high-energy synchrotron x-rays me......, multiscale phenomena in situ is a key step toward formulating and validating multiscale models that account for the entire heterogeneity of materials....

  12. X-Ray Absorption with Transmission X-Ray Microscopes

    NARCIS (Netherlands)

    de Groot, F.M.F.

    2016-01-01

    In this section we focus on the use of transmission X-ray microscopy (TXM) to measure the XAS spectra. In the last decade a range of soft X-ray and hard X-ray TXM microscopes have been developed, allowing the measurement of XAS spectra with 10–100 nm resolution. In the hard X-ray range the TXM

  13. Nonlocal heat transport and improved target design for x-ray heating studies at x-ray free electron lasers

    Science.gov (United States)

    Hoidn, Oliver; Seidler, Gerald T.

    2018-01-01

    The extremely high-power densities and short durations of single pulses of x-ray free electron lasers (XFELs) have opened new opportunities in atomic physics, where complex excitation-relaxation chains allow for high ionization states in atomic and molecular systems, and in dense plasma physics, where XFEL heating of solid-density targets can create unique dense states of matter having temperatures on the order of the Fermi energy. We focus here on the latter phenomena, with special emphasis on the problem of optimum target design to achieve high x-ray heating into the warm dense matter (WDM) state. We report fully three-dimensional simulations of the incident x-ray pulse and the resulting multielectron relaxation cascade to model the spatial energy density deposition in multicomponent targets, with particular focus on the effects of nonlocal heat transport due to the motion of high energy photoelectrons and Auger electrons. We find that nanoscale high-Z /low-Z multicomponent targets can give much improved energy density deposition in lower-Z materials, with enhancements reaching a factor of 100. This has three important benefits. First, it greatly enlarges the thermodynamic parameter space in XFEL x-ray heating studies of lower-Z materials. Second, it allows the use of higher probe photon energies, enabling higher-information content x-ray diffraction (XRD) measurements such as in two-color XFEL operations. Third, while this is merely one step toward optimization of x-ray heating target design, the demonstration of the importance of nonlocal heat transport establishes important common ground between XFEL-based x-ray heating studies and more traditional laser plasma methods.

  14. Dark field X-ray microscopy for studies of recrystallization

    DEFF Research Database (Denmark)

    Ahl, Sonja Rosenlund; Simons, Hugh; Jakobsen, Anders Clemen

    2015-01-01

    We present the recently developed technique of Dark Field X-Ray Microscopy that utilizes the diffraction of hard X-rays from individual grains or subgrains at the (sub)micrometre- scale embedded within mm-sized samples. By magnifying the diffracted signal, 3D mapping of orientations and strains...... external influences. The capabilities of Dark Field X- Ray Microscopy are illustrated by examples from an ongoing study of recrystallization of 50% cold-rolled Al1050 specimens....

  15. X-ray diffraction studies of NbTe 2 single crystal

    Indian Academy of Sciences (India)

    The composition of the grown crystals was confirmed on the basis of energy dispersive analysis by X-ray (EDAX) and remaining structural characterization was also accomplished by X-ray diffraction (XRD) studies. Lattice parameters, volume and X-ray density have been carried out for the grown crystals. The particle size ...

  16. X rays and condensed matter

    International Nuclear Information System (INIS)

    Daillant, J.

    1997-01-01

    After a historical review of the discovery and study of X rays, the various interaction processes between X rays and matter are described: Thomson scattering, Compton scattering, X-photon absorption through photoelectric effect, and magnetic scattering. X ray sources such as the European Synchrotron Radiation Facility (ESRF) are described. The various X-ray applications are presented: imagery such as X tomography, X microscopy, phase contrast; X-ray photoelectron spectroscopy and X-ray absorption spectroscopy; X-ray scattering and diffraction techniques

  17. Pseudocapacitance of MnO{sub 2} originates from reversible insertion/desertion of thiocyanate anions studied using in situ X-ray absorption spectroscopy in ionic liquid electrolyte

    Energy Technology Data Exchange (ETDEWEB)

    Lee, Ming-Tsung; Tsai, Wen-Ta; Chang, Jeng-Kuei [Department of Materials Science and Engineering, National Cheng Kung University, 1 University Road, Tainan (China); Deng, Ming-Jay; Cheng, Hui-Fang; Sun, I-Wen [Department of Chemistry, National Cheng Kung University, 1 University Road, Tainan (China)

    2010-02-01

    Charge storage mechanisms of electrodeposited MnO{sub 2} in various aprotic ionic liquids (ILs) are studied using in situ X-ray absorption spectroscopy (XAS). The analytical results show that a unique thiocyanate (SCN{sup -}) anion can reversibly insert/desert into/from the tunnels between the [MnO{sub 6}] octahedral subunits depending on the applied potential. This process charge compensates the Mn{sup 3+}/Mn{sup 4+} redox transition upon charging-discharging and thus contributes to an ideal pseudocapacitive behavior of the MnO{sub 2} electrode. The present work would open up a route for developing a novel oxide-based supercapacitor, with high cell-voltage, high thermal stability, and high safety, incorporating IL electrolytes. (author)

  18. X pinch a point x-ray source

    International Nuclear Information System (INIS)

    Garg, A.B.; Rout, R.K.; Shyam, A.; Srinivasan, M.

    1993-01-01

    X ray emission from an X pinch, a point x-ray source has been studied using a pin-hole camera by a 30 kV, 7.2 μ F capacitor bank. The wires of different material like W, Mo, Cu, S.S.(stainless steel) and Ti were used. Molybdenum pinch gives the most intense x-rays and stainless steel gives the minimum intensity x-rays for same bank energy (∼ 3.2 kJ). Point x-ray source of size (≤ 0.5 mm) was observed using pin hole camera. The size of the source is limited by the size of the pin hole camera. The peak current in the load is approximately 150 kA. The point x-ray source could be useful in many fields like micro lithography, medicine and to study the basic physics of high Z plasmas. (author). 4 refs., 3 figs

  19. Look fast: Crystallization of conjugated molecules during solution shearing probed in-situ and in real time by X-ray scattering

    KAUST Repository

    Smilgies, Detlef Matthias

    2012-12-20

    High-speed solution shearing, in which a drop of dissolved material is spread by a coating knife onto the substrate, has emerged as a versatile, yet simple coating technique to prepare high-mobility organic thin film transistors. Solution shearing and subsequent drying and crystallization of a thin film of conjugated molecules is probed in situ using microbeam grazing incidence wide-angle X-ray scattering (μGIWAXS). We demonstrate the advantages of this approach to study solution based crystal nucleation and growth, and identify casting parameter combinations to cast highly ordered and laterally aligned molecular thin films. Copyright © 2013 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  20. Look fast: Crystallization of conjugated molecules during solution shearing probed in-situ and in real time by X-ray scattering

    KAUST Repository

    Smilgies, Detlef Matthias; Li, Ruipeng; Giri, Gaurav; Chou, Kang Wei; Diao, Ying; Bao, Zhenan; Amassian, Aram

    2012-01-01

    High-speed solution shearing, in which a drop of dissolved material is spread by a coating knife onto the substrate, has emerged as a versatile, yet simple coating technique to prepare high-mobility organic thin film transistors. Solution shearing and subsequent drying and crystallization of a thin film of conjugated molecules is probed in situ using microbeam grazing incidence wide-angle X-ray scattering (μGIWAXS). We demonstrate the advantages of this approach to study solution based crystal nucleation and growth, and identify casting parameter combinations to cast highly ordered and laterally aligned molecular thin films. Copyright © 2013 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  1. Tokamak physics studies using x-ray diagnostic methods

    International Nuclear Information System (INIS)

    Hill, K.W.; Bitter, M.; von Goeler, S.

    1987-03-01

    X-ray diagnostic measurements have been used in a number of experiments to improve our understanding of important tokamak physics issues. The impurity content in TFTR plasmas, its sources and control have been clarified through soft x-ray pulse-height analysis (PHA) measurements. The dependence of intrinsic impurity concentrations and Z/sub eff/ on electron density, plasma current, limiter material and conditioning, and neutral-beam power have shown that the limiter is an important source of metal impurities. Neoclassical-like impurity peaking following hydrogen pellet injection into Alcator C and a strong effect of impurities on sawtooth behavior were demonstrated by x-ray imaging (XIS) measurements. Rapid inward motion of impurities and continuation of m = 1 activity following an internal disruption were demonstrated with XIS measurements on PLT using injected aluminum to enhance the signals. Ion temperatures up to 12 keV and a toroidal plasma rotation velocity up to 6 x 10 5 m/s have been measured by an x-ray crystal spectrometer (XCS) with up to 13 MW of 85-keV neutral-beam injection in TFTR. Precise wavelengths and relative intensities of x-ray lines in several helium-like ions and neon-like ions of silver have been measured in TFTR and PLT by the XCS. The data help to identify the important excitation processes predicted in atomic physics. Wavelengths of n = 3 to 2 silver lines of interest for x-ray lasers were measured, and precise instrument calibration techniques were developed. Electron thermal conductivity and sawtooth dynamics have been studied through XIS measurements on TFTR of heat-pulse propagation and compound sawteeth. A non-Maxwellian electron distribution function has been measured, and evidence of the Parail-Pogutse instability identified by hard x-ray PHA measurements on PLT during lower-hybrid current-drive experiments

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

    Energy Technology Data Exchange (ETDEWEB)

    Sun Haohua; Kou Bingquan; Xi Yan; Qi Juncheng; Sun Jianqi; Mohr, Juergen; Boerner, Martin; Zhao Jun; Xu, Lisa X.; Xiao Tiqiao; Wang Yujie [Department of Physics, Shanghai Jiao Tong University, Shanghai 200240 (China); School of Biomedical Engineering, Shanghai Jiao Tong University, Shanghai 200240 (China) and Med-X Research Institute, Shanghai Jiao Tong University, Shanghai 200040 (China); Shanghai Institute of Applied Physics, Chinese Academy of Sciences, Shanghai 201800 (China); Karlsruhe Institute of Technology (KIT), Institute for Microstructure Technology (IMT), Hermannvon-Helmholtz-Platz 1, 76344 Eggenstein-Leopoldshafen (Germany)

    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.

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

    International Nuclear Information System (INIS)

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

    2012-01-01

    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.

  4. Crystal defect studies using x-ray diffuse scattering

    Energy Technology Data Exchange (ETDEWEB)

    Larson, B.C.

    1980-01-01

    Microscopic lattice defects such as point (single atom) defects, dislocation loops, and solute precipitates are characterized by local electronic density changes at the defect sites and by distortions of the lattice structure surrounding the defects. The effect of these interruptions of the crystal lattice on the scattering of x-rays is considered in this paper, and examples are presented of the use of the diffuse scattering to study the defects. X-ray studies of self-interstitials in electron irradiated aluminum and copper are discussed in terms of the identification of the interstitial configuration. Methods for detecting the onset of point defect aggregation into dislocation loops are considered and new techniques for the determination of separate size distributions for vacancy loops and interstitial loops are presented. Direct comparisons of dislocation loop measurements by x-rays with existing electron microscopy studies of dislocation loops indicate agreement for larger size loops, but x-ray measurements report higher concentrations in the smaller loop range. Methods for distinguishing between loops and three-dimensional precipitates are discussed and possibilities for detailed studies considered. A comparison of dislocation loop size distributions obtained from integral diffuse scattering measurements with those from TEM show a discrepancy in the smaller sizes similar to that described above.

  5. Crystal defect studies using x-ray diffuse scattering

    International Nuclear Information System (INIS)

    Larson, B.C.

    1980-01-01

    Microscopic lattice defects such as point (single atom) defects, dislocation loops, and solute precipitates are characterized by local electronic density changes at the defect sites and by distortions of the lattice structure surrounding the defects. The effect of these interruptions of the crystal lattice on the scattering of x-rays is considered in this paper, and examples are presented of the use of the diffuse scattering to study the defects. X-ray studies of self-interstitials in electron irradiated aluminum and copper are discussed in terms of the identification of the interstitial configuration. Methods for detecting the onset of point defect aggregation into dislocation loops are considered and new techniques for the determination of separate size distributions for vacancy loops and interstitial loops are presented. Direct comparisons of dislocation loop measurements by x-rays with existing electron microscopy studies of dislocation loops indicate agreement for larger size loops, but x-ray measurements report higher concentrations in the smaller loop range. Methods for distinguishing between loops and three-dimensional precipitates are discussed and possibilities for detailed studies considered. A comparison of dislocation loop size distributions obtained from integral diffuse scattering measurements with those from TEM show a discrepancy in the smaller sizes similar to that described above

  6. A reaction cell with sample laser heating for in situ soft X-ray absorption spectroscopy studies under environmental conditions.

    Science.gov (United States)

    Escudero, Carlos; Jiang, Peng; Pach, Elzbieta; Borondics, Ferenc; West, Mark W; Tuxen, Anders; Chintapalli, Mahati; Carenco, Sophie; Guo, Jinghua; Salmeron, Miquel

    2013-05-01

    A miniature (1 ml volume) reaction cell with transparent X-ray windows and laser heating of the sample has been designed to conduct X-ray absorption spectroscopy studies of materials in the presence of gases at atmospheric pressures. Heating by laser solves the problems associated with the presence of reactive gases interacting with hot filaments used in resistive heating methods. It also facilitates collection of a small total electron yield signal by eliminating interference with heating current leakage and ground loops. The excellent operation of the cell is demonstrated with examples of CO and H2 Fischer-Tropsch reactions on Co nanoparticles.

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

    International Nuclear Information System (INIS)

    Tamura, Nobumichi; Chen, Kai; Kunz, Martin

    2009-01-01

    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.

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

    Energy Technology Data Exchange (ETDEWEB)

    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.

  9. Modeling the X-ray Process, and X-ray Flaw Size Parameter for POD Studies

    Science.gov (United States)

    Koshti, Ajay M.

    2014-01-01

    Nondestructive evaluation (NDE) method reliability can be determined by a statistical flaw detection study called probability of detection (POD) study. In many instances, the NDE flaw detectability is given as a flaw size such as crack length. The flaw is either a crack or behaving like a crack in terms of affecting the structural integrity of the material. An alternate approach is to use a more complex flaw size parameter. The X-ray flaw size parameter, given here, takes into account many setup and geometric factors. The flaw size parameter relates to X-ray image contrast and is intended to have a monotonic correlation with the POD. Some factors such as set-up parameters, including X-ray energy, exposure, detector sensitivity, and material type that are not accounted for in the flaw size parameter may be accounted for in the technique calibration and controlled to meet certain quality requirements. The proposed flaw size parameter and the computer application described here give an alternate approach to conduct the POD studies. Results of the POD study can be applied to reliably detect small flaws through better assessment of effect of interaction between various geometric parameters on the flaw detectability. Moreover, a contrast simulation algorithm for a simple part-source-detector geometry using calibration data is also provided for the POD estimation.

  10. Support Effects in Catalysis Studied by in-situ Sum Frequency Generation Vibrational Spectroscopy and in-situ X-Ray Spectroscopies

    Science.gov (United States)

    Kennedy, Griffin John

    which the molecule binds via the aldehyde group. These sites are believed to be the active sites for alcohol production. In the case of Co3O 4 ambient pressure x-ray photoelectron spectroscopy and x-ray absorption spectroscopy reveal a reduction of the oxide surface under reaction conditions indicating the adsorption sites on the oxide exist on a reduced surface, additional evidence for the site being an O-vacancy. Lastly a before undiscovered example of encapsulation of a metal particle by an oxide support is observed for the Pt/Co3O4 system by ambient pressure x-ray photoelectron spectroscopy. Under mild conditions an encapsulated state is reached in which the oxide covers the Pt surface, yet does not inhibit reactivity. In fact the total activity of the catalyst increases dramatically and a change in product selectivity was observed. (Abstract shortened by ProQuest.).

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

    Energy Technology Data Exchange (ETDEWEB)

    Koval’chuk, M. V.; Yatsishina, E. B.; Blagov, A. E.; Tereshchenko, E. Yu., E-mail: elenatereschenko@yandex.ru; Prosekov, P. A.; Dyakova, Yu. A. [National Research Centre “Kurchatov Institute” (Russian Federation)

    2016-09-15

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

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

    International Nuclear Information System (INIS)

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

    2016-01-01

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

  13. On revealing the vertical structure of nanoparticle films with elemental resolution: A total external reflection X-ray standing waves study

    Energy Technology Data Exchange (ETDEWEB)

    Zargham, Ardalan, E-mail: zargham@ifp.uni-bremen.d [Institute of Solid State Physics, University of Bremen, Otto-Hahn-Allee 1, 28359 Bremen (Germany); Schmidt, Thomas; Flege, Jan Ingo; Sauerbrey, Marc; Hildebrand, Radowan [Institute of Solid State Physics, University of Bremen, Otto-Hahn-Allee 1, 28359 Bremen (Germany); Roehe, Sarah; Baeumer, Marcus [Applied and Physical Chemistry, University of Bremen, Leobener Str. 2, 28359, Bremen (Germany); Falta, Jens [Institute of Solid State Physics, University of Bremen, Otto-Hahn-Allee 1, 28359 Bremen (Germany)

    2010-02-15

    We present a promising combination of methods to precisely determine the morphology of nanostructures, drawing on the example of monodisperse CoPt{sub 3} nanoparticle films deposited by spin coating and dip coating techniques on functionalized Au substrates. Ex-situ X-ray standing waves in total external reflection combined with X-ray reflectivity measurements were employed to determine element-specific atomic-density distributions in vertical direction.

  14. High-energy x-ray scattering studies of battery materials

    International Nuclear Information System (INIS)

    Glazer, Matthew P. B.; Okasinski, John S.; Almer, Jonathan D.; Ren, Yang

    2016-01-01

    High-energy x-ray (HEX) scattering is a sensitive and powerful tool to nondestructively probe the atomic and mesoscale structures of battery materials under synthesis and operational conditions. The penetration power of HEXs enables the use of large, practical samples and realistic environments, allowing researchers to explore the inner workings of batteries in both laboratory and commercial formats. This article highlights the capability and versatility of HEX techniques, particularly from synchrotron sources, to elucidate materials synthesis processes and thermal instability mechanisms in situ, to understand (dis)charging mechanisms in operando under a variety of cycling conditions, and to spatially resolve electrode/electrolyte responses to highlight connections between inhomogeneity and performance. Such studies have increased our understanding of the fundamental mechanisms underlying battery performance. Here, by deepening our understanding of the linkages between microstructure and overall performance, HEXs represent a powerful tool for validating existing batteries and shortening battery-development timelines.

  15. Simulation study on unfolding methods for diagnostic X-rays and mixed gamma rays

    International Nuclear Information System (INIS)

    Hashimoto, Makoto; Ohtaka, Masahiko; Ara, Kuniaki; Kanno, Ikuo; Imamura, Ryo; Mikami, Kenta; Nomiya, Seiichiro; Onabe, Hideaki

    2009-01-01

    A photon detector operating in current mode that can sense X-ray energy distribution has been reported. This detector consists of a row of several segment detectors. The energy distribution is derived using an unfolding technique. In this paper, comparisons of the unfolding techniques among error reduction, spectrum surveillance, and neural network methods are discussed through simulation studies on the detection of diagnostic X-rays and gamma rays emitted by a mixture of 137 Cs and 60 Co. For diagnostic X-ray measurement, the spectrum surveillance and neural network methods appeared promising, while the error reduction method yielded poor results. However, in the case of measuring mixtures of gamma rays, the error reduction method was both sufficient and effective. (author)

  16. X-ray microdiffraction study of Cu interconnects

    International Nuclear Information System (INIS)

    Zhang, X.; Solak, H.; Cerrina, F.; Lai, B.; Cai, Z.; Ilinski, P.; Legnini, D.; Rodrigues, W.

    2000-01-01

    We have used x-ray microdiffraction to study the local structure and strain variation of copper interconnects. Different types of local microstructures have been found in different samples. Our data show that the Ti adhesion layer has a very dramatic effect on Cu microstructure. Strain measurement was conducted before and after electromigration test, Cu fluorescence was used to find the mass variations around voids and hillocks, and x-ray microdiffraction was used to measure the strain change around that interested region. (c) 2000 American Institute of Physics

  17. Scanning of Adsorption Hysteresis In Situ with Small Angle X-Ray Scattering.

    Directory of Open Access Journals (Sweden)

    Athanasios Ch Mitropoulos

    Full Text Available Everett's theorem-6 of the domain theory was examined by conducting adsorption in situ with small angle x-ray scattering (SAXS supplemented by the contrast matching technique. The study focuses on the spectrum differences of a point to which the system arrives from different scanning paths. It is noted that according to this theorem at a common point the system has similar macroscopic properties. Furthermore it was examined the memory string of the system. We concluded that opposite to theorem-6: a at a common point the system can reach in a finite (not an infinite number of ways, b a correction for the thickness of the adsorbed film prior to capillary condensation is necessary, and c the scattering curves although at high-Q values coincide, at low-Q values are different indicating different microscopic states. That is, at a common point the system holds different metastable states sustained by hysteresis effects. These metastable states are the ones which highlight the way of a system back to a return point memory (RPM. Entering the hysteresis loop from different RPMs different histories are implanted to the paths toward the common point. Although in general the memory points refer to relaxation phenomena, they also constitute a characteristic feature of capillary condensation. Analogies of the no-passing rule and the adiabaticity assumption in the frame of adsorption hysteresis are discussed.

  18. Scanning of Adsorption Hysteresis In Situ with Small Angle X-Ray Scattering

    Science.gov (United States)

    Mitropoulos, Athanasios Ch.; Favvas, Evangelos P.; Stefanopoulos, Konstantinos L.; Vansant, Etienne F.

    2016-01-01

    Everett’s theorem-6 of the domain theory was examined by conducting adsorption in situ with small angle x-ray scattering (SAXS) supplemented by the contrast matching technique. The study focuses on the spectrum differences of a point to which the system arrives from different scanning paths. It is noted that according to this theorem at a common point the system has similar macroscopic properties. Furthermore it was examined the memory string of the system. We concluded that opposite to theorem-6: a) at a common point the system can reach in a finite (not an infinite) number of ways, b) a correction for the thickness of the adsorbed film prior to capillary condensation is necessary, and c) the scattering curves although at high-Q values coincide, at low-Q values are different indicating different microscopic states. That is, at a common point the system holds different metastable states sustained by hysteresis effects. These metastable states are the ones which highlight the way of a system back to a return point memory (RPM). Entering the hysteresis loop from different RPMs different histories are implanted to the paths toward the common point. Although in general the memory points refer to relaxation phenomena, they also constitute a characteristic feature of capillary condensation. Analogies of the no-passing rule and the adiabaticity assumption in the frame of adsorption hysteresis are discussed. PMID:27741263

  19. X-ray diffraction study of delta-stabilized plutonium alloys under pressure

    Energy Technology Data Exchange (ETDEWEB)

    Faure, Ph, E-mail: philippe.faure@cea.f [CEA, Valduc, F-21120 Is-sur-Tille (France); Genestier, C. [CEA, Valduc, F-21120 Is-sur-Tille (France)

    2010-02-15

    Previous extensive studies of the delta -> alpha'-phase transformation induced by temperature and/or by pressure in delta-stabilized plutonium alloys indicate strong dependence on parameters such as solute type, solute distribution, chemical impurities, kinetics, thermodynamic path.... The present paper reports results obtained on two Pu-2.3at.%Ga binary alloys differing by solute homogenization treatment and studied under pressure by in situ by X-ray diffraction in diamond anvil cells. The gamma'-phase appears as an intermediate phase during the delta -> alpha'-phase transformation. In cored samples, unexpanded alpha'-phase is formed at the beginning of the transformation, from domains with low solute content, and expanded alpha'-phase subsequently forms (from domains with higher solute content) as the transformation progresses with the pressure increase.

  20. In situ grazing incidence small-angle X-ray scattering investigation of polystyrene nanoparticle spray deposition onto silicon.

    Science.gov (United States)

    Herzog, Gerd; Benecke, Gunthard; Buffet, Adeline; Heidmann, Berit; Perlich, Jan; Risch, Johannes F H; Santoro, Gonzalo; Schwartzkopf, Matthias; Yu, Shun; Wurth, Wilfried; Roth, Stephan V

    2013-09-10

    We investigated the spray deposition and subsequent self-assembly during drying of a polystyrene nanoparticle dispersion with in situ grazing incidence small-angle X-ray scattering at high time resolution. During the fast deposition of the dispersion and the subsequent evaporation of the solvent, different transient stages of nanoparticle assembly can be identified. In the first stage, the solvent starts to evaporate without ordering of the nanoparticles. During the second stage, large-scale structures imposed by the breakup of the liquid film are observable. In this stage, the solvent evaporates further and nanoparticle ordering starts. In the late third drying stage, the nanoparticles self-assemble into the final layer structure.

  1. High-pressure X-ray diffraction studies of potassium chlorate

    Energy Technology Data Exchange (ETDEWEB)

    Pravica, Michael; Bai, Ligang; Bhattacharya, Neelanjan (UNLV)

    2012-03-15

    Two static high-pressure X-ray diffraction (XRD) studies of potassium chlorate have been performed at pressures of up to {approx}14.3 GPa in a diamond anvil cell at ambient temperature using the 16 ID-B undulator beamline at the Advanced Photon Source for the X-ray source. The first experiment was conducted to ascertain decomposition rates of potassium chlorate as a function of pressure. Below 2 GPa, the sample was observed to decompose rapidly in the presence of the X-ray beam and release oxygen. Above 2 GPa (near the phase I phase II transition), the decomposition rate dramatically slowed so that good quality XRD patterns could be acquired. This suggests a phase-dependent decomposition rate. In the second study, X-ray diffraction spectra were collected at pressures from 2 to 14.3 GPa by aligning virgin portions of the sample into the focused X-ray beam at each pressure. The results suggest the co-existence of mixed monoclinic (I) and rhombohedral (II) phases of potassium chlorate near 2 GPa. At pressures beyond 4 GPa, the XRD patterns show a very good fit to KClO{sub 3} in the rhombohedral phase with space group R3m, in agreement with earlier studies. No further phase transitions were observed with pressure. Decompression of the sample to ambient pressure indicated mixed phases I and II coupled with a small amount of synchrotron X-ray-induced decomposition product. The equation of state within this pressure regime has been determined.

  2. X-ray scattering studies of surfaces and interfaces

    International Nuclear Information System (INIS)

    Sanyal, M.K.

    1998-01-01

    Here we shall briefly review the basics and some applications of x-ray specular reflectivity and diffuse scattering techniques. These x-ray scattering techniques are uniquely suited to study of the structure of surfaces and interfaces at atomic resolutions as they are nondestructive and can probe even interfaces which are buried. The study of structure of surfaces and interfaces is not only required in understanding physics in reduced dimensions but is also essential in developing technologically important materials

  3. X-ray astronomy

    International Nuclear Information System (INIS)

    Giacconi, R.; Gursky, H.

    1974-01-01

    This text contains ten chapters and three appendices. Following an introduction, chapters two through five deal with observational techniques, mechanisms for the production of x rays in a cosmic setting, the x-ray sky and solar x-ray emission. Chapters six through ten include compact x-ray sources, supernova remnants, the interstellar medium, extragalactic x-ray sources and the cosmic x-ray background. Interactions of x rays with matter, units and conversion factors and a catalog of x-ray sources comprise the three appendices. (U.S.)

  4. X-ray investigation of Nb/O interfaces

    International Nuclear Information System (INIS)

    Delheusy, M.

    2008-01-01

    X-ray free electron lasers and the future International Linear Collider project are based on the performance of niobium superconducting RF cavities for efficient particle acceleration. A remarkable increase of the RF accelerating field is usually achieved by low-temperature annealing of the cavities (T≤150 C, several hours). The microscopic origin of this effect has remained unclear; however, it has been argued that a redistribution of subsurface interstitial oxygen into niobium is involved. In this study, the near surface structure of oxidized niobium single crystals and its evolution upon vacuum annealing has been studied by means of non-destructive in-situ surface sensitive x-ray techniques: x-ray reflectivity (XRR), grazing incidence x-ray diffraction (GIXD), diffuse scattering (GIDXS), crystal truncation rods measurements (CTRs), and high-resolution core-level spectroscopy (HRCLS). A first insight into the interplay between the oxide formation/dissolution and the occurrence of 181 subsurface interstitial oxygen has been given. The natural oxide on Nb(110) and Nb(100) surfaces is constituted of Nb 2 O 5 , NbO 2 and NbO, from the surface to the interface. It reduces progressively upon heating from Nb 2 O 5 to NbO 2 at low temperatures, and to NbO at 300 C. The Nb(110)/NbO(111) interface presents a Nishiyma-Wassermann epitaxial orientation relationship. The depth-distribution of interstitial oxygen has been established indicating that most of the oxygen is located in the direct vicinity of the oxide/niobium interface. No evidence of oxygen depletion below the oxide layer has been observed for the low temperature thermal treatments and surface preparations investigated in this study. (author) [fr

  5. X-ray investigation of Nb/O interfaces

    Energy Technology Data Exchange (ETDEWEB)

    Delheusy, Melissa

    2008-07-07

    X-ray free electron lasers and the future International Linear Collider project are based on the performance of niobium superconducting rf cavities for efficient particle acceleration. A remarkable increase of the rf accelerating field is usually achieved by low-temperature annealing of the cavities (T<150 C, several hours). The microscopic origin of this effect has remained unclear; however, it has been argued that a redistribution of subsurface interstitial oxygen into niobium is involved. In this study, the near surface structure of oxidized niobium single crystals and its evolution upon vacuum annealing has been studied by means of non-destructive in-situ surface sensitive X-ray techniques: X-ray reflectivity (XRR), grazing incidence X-ray diffraction (GIXD), diffuse scattering (GIDXS), crystal truncation rods measurements (CTRs), and high-resolution core-level spectroscopy (HRCLS). A first insight into the interplay between the oxide formation/dissolution and the occurrence of subsurface interstitial oxygen has been given. The natural oxide on Nb(110) and Nb(100) surfaces is constituted of Nb{sub 2}O{sub 5}, NbO{sub 2} and NbO, from the surface to the interface. It reduces progressively upon heating from Nb{sub 2}O{sub 5} to NbO{sub 2} at low temperatures, and to NbO at 300 C. The Nb(110)/NbO(111) interface presents a Nishiyama-Wassermann epitaxial orientation relationship. The depth-distribution of interstitial oxygen has been established indicating that most of the oxygen is located in the direct vicinity of the oxide/niobium interface. No evidence of oxygen depletion below the oxide layer has been observed for the low temperature thermal treatments and surface preparations investigated in this study. (orig.)

  6. Fatigue damage observed non-destructively in fibre composite coupon test specimens by X-ray CT

    DEFF Research Database (Denmark)

    Jespersen, Kristine Munk; Mikkelsen, Lars Pilgaard

    2016-01-01

    This study presents a method for monitoring the 3D fatigue damage progression on a micro-structural level in a glass fibre/polymer coupon test specimen by means of laboratory X-ray Computed Tomography (CT). A modified mount and holder made for the standard test samples to fit into the X-ray CT...... scanner along with a tension clamp solution is presented. Initially, the same location of the test specimen is inspected by ex-situ X-ray CT during the fatigue loading history, which shows the damage progression on a micro-structural level. The openings of individual uni-directional (UD) fibre fractures...

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

    International Nuclear Information System (INIS)

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

    2014-01-01

    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

  8. Effects of quartz particle size and water-to-solid ratio on hydrothermal synthesis of tobermorite studied by in-situ time-resolved X-ray diffraction

    International Nuclear Information System (INIS)

    Kikuma, J.; Tsunashima, M.; Ishikawa, T.; Matsuno, S.; Ogawa, A.; Matsui, K.; Sato, M.

    2011-01-01

    Hydrothermal synthesis process of tobermorite (5CaO.6SiO 2 .5H 2 O) has been investigated by in-situ X-ray diffraction using high-energy X-rays from a synchrotron radiation source in combination with a purpose-build autoclave cell. Dissolution rates of quartz were largely affected by its particle size distribution in the starting mixtures. However, the composition (Ca/Si) of non-crystalline C-S-H at the start of tobermorite formation was identical regardless of the quartz dissolution rate. An effect of water-to-solid ratio (w/s) was investigated for samples using fine particle quartz. Tobermorite did not occur with w/s of 1.7 but occurred with w/s higher than 3.0. Surprisingly, however, the dissolution curves of quartz were nearly identical for all samples with w/s from 1.7 to 9, indicating that the dissolution rate is predominated by surface area. Possible reaction mechanism for tobermorite formation will be discussed in terms of Ca and/or silicate ion concentration in the liquid phase and distribution of Ca/Si in non-crystalline C-S-H. - Graphical abstract: Time-resolved XRD data set was obtained at up to 190 deg. C under a saturated steam pressure. Tobermorite (5CaO.6SiO 2 .5H 2 O) formation reaction was investigated in detail for several different starting materials. Highlights: → Hydrothermal formation of tobermorite was monitored by in-situ XRD. → Ca/Si of C-S-H at the start time of tobermorite formation was determined. → The Ca/Si value was identical regardless of the quartz particle size in the starting mixture.

  9. High-Resolution X-ray Emission and X-ray Absorption Spectroscopy

    NARCIS (Netherlands)

    Groot, F.M.F. de

    2000-01-01

    In this review, high-resolution X-ray emission and X-ray absorption spectroscopy will be discussed. The focus is on the 3d transition-metal systems. To understand high-resolution X-ray emission and reso-nant X-ray emission, it is first necessary to spend some time discussing the X-ray absorption

  10. X-ray Diffraction Study of Molybdenum Diselenide to 35.9 GPa

    International Nuclear Information System (INIS)

    Aksoy, R.; Selvi, E.; Ma, Y.

    2008-01-01

    In situ high-pressure angle dispersive synchrotron X-ray diffraction studies of molybdenum diselenide (MoSe2) were carried out in a diamond-anvil cell to 35.9 GPa. No evidence of a phase transformation was observed in the pressure range. By fitting the pressure-volume data to the third-order Birch-Murnaghan equation of state, the bulk modulus, K0T, was determined to be 45.7±0.3 GPa with its pressure derivative, K'0T, being 11.6±0.1. It was found that the c-axis decreased linearly with pressure at a slope of -0.1593 when pressures were lower than 10 GPa. It showed different linear decrease with the slope of a -0.0236 at pressures higher than 10 GPa.

  11. Wide-area phase-contrast X-ray imaging using large X-ray interferometers

    Energy Technology Data Exchange (ETDEWEB)

    Momose, Atsushi E-mail: momose@exp.t.u-tokyo.ac.jp; Takeda, Tohoru; Yoneyama, Akio; Koyama, Ichiro; Itai, Yuji

    2001-07-21

    Large X-ray interferometers are developed for phase-contrast X-ray imaging aiming at medical applications. A monolithic X-ray interferometer and a separate one are studied, and currently a 25 mmx20 mm view area can be generated. This paper describes the strategy of our research program and some recent developments.

  12. Wide-area phase-contrast X-ray imaging using large X-ray interferometers

    Science.gov (United States)

    Momose, Atsushi; Takeda, Tohoru; Yoneyama, Akio; Koyama, Ichiro; Itai, Yuji

    2001-07-01

    Large X-ray interferometers are developed for phase-contrast X-ray imaging aiming at medical applications. A monolithic X-ray interferometer and a separate one are studied, and currently a 25 mm×20 mm view area can be generated. This paper describes the strategy of our research program and some recent developments.

  13. Flash X-ray

    International Nuclear Information System (INIS)

    Sato, Eiichi

    2003-01-01

    Generation of quasi-monochromatic X-ray by production of weakly ionized line plasma (flash X-ray), high-speed imaging by the X-ray and high-contrast imaging by the characteristic X-ray absorption are described. The equipment for the X-ray is consisted from the high-voltage power supply and condenser, turbo molecular pump, and plasma X-ray tube. The tube has a long linear anticathode to produce the line plasma and flash X-ray at 20 kA current at maximum. X-ray spectrum is measured by the imaging plate equipped in the computed radiography system after diffracted by a LiF single crystal bender. Cu anticathode generates sharp peaks of K X-ray series. The tissue images are presented for vertebra, rabbit ear and heart, and dog heart by X-ray fluoroscopy with Ce anticathode. Generation of K-orbit characteristic X-ray with extremely low bremsstrahung is to be attempted for medical use. (N.I.)

  14. Ultrashort X-ray pulse science

    Energy Technology Data Exchange (ETDEWEB)

    Chin, Alan Hap [Univ. of California, Berkeley, CA (US). Dept. of Physics; Lawrence Berkeley National Lab. (LBNL), Berkeley, CA (United States)

    1998-05-01

    A variety of phenomena involves atomic motion on the femtosecond time-scale. These phenomena have been studied using ultrashort optical pulses, which indirectly probe atomic positions through changes in optical properties. Because x-rays can more directly probe atomic positions, ultrashort x-ray pulses are better suited for the study of ultrafast structural dynamics. One approach towards generating ultrashort x-ray pulses is by 90° Thomson scattering between terawatt laser pulses and relativistic electrons. Using this technique, the author generated ~ 300 fs, 30 keV (0.4 Å) x-ray pulses. These x-ray pulses are absolutely synchronized with ultrashort laser pulses, allowing femtosecond optical pump/x-ray probe experiments to be performed. Using the right-angle Thomson scattering x-ray source, the author performed time-resolved x-ray diffraction studies of laser-perturbated InSb. These experiments revealed a delayed onset of lattice expansion. This delay is due to the energy relaxation from a dense electron-hole plasma to the lattice. The dense electron-hole plasma first undergoes Auger recombination, which reduces the carrier concentration while maintaining energy content. Longitudinal-optic (LO) phonon emission then couples energy to the lattice. LO phonon decay into acoustic phonons, and acoustic phonon propagation then causes the growth of a thermally expanded layer. Source characterization is instrumental in utilizing ultrashort x-ray pulses in time-resolved x-ray spectroscopies. By measurement of the electron beam diameter at the generation point, the pulse duration of the Thomson scattered x-rays is determined. Analysis of the Thomson scattered x-ray beam properties also provides a novel means of electron bunch characterization. Although the pulse duration is inferred for the Thomson scattering x-ray source, direct measurement is required for other x-ray pulse sources. A method based on the laser-assisted photoelectric effect (LAPE) has been demonstrated as a

  15. Ultrashort X-ray pulse science

    International Nuclear Information System (INIS)

    Chin, A.H.; Lawrence Berkeley National Lab., CA

    1998-01-01

    A variety of phenomena involves atomic motion on the femtosecond time-scale. These phenomena have been studied using ultrashort optical pulses, which indirectly probe atomic positions through changes in optical properties. Because x-rays can more directly probe atomic positions, ultrashort x-ray pulses are better suited for the study of ultrafast structural dynamics. One approach towards generating ultrashort x-ray pulses is by 90 o Thomson scattering between terawatt laser pulses and relativistic electrons. Using this technique, the author generated ∼ 300 fs, 30 keV (0.4 (angstrom)) x-ray pulses. These x-ray pulses are absolutely synchronized with ultrashort laser pulses, allowing femtosecond optical pump/x-ray probe experiments to be performed. Using the right-angle Thomson scattering x-ray source, the author performed time-resolved x-ray diffraction studies of laser-perturbated InSb. These experiments revealed a delayed onset of lattice expansion. This delay is due to the energy relaxation from a dense electron-hole plasma to the lattice. The dense electron-hole plasma first undergoes Auger recombination, which reduces the carrier concentration while maintaining energy content. Longitudinal-optic (LO) phonon emission then couples energy to the lattice. LO phonon decay into acoustic phonons, and acoustic phonon propagation then causes the growth of a thermally expanded layer. Source characterization is instrumental in utilizing ultrashort x-ray pulses in time-resolved x-ray spectroscopies. By measurement of the electron beam diameter at the generation point, the pulse duration of the Thomson scattered x-rays is determined. Analysis of the Thomson scattered x-ray beam properties also provides a novel means of electron bunch characterization. Although the pulse duration is inferred for the Thomson scattering x-ray source, direct measurement is required for other x-ray pulse sources. A method based on the laser-assisted photoelectric effect (LAPE) has been

  16. Study of x-ray CCD image sensor and application

    Science.gov (United States)

    Wang, Shuyun; Li, Tianze

    2008-12-01

    In this paper, we expounded the composing, specialty, parameter, its working process, key techniques and methods for charge coupled devices (CCD) twice value treatment. Disposal process for CCD video signal quantification was expatiated; X-ray image intensifier's constitutes, function of constitutes, coupling technique of X-ray image intensifier and CCD were analyzed. We analyzed two effective methods to reduce the harm to human beings when X-ray was used in the medical image. One was to reduce X-ray's radiation and adopt to intensify the image penetrated by X-ray to gain the same effect. The other was to use the image sensor to transfer the images to the safe area for observation. On this base, a new method was presented that CCD image sensor and X-ray image intensifier were combined organically. A practical medical X-ray photo electricity system was designed which can be used in the records and time of the human's penetrating images. The system was mainly made up with the medical X-ray, X-ray image intensifier, CCD vidicon with high resolution, image processor, display and so on. Its characteristics are: change the invisible X-ray into the visible light image; output the vivid images; short image recording time etc. At the same time we analyzed the main aspects which affect the system's resolution. Medical photo electricity system using X-ray image sensor can reduce the X-ray harm to human sharply when it is used in the medical diagnoses. At last we analyzed and looked forward the system's application in medical engineering and the related fields.

  17. A feasibility study of dynamic stress analysis inside a running internal combustion engine using synchrotron X-ray beams.

    Science.gov (United States)

    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).

  18. In situ characterization of delamination and crack growth of a CGO–LSM multi-layer ceramic sample investigated by X-ray tomographic microscopy

    DEFF Research Database (Denmark)

    Bjørk, Rasmus; Esposito, Vincenzo; Lauridsen, Erik Mejdal

    2014-01-01

    The densification, delamination and crack growth behavior in a Ce0.9Gd0.1O1.95 (CGO) and (La0.85Sr0.15)0.9MnO3 (LSM) multi-layer ceramic sample was studied using in situ X-ray tomographic microscopy (microtomography) to investigate the critical dynamics of crack propagation and delamination...... in a multilayered sample. Naturally occurring defects, caused by the sample preparation process, are shown not to be critical in sample degradation. Instead defects are nucleated during the debinding step. Crack growth is significantly faster along the material layers than perpendicular to them, and crack growth...

  19. X-Ray

    Science.gov (United States)

    ... enema. What you can expect During the X-ray X-rays are performed at doctors' offices, dentists' offices, ... as those using a contrast medium. Your child's X-ray Restraints or other techniques may be used to ...

  20. Thin, X-ray-Transparent Windows for Imaging Applications with a Pneumatically Pressurized Enclosure

    International Nuclear Information System (INIS)

    Shu Deming; Wang Jin; Preissner, Curt

    2007-01-01

    We have developed a novel thin, x-ray-transparent window system for environmental chambers involving pneumatic pressures above 10 bar. The windows allow for x-ray access to fuel sprays injected into a pressurized chamber that mimics realistic internal combustion engine cylinder operating conditions. The design of the window system and its experimental test results are presented in this paper, as well as its further development for in situ x-ray imaging applications in a high-pressure and high-temperature environment

  1. A study on the measurement of effective energy of leakage X-rays

    International Nuclear Information System (INIS)

    Fijimoto, Nobuhisa; Oogama, Noboru; Nishitani, Motohiro; Yamada, Katsuhiko

    1997-01-01

    It is important to correct for the energy response of the X-ray detector in measuring X-ray leakage from the protective barrier of the examination room. However, measurement of effective energy of leakage X-rays is very difficult in the clinical setting. In this paper, we discuss a method for estimating the effective energy of both primary and scattered X-rays. This method is based on the measurement of leakage X-ray spectra using a semiconductor-fitted X-ray detector and analyzing the relationship between X-ray tube voltage and effective energy. In this study. we found that the effective energy of leakage X-rays was not dependent on the thickness of shielding materials like concrete and lead. With the concrete barrier, it was possible to express the relation-ship between X-ray tube voltage and the effective energy of leakage X-rays with a simple approximate equation. With the lead-lined barrier, the absorption of the K-edge of lead needs to be considered in estimating the effective energy of leakage X-rays at relatively high tube voltages. (author)

  2. In situ stress determination by X-ray diffractometry and its prospects

    International Nuclear Information System (INIS)

    Castex, Louis

    The mechanical behavior of the metallic construction generally relates to the amount of the residual stress which reigned in the constitutive material. It is then essential to evaluate the residual stress inside the material without destruction. The X-ray diffractometry apparatus which we have developed for this study consisted of the use of the linear sensitive detector, the special psi-goniometer and the programming computer [fr

  3. Interaction between U/UO2 bilayers and hydrogen studied by in-situ X-ray diffraction

    Science.gov (United States)

    Darnbrough, J. E.; Harker, R. M.; Griffiths, I.; Wermeille, D.; Lander, G. H.; Springell, R.

    2018-04-01

    This paper reports experiments investigating the reaction of H2 with uranium metal-oxide bilayers. The bilayers consist of ≤ 100 nm of epitaxial α-U (grown on a Nb buffer deposited on sapphire) with a UO2 overlayer of thicknesses of between 20 and 80 nm. The oxides were made either by depositing via reactive magnetron sputtering, or allowing the uranium metal to oxidise in air at room temperature. The bilayers were exposed to hydrogen, with sample temperatures between 80 and 200 C, and monitored via in-situ x-ray diffraction and complimentary experiments conducted using Scanning Transmission Electron Microscopy - Electron Energy Loss Spectroscopy (STEM-EELS). Small partial pressures of H2 caused rapid consumption of the U metal and lead to changes in the intensity and position of the diffraction peaks from both the UO2 overlayers and the U metal. There is an orientational dependence in the rate of U consumption. From changes in the lattice parameter we deduce that hydrogen enters both the oxide and metal layers, contracting the oxide and expanding the metal. The air-grown oxide overlayers appear to hinder the H2-reaction up to a threshold dose, but then on heating from 80 to 140 C the consumption is more rapid than for the as-deposited overlayers. STEM-EELS establishes that the U-hydride layer lies at the oxide-metal interface, and that the initial formation is at defects or grain boundaries, and involves the formation of amorphous and/or nanocrystalline UH3. This explains why no diffraction peaks from UH3 are observed.

  4. High-energy X-ray diffraction studies of disordered materials

    International Nuclear Information System (INIS)

    Kohara, Shinji; Suzuya, Kentaro

    2003-01-01

    With the arrival of the latest generation of synchrotron sources and the introduction of advanced insertion devices (wigglers and undulators), the high-energy (E≥50 keV) X-ray diffraction technique has become feasible, leading to new approaches in the quantitative study of the structure of disordered materials. High-energy X-ray diffraction has several advantages: higher resolution in real space due to a wide range of scattering vector Q, smaller correction terms (especially the absorption correction), reduction of truncation errors, the feasibility of running under extreme environments, including high-temperatures and high-pressures, and the ability to make direct comparisons between X-ray and neutron diffraction data. Recently, high-energy X-ray diffraction data have been combined with neutron diffraction data from a pulsed source to provide more detailed and reliable structural information than that hitherto available

  5. Electromigration in integrated circuit interconnects studied by X-ray microscopy

    Energy Technology Data Exchange (ETDEWEB)

    Schneider, G. E-mail: gschnei1@gwdg.de; Denbeaux, G.; Anderson, E.; Bates, W.; Salmassi, F.; Nachimuthu, P.; Pearson, A.; Richardson, D.; Hambach, D.; Hoffmann, N.; Hasse, W.; Hoffmann, K

    2003-01-01

    To study mass transport phenomena in advanced microelectronic devices with X-rays requires penetration of dielectric and Si layers up to 30 {mu}m thick. X-ray imaging at 1.8 keV photon energy provides a high amplitude contrast between Cu or Al interconnects and dielectric layers and can penetrate through the required thickness. To perform X-ray microscopy at 1.8 keV, a new Ru/Si multilayer was designed for the transmission X-ray microscope XM-1 installed at the Advanced Light Source in Berkeley. The mass flow in a passivated Cu interconnect was studied at current densities up to 10{sup 7} A/cm{sup 2}. In addition, we demonstrated the high material contrast from different elements in integrated circuits with a resolution of about 40 nm.

  6. Electromigration in integrated circuit interconnects studied by X-ray microscopy

    CERN Document Server

    Schneider, G; Anderson, E; Bates, W; Salmassi, F; Nachimuthu, P; Pearson, A; Richardson, D; Hambach, D; Hoffmann, N; Hasse, W; Hoffmann, K

    2003-01-01

    To study mass transport phenomena in advanced microelectronic devices with X-rays requires penetration of dielectric and Si layers up to 30 mu m thick. X-ray imaging at 1.8 keV photon energy provides a high amplitude contrast between Cu or Al interconnects and dielectric layers and can penetrate through the required thickness. To perform X-ray microscopy at 1.8 keV, a new Ru/Si multilayer was designed for the transmission X-ray microscope XM-1 installed at the Advanced Light Source in Berkeley. The mass flow in a passivated Cu interconnect was studied at current densities up to 10 sup 7 A/cm sup 2. In addition, we demonstrated the high material contrast from different elements in integrated circuits with a resolution of about 40 nm.

  7. Synchrotron x-ray microbeam characteristics for x-ray fluorescence analysis

    International Nuclear Information System (INIS)

    Iida, Atsuo; Noma, Takashi

    1995-01-01

    X-ray fluorescence analysis using a synchrotron x-ray microprobe has become an indispensable technique for non-destructive micro-analysis. One of the most important parameters that characterize the x-ray microbeam system for x-ray fluorescence analysis is the beam size. For practical analysis, however, the photon flux, the energy resolution and the available energy range are also crucial. Three types of x-ray microbeam systems, including monochromatic and continuum excitation systems, were compared with reference to the sensitivity, the minimum detection limit and the applicability to various types of x-ray spectroscopic analysis. 16 refs., 5 figs

  8. X-ray hot plasma diagnostics

    International Nuclear Information System (INIS)

    Cojocaru, E.

    1984-11-01

    X-ray plasma emission study is powerful diagnostic tool of hot plasmas. In this review article the main techniques of X-ray plasma emission measurement are shortly presented: X-ray spectrometry using absorbent filters, crystal and grating spectrometers, imaging techniques using pinhole cameras, X-ray microscopes and Fresnel zone plate cameras, X-ray plasma emission calorimetry. Advances in these techniques with examples for different hot plasma devices are also presentes. (author)

  9. In situ 3D characterization of high temperature fatigue damage mechanisms in a cast aluminum alloy using synchrotron X-ray tomography

    International Nuclear Information System (INIS)

    Dezecot, Sebastien; Buffiere, Jean-Yves; Koster, Alain; Maurel, Vincent; Szmytka, Fabien; Charkaluk, Eric; Dahdah, Nora; El Bartali, Ahmed; Limodin, Nathalie; Witz, Jean-Francois

    2016-01-01

    Fatigue tests were performed at 250 °C on a cast AlSi7Cu3Mg aluminum alloy and monitored with Synchrotron in situ X-ray tomography in order to understand the micro-mechanisms of crack initiation and propagation. The analysis of the 3D images reveals that internal shrinkage pores are responsible for the main crack initiation. Crack propagation is mainly due to the complex and highly interconnected network of hard particles of the eutectic regions.

  10. Advances in martensitic transformations in Cu-based shape memory alloys achieved by in situ neutron and synchrotron X-ray diffraction methods

    Czech Academy of Sciences Publication Activity Database

    Malard, B.; Šittner, Petr; Berveiller, S.; Patoor, E.

    2012-01-01

    Roč. 13, č. 3 (2012), s. 280-292 ISSN 1631-0705 R&D Projects: GA ČR GAP108/10/1296; GA ČR GAP107/12/0800 EU Projects: European Commission(XE) 262806 - SmartNets Institutional research plan: CEZ:AV0Z10100520 Keywords : stress induced martensitic transformation * Cu-based shape memory alloys * neutron diffraction * X-ray * synchrotron * in situ * multiscale analysis Subject RIV: BM - Solid Matter Physics ; Magnetism Impact factor: 1.818, year: 2012

  11. X-ray sky

    International Nuclear Information System (INIS)

    Gruen, M.; Koubsky, P.

    1977-01-01

    The history is described of the discoveries of X-ray sources in the sky. The individual X-ray detectors are described in more detail, i.e., gas counters, scintillation detectors, semiconductor detectors, and the principles of X-ray spectrometry and of radiation collimation aimed at increased resolution are discussed. Currently, over 200 celestial X-ray sources are known. Some were identified as nebulae, in some pulsations were found or the source was identified as a binary star. X-ray bursts of novae were also observed. The X-ray radiation is briefly mentioned of spherical star clusters and of extragalactic X-ray sources. (Oy)

  12. X-ray fluorescence analyzers for investigating postmediaeval pottery from Southern Moravia

    International Nuclear Information System (INIS)

    Trojek, Tomas; Hlozek, Matin; Cechak, Tomas; Musilek, Ladislav

    2010-01-01

    This paper deals with an investigation of ceramic archaeological finds with the use of in-situ X-ray fluorescence analysis. Firstly, three configurations of X-ray fluorescence analyzers constructed and used at the Czech Technical University in Prague are described and compared for use in a non-destructive survey of siliceous materials. Detection limits, depth of analysis, the relation of the analyzed area, the homogeneity of the samples, and variations in the element concentrations are discussed. Secondly, many shards of postmediaeval pottery from Southern Moravia are analyzed with X-ray fluorescence analysis and some of them also with electron microprobe analysis. Selected results are described.

  13. Effect of Cl2- and HBr-based inductively coupled plasma etching on InP surface composition analyzed using in situ x-ray photoelectron spectroscopy

    International Nuclear Information System (INIS)

    Bouchoule, S.; Vallier, L.; Patriarche, G.; Chevolleau, T.; Cardinaud, C.

    2012-01-01

    A Cl 2 -HBr-O 2 /Ar inductively coupled plasma (ICP) etching process has been adapted for the processing of InP-based heterostructures in a 300-mm diameter CMOS etching tool. Smooth and anisotropic InP etching is obtained at moderate etch rate (∼600 nm/min). Ex situ x-ray energy dispersive analysis of the etched sidewalls shows that the etching anisotropy is obtained through a SiO x passivation mechanism. The stoichiometry of the etched surface is analyzed in situ using angle-resolved x-ray photoelectron spectroscopy. It is observed that Cl 2 -based ICP etching results in a significantly P-rich surface. The phosphorous layer identified on the top surface is estimated to be ∼1-1.3-nm thick. On the other hand InP etching in HBr/Ar plasma results in a more stoichiometric surface. In contrast to the etched sidewalls, the etched surface is free from oxides with negligible traces of silicon. Exposure to ambient air of the samples submitted to Cl 2 -based chemistry results in the complete oxidation of the P-rich top layer. It is concluded that a post-etch treatment or a pure HBr plasma step may be necessary after Cl 2 -based ICP etching for the recovery of the InP material.

  14. Femtosecond X-ray magnetic circular dichroism absorption spectroscopy at an X-ray free electron laser

    Energy Technology Data Exchange (ETDEWEB)

    Higley, Daniel J., E-mail: dhigley@stanford.edu; Yuan, Edwin [SLAC National Accelerator Laboratory, 2575 Sand Hill Road, Menlo Park, California 94025 (United States); Department of Applied Physics, Stanford University, Stanford, California 94305 (United States); Hirsch, Konstantin; Dakovski, Georgi L.; Jal, Emmanuelle; Lutman, Alberto A.; Coslovich, Giacomo; Hart, Philip; Hoffmann, Matthias C.; Mitra, Ankush; Moeller, Stefan; Ohldag, Hendrik; Seaberg, Matthew; Stöhr, Joachim; Nuhn, Heinz-Dieter; Reid, Alex H.; Dürr, Hermann A.; Schlotter, William F. [SLAC National Accelerator Laboratory, 2575 Sand Hill Road, Menlo Park, California 94025 (United States); Liu, Tianmin; MacArthur, James P. [SLAC National Accelerator Laboratory, 2575 Sand Hill Road, Menlo Park, California 94025 (United States); Department of Physics, Stanford University, Stanford, California 94305 (United States); and others

    2016-03-15

    X-ray magnetic circular dichroism spectroscopy using an X-ray free electron laser is demonstrated with spectra over the Fe L{sub 3,2}-edges. The high brightness of the X-ray free electron laser combined with high accuracy detection of incident and transmitted X-rays enables ultrafast X-ray magnetic circular dichroism studies of unprecedented sensitivity. This new capability is applied to a study of all-optical magnetic switching dynamics of Fe and Gd magnetic sublattices in a GdFeCo thin film above its magnetization compensation temperature.

  15. In situ synchrotron x-ray characterization of microstructure formation in solidification processing of Al-based metallic alloys

    International Nuclear Information System (INIS)

    Billia, Bernard; Nguyen-Thi, Henri; Mangelinck-Noel, Nathalie

    2010-01-01

    The microstructure formed during the solidification step has a major influence on the properties of materials processed by major techniques (casting, welding ...). In situ and real-time characterization by synchrotron X-ray imaging is the method of choice to unveil the dynamical formation of the solidification microstructure in metallic alloys, and thus provide precise data for the critical validation of the theoretical predictions that is needed for sound advancement of modeling and numerical simulation. After a description of the experimental procedure used at the European Synchrotron Radiation Facility (ESRF), dynamical phenomena in the formation of the grain structure and dendritic or equiaxed solidification microstructure in Al-based alloys are presented. Beyond fluid flow interaction, earth gravity induces stresses, deformation and fragmentation in the dendritic mush. Settling of dendrite arms and equiaxed grains thus occurs, in particular in the columnar to equiaxed transition. Other types of stresses and strains are caused by the mere formation of the solidification microstructure itself. In white-beam X-ray topography, stresses and strains are manifested by specific contrasts and breaking of the Laue images into several pieces. Finally, quantitative analysis of the grey level in radiographs enables the analysis of solute segregation, which noticeably results in solutal poisoning of growth when equiaxed grains are interacting. (author)

  16. Chandra and RXTE studies of the X-ray/gamma-ray millisecond pulsar PSR J0218+4232

    NARCIS (Netherlands)

    Kuiper, L.; Hermsen, W.; Stappers, B.W.

    2004-01-01

    We report on high-resolution spatial and timing observations of the millisecond pulsar PSR J0218+4232 performed with the Chandra X-ray Observatory (CXO) and the Rossi X-ray Timing Explorer (RXTE). With these observations we were able to study: (a) the possible spatial extent at X-ray energies of the

  17. Applicability of X-ray reflectometry to studies of polymer solar cell degradation

    DEFF Research Database (Denmark)

    Andreasen, Jens Wenzel; Gevorgyan, Suren; Schleputz, C.M.

    2008-01-01

    Although degradation of polymer solar cells is widely acknowledged, the cause, physical or chemical, has not been identified. The purpose of this work is to determine the applicability of X-ray reflectometry for in situ observation of physical degradation mechanisms. We find that the rough...... interfaces of the polymer solar cell constituent layers seriously obstruct the sensitivity of the technique, rendering it impossible to elucidate changes in the layer/interface structure at the sub-nanometer level. (c) 2008 Elsevier B.V. All rights reserved....

  18. A quality measurement study of a diagnostic x-ray

    International Nuclear Information System (INIS)

    Nishitani, Motohiro; Fujimoto, Nobuhisa; Yamada, Katsuhiko

    1982-01-01

    It is important to check periodically the quality and quantity of the X-rays emitted, in order to obtain the best possible performance from your diagnostic X-ray apparatus. The best way of checking the exact quality of the X-ray is to measure the spectrum of the X-ray, but it is not an easy task to carry out. The second way is to plot the attenuation curve of the X-rays. We have developed a method to plot the attenuation curve by a single exposure, utilizing J.r. Greening's empirical formula. The output of the three cavity ionization chambers, one with 7 mmAl filter, another with a 3 mmAl and the third without any filter, exposed to the same X-ray, were put into a microcomputer. The programming was arranged to display the attenuation curve of the X-rays, effective energy of the X-rays, the 1st HVL and the 2nd HVL on the CRT. The attenuation curves of the X-rays, emitted at a tube voltage at between 60 and 140 kV obtained by this method, agreed with the experimental results with an error of +-4 %. The effective energy obtained by this method agreed with the experimental data with an error of +-1 %. (author)

  19. An in situ cell to study phase transitions in individual aerosol particles on a substrate using scanning transmission x-ray microspectroscopy

    International Nuclear Information System (INIS)

    Huthwelker, T.; Zelenay, V.; Birrer, M.; Krepelova, A.; Raabe, J.; Ammann, M.; Tzvetkov, G.; Vernooij, M. G. C.

    2010-01-01

    A new in situ cell to study phase transitions and chemical processes on individual aerosol particles in the x-ray transmission microscope at the PolLux beamline of the Swiss light source has been built. The cell is machined from stainless steel and aluminum components and is designed to be used in the standard mount of the microscope without need of complicated rearrangements of the microscope. The cell consists of two parts, a back part which contains connections for the gas supply, heating, cooling devices, and temperature measurement. The second part is a removable clip, which hosts the sample. This clip can be easily exchanged and brought into a sampling unit for aerosol particles. Currently, the cell can be operated at temperatures ranging from -40 to +50 deg. C. The function of the cell is demonstrated using two systems of submicron size: inorganic sodium bromide aerosols and soot originating from a diesel passenger car. For the sodium bromide we demonstrate how phase transitions can be studied in these systems and that O1s spectra from aqueous sodium bromide solution can be taken from submicron sized particles. For the case of soot, we demonstrate that the uptake of water onto individual soot particles can be studied.

  20. X-ray diffraction investigation of self-annealing in nanocrystalline copper electrodeposits

    DEFF Research Database (Denmark)

    Pantleon, Karen; Somers, Marcel A. J.

    2006-01-01

    X-ray diffraction analysis and electrical resistivity measurements were conducted simultaneously for in-situ examination of self-annealing in copper electrodeposits. Considerable growth of the as-deposited nano-sized crystallites occurs with time and the crystallographic texture changes by multip...... twinning during self-annealing. The kinetics of self-annealing depends on the layer thickness as well as on the orientation and/or the size of the as-deposited crystallites. (c) 2006 Acta Materialia Inc. Published by Elsevier Ltd. All rights reserved.......X-ray diffraction analysis and electrical resistivity measurements were conducted simultaneously for in-situ examination of self-annealing in copper electrodeposits. Considerable growth of the as-deposited nano-sized crystallites occurs with time and the crystallographic texture changes by multiple...

  1. X-ray magnification studies in biology and some other applications. Chapter 6

    International Nuclear Information System (INIS)

    Van Emden, H.F.; Ely, R.V.

    1980-01-01

    The facilities of X-ray mirofocal equipment of particular value in biological research are outlined. The applications of X-ray magnification techniques in various entomological studies is described particularly for observing plant pests. The value of these techniques in miscellaneous botanical studies is also described, e.g. in seed quality analysis, the monitoring of the early stages of reproductive development in seeds, the distribution of crystals in plant tissues and the X-ray absorption of cell constituents. Reference is also made to the use of transmission target techniques which permit higher direct X-ray magnifications of small selected specimen areas, e.g. penetration of paints and resins into timber. Further miscellaneous research applications of X-ray magnification techniques are described, e.g. in geological studies of fossils and sedimentary rocks, in archaeological studies of metal objects, excavated human bones etc. and in Fine Art studying the technique of past artists and detecting art forgeries. Finally it is pointed out that another important application of microfocal X-rays could be in the study of radiation damage in living animals or plants. (U.K.)

  2. Catalogue of response spectra for unfolding in situ gamma-ray pulse-height distributions

    International Nuclear Information System (INIS)

    Dymke, N.

    1982-01-01

    To unfold in situ gamma-ray pulse-height distributions by means of a response matrix technique, the matrix must be in keeping with the measurement geometry, detector size, and energy range to be covered by the measurements. A methodology has been described for determination of standard gamma-ray spectra needed in deriving response matrices and a spectrum catalogue compiled containing graphs and data for the 0-3 MeV (4 x 4 in. NaI(Tl)) and 0-8 MeV (1.5 x 1.5 in. NaI(Tl)) ranges. (author)

  3. Time-resolved X-ray studies using third generation synchrotron radiation sources

    International Nuclear Information System (INIS)

    Mills, D.M.

    1991-10-01

    The third generation, high-brilliance, hard x-ray, synchrotron radiation (SR) sources currently under construction (ESRF at Grenoble, France; APS at Argonne, Illinois; and SPring-8 at Harima, Japan) will usher in a new era of x-ray experimentation for both physical and biological sciences. One of the most exciting areas of experimentation will be the extension of x-ray scattering and diffraction techniques to the study of transient or time-evolving systems. The high repetition rate, short-pulse duration, high brilliance, and variable spectral bandwidth of these sources make them ideal for x-ray time-resolved studies. The temporal properties (bunch length, interpulse period, etc.) of these new sources will be summarized. Finally, the scientific potential and the technological challenges of time-resolved x-ray scattering from these new sources will be described. 13 refs., 4 figs

  4. Commercial Applications of X Ray Spectrometric Techniques

    Energy Technology Data Exchange (ETDEWEB)

    Wegrzynek, D., E-mail: D.Wedgrznek@iaea.org [International Atomic Energy Agency, The IAEA Laboratories, Seibersdorf, Vienna (Austria)

    2013-07-15

    In the 21st century, the X-ray fluorescence (XRF) technique is widely used in process control, industrial applications and for routine elemental analysis. The technique has a multielement capability capable of detecting elements with Z {>=} 10, with a few instruments capable of detecting also elements with Z {>=} 5. It is characterized by a non-destructive analysis process and relatively good detection limits, typically one part per million, for a wide range of elements. The first commercial XRF instruments were introduced to the market about 50 years ago. They were the wavelength dispersive X ray fluorescence (WDXRF) spectrometers utilizing Bragg's law and reflection on crystal lattices for sequential elemental analysis of sample composition. The advances made in radiation detector technology, especially the introduction of semiconductor detectors, improvements in signal processing electronics, availability and exponential growth of personal computer market led to invention of energy dispersive X ray fluorescence (EDXRF) technique. The EDXRF is more cost effective as compared to WDXRF. It also allows for designing compact instruments. Such instruments can be easily tailored to the needs of different customers, integrated with industrial installations, and also miniaturized for the purpose of in-situ applications. The versatility of the technique has been confirmed in a spectacular way by using the XRF and X-ray spectrometric techniques, among few others, during the NASA and ESA missions in search for the evidence of life and presence of water on the surface of Mars. The XRF technique has achieved its strong position within the atomic spectroscopy group of analytical techniques not only due to its versatility but also due to relatively low running costs, as compared to the commonly used methods, e.g., atomic absorption spectrometry (AAS) or inductively coupled plasma atomic emission/mass spectrometry (ICP-AES/MS). Presently, the XRF technique together with X ray

  5. X-ray and neutron scattering studies of complex confined fluids

    International Nuclear Information System (INIS)

    Sinha, S. K.

    1999-01-01

    We review recent X-ray and neutron scattering studies of the structure and dynamics of confined complex fluids. This includes the study of polymer conformations and binary fluid phase transitions in porous media using Small Angle Neutron scattering, and the use of synchrotrons radiation to study ordering and fluctuation phenomena at solid/liquid and liquid/air interfaces. Ordering of liquids near a solid surface or in confinement will be discussed, and the study, via specular and off-specular X-ray reflectivity, of capillary wave fluctuations on liquid polymer films. Finally, we shall discuss the use of high-brilliance beams from X-ray synchrotrons to study via photon correlation spectroscopy the slow dynamics of soft condensed matter systems

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

    Energy Technology Data Exchange (ETDEWEB)

    Zhang Xiaodan; Xia Chengjie; Sun Haohua; Wang Yujie [Department of Physics, Shanghai Jiao Tong University, 800 Dong Chuan Road, Shanghai 200240 (China)

    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.

  7. High-pressure behavior of synthetic mordenite-Na. An in situ single-crystal synchrotron X-ray diffraction study

    Energy Technology Data Exchange (ETDEWEB)

    Lotti, Paolo; Merlini, Marco [Univ. degli Studi di Milano, (Italy). Dipt. di Scienze della Terra; Gatta, G. Diego [Univ. degli Studi di Milano, (Italy). Dipt. di Scienze della Terra; CNR, Bari (Italy). Int. di Cristallografia; Liermann, Hanns-Peter [DESY, Hamburg (Germany). Photon Sciences

    2015-05-01

    The high-pressure behavior of a synthetic mordenite-Na (space group: Cmcm or Cmc2{sub 1}) was studied by in situ single-crystal synchrotron X-ray diffraction with a diamond anvil cell up to 9.22(7) GPa. A phase transition, likely displacive in character, occurred between 1.68(7) and 2.70(8) GPa, from a C-centered to a primitive space group: possibly Pbnm, Pbnn or Pbn2{sub 1}. Fitting of the experimental data with III-BM equations of state allowed to describe the elastic behavior of the high-pressure polymorph with a primitive lattice. A very high volume compressibility [K{sub V0} = 25(2) GPa, β{sub V0} = 1/K{sub V0} = 0.040(3) GPa{sup -1}; K{sub V}' = (∂K{sub V}/∂P){sub T} = 2.0(3)], coupled with a remarkable elastic anisotropy (β{sub b}>>β{sub c}>β{sub a}), was found. Interestingly, the low-P and high-P polymorphs show the same anisotropic compressional scheme. A structure collapse was not observed up to 9.22(7) GPa, even though a strong decrease of the number of observed reflections at the highest pressures suggests an impending amorphization. The structure refinements performed at room-P, 0.98(2) and 1.68(7) GPa allowed to describe, at a first approximation, the mechanisms that govern the framework deformation in the low-P regime: the bulk compression is strongly accommodated by the increase of the ellipticity of the large 12-membered ring channels running along [001].

  8. The NASA X-Ray Mission Concepts Study

    Science.gov (United States)

    Petre, Robert; Ptak, A.; Bookbinder, J.; Garcia, M.; Smith, R.; Bautz, M.; Bregman, J.; Burrows, D.; Cash, W.; Jones-Forman, C.; hide

    2012-01-01

    The 2010 Astrophysics Decadal Survey recommended a significant technology development program towards realizing the scientific goals of the International X-ray Observatory (IXO). NASA has undertaken an X-ray mission concepts study to determine alternative approaches to accomplishing IXO's high ranking scientific objectives over the next decade given the budget realities, which make a flagship mission challenging to implement. The goal of the study is to determine the degree to which missions in various cost ranges from $300M to $2B could fulfill these objectives. The study process involved several steps. NASA released a Request for Information in October 2011, seeking mission concepts and enabling technology ideas from the community. The responses included a total of 14 mission concepts and 13 enabling technologies. NASA also solicited membership for and selected a Community Science Team (CST) to guide the process. A workshop was held in December 2011 in which the mission concepts and technology were presented and discussed. Based on the RFI responses and the workshop, the CST then chose a small group of notional mission concepts, representing a range of cost points, for further study. These notional missions concepts were developed through mission design laboratory activities in early 2012. The results of all these activities were captured in the final X-ray mission concepts study report, submitted to NASA in July 2012. In this presentation, we summarize the outcome of the study. We discuss background, methodology, the notional missions, and the conclusions of the study report.

  9. Skull x-ray

    Science.gov (United States)

    X-ray - head; X-ray - skull; Skull radiography; Head x-ray ... There is low radiation exposure. X-rays are monitored and regulated to provide the minimum amount of radiation exposure needed to produce the image. Most ...

  10. Neck x-ray

    Science.gov (United States)

    X-ray - neck; Cervical spine x-ray; Lateral neck x-ray ... There is low radiation exposure. X-rays are monitored so that the lowest amount of radiation is used to produce the image. Pregnant women and ...

  11. X-ray studies of BL Lacertae objects

    International Nuclear Information System (INIS)

    Madejski, G.M.

    1986-01-01

    This thesis presents spectral x-ray data for BL Lac objects observed by the IPC and MPC aboard the Einstein Observatory and interprets that data in a context of their overall radiation spectra using synchrotron and synchrotron self-Compton models. The objects considered are: OJ 287, PKS 0735 + 178, I Zw 186, PKS 0548-322, Mkn 180, BL Lacertae, PKS 2155-304, H 0414-009 and H 0323 + 022. X-ray spectra of BL Lac objects are well described by a power law model with a low energy cutoff due to absorption within the own Galaxy. The best fit values of the energy spectral index α in the IPC (0.2-4.0 keV) band range from 0.73 to 2.35, with a mean of 1.2 and rms spread of 0.51. No single, universal index can fit the spectra of all objects. For all objects except PKS 0735 + 178, the x-ray spectrum is an extrapolation of the infrared/optical UV spectrum; in PKS 0735 + 178, the x-ray spectrum lies significantly below such an extrapolation. The overall electromagnetic distribution in those objects is interpreted as arising due to the synchrotron process in at least two spatial regions, with sizes respectively ∼10 18 cm for the radio component and ∼10 16 cm for the optical component. In objects where the x-ray spectrum lies on the extrapolation of the infrared-optical-ultraviolet spectrum, the x-ray emission is interpreted also to be due to the synchrotron process

  12. Effects of thermal annealing on C/FePt granular multilayers: in situ and ex situ studies

    International Nuclear Information System (INIS)

    Babonneau, D; Abadias, G; Toudert, J; Girardeau, T; Fonda, E; Micha, J S; Petroff, F

    2008-01-01

    The comprehensive study of C/FePt granular multilayers prepared by ion-beam sputtering at room temperature and subsequent annealing is reported. The as-deposited multilayers consist of carbon-encapsulated FePt nanoparticles (average size ∼3 nm) with a disordered face-centered-cubic structure. The effects of thermal annealing on the structural and magnetic properties are investigated by using dedicated ex situ and in situ techniques, including high-resolution transmission electron microscopy, extended x-ray absorption fine structure, magnetometry, and coupled grazing incidence small-angle x-ray scattering and x-ray diffraction. Our structural data show that the particle size and interparticle distance increase slightly with annealing at temperatures below 790 K by thermally activated migration of Fe and Pt atoms. We find that thermal annealing at temperatures above 870 K results in the dramatic growth of the FePt nanoparticles by coalescence and their gradual L1 0 ordering. In addition, we observe a preferential graphitization of the carbon matrix, which provides protection against oxidation for the FePt nanoparticles. Magnetization measurements indicate that progressive magnetic hardening occurs after annealing. The dependences of the blocking temperature, saturation magnetization, coercivity, and magnetocrystalline anisotropy energy on the annealing temperature are discussed on the basis of the structural data

  13. X-ray filter for chest X-rays

    International Nuclear Information System (INIS)

    Ferlic, D.J.

    1984-01-01

    A description is given of an X-ray filter comprised of a sheet of radiation absorbing material with an opening corresponding to the spine and central portion of the heart. The upper portion of the filter exhibits a relatively narrow opening which becomes gradually wider toward the lower portion of the filter. This filter will permit an acceptable density level of x-ray exposure for the lungs while allowing a higher level of x-ray exposure for the mediastinum areas of the body. (author)

  14. Crystallization kinetics of Fe-B based amorphous alloys studied in-situ using X-rays diffraction and differential scanning calorimetry

    Directory of Open Access Journals (Sweden)

    Santos D.R. dos

    2001-01-01

    Full Text Available The crystallization processes for the amorphous metallic alloys Fe74B17Si2Ni4Mo3 and Fe86B6Zr7Cu1 (at. % were investigated using X-rays diffraction measurements performed in-situ during Joule-heating, with simultaneous monitoring of the electrical resistance. We determined the main structural transitions and crystalline phases formed during heating, and correlated these results to the observed resistance variations. As the annealing current is increased, the resistance shows an initial decrease due to stress relaxation, followed by a drop to a minimum value due to massive nucleation and growth of alpha-Fe nanocrystals. Further annealing causes the formation of small fractions of Fe-B, B2Zr or ZrO2, while the resistance increases due to temperature enhancement. In situ XRD measurements allowed the identification of metastable phases, as the gamma-Fe phase which occurs at high temperatures. The exothermal peaks observed in the differential scanning calorimetry (DSC for each alloy corroborate the results. We also have performed DSC measurements with several heating rates, which allowed the determination of the Avrami exponent and crystallization activation energy for each alloy. The obtained activation energies (362 and 301 kJ/mol for Fe-B-Zr-Cu; 323 kJ/mol for Fe-B-Si-Ni-Mo are comparable to reported values for amorphous iron alloys, while the Avrami exponent values (n = 1.0 or n = 1.2 are consistent with diffusion controlled crystallization processes with nucleation rates close to zero.

  15. X-ray astronomy 2000: Wide field X-ray monitoring with lobster-eye telescopes

    International Nuclear Information System (INIS)

    Inneman, A.; Hudec, R.; Pina, L.; Gorenstein, P.

    2001-01-01

    The recently available first prototypes of innovative very wide field X-ray telescopes of Lobster-Eye type confirm the feasibility to develop such flight instruments in a near future. These devices are expected to allow very wide field (more than 1000 square degrees) monitoring of the sky in X-rays (up to 10 keV and perhaps even more) with faint limits. We will discuss the recent status of the development of very wide field X-ray telescopes as well as related scientific questions including expected major contributions such as monitoring and study of X-ray afterglows of Gamma Ray Bursts

  16. In situ synchrotron X-ray diffraction study of surface scale formation during CO2 corrosion of carbon steel at temperatures up to 90 oC

    International Nuclear Information System (INIS)

    Ingham, B.; Ko, M.; Kear, G.; Kappen, P.; Laycock, N.; Kimpton, J.A.; Williams, D.E.

    2010-01-01

    In situ synchrotron X-ray diffraction was used to follow the formation of corrosion product scales on carbon steel in CO 2 saturated brine at temperatures from 40 to 90 o C. The corrosion process was accelerated by applying a small anodic current, and in selected tests a scale inhibitor, amino trimethylene phosphonic acid (ATMPA), was added. Siderite was identified as the major phase in the scale formed in all conditions. With increasing temperature, the scale formation rate increased, while the scale thickness and crystallite size decreased. Above 60 o C, the scale became increasingly protective. The scale thickness and crystallite size decreased with increasing ATMPA concentration.

  17. NIKOLA TESLA AND THE X-RAY

    OpenAIRE

    Rade R. Babic

    2005-01-01

    After professor Wilhelm Konrad Röntgen published his study of an x-ray discovery (Academy Bulletin, Berlin, 08. 11. 1895.), Nikola Tesla published his first study of an x-ray on the 11th of March in 1896. (X-ray, Electrical Review). Until the 11th of August in 1897 he had published ten studies on this subject. All Tesla,s x-ray studies were experimental, which is specific to his work. Studying the nature of the x-ray, he established a new medical branch-radiology. He wrote:” There’s no doubt...

  18. X-ray Absorption Spectroscopy

    Energy Technology Data Exchange (ETDEWEB)

    Yano, Junko; Yachandra, Vittal K.

    2009-07-09

    This review gives a brief description of the theory and application of X-ray absorption spectroscopy, both X-ray absorption near edge structure (XANES) and extended X-ray absorption fine structure (EXAFS), especially, pertaining to photosynthesis. The advantages and limitations of the methods are discussed. Recent advances in extended EXAFS and polarized EXAFS using oriented membranes and single crystals are explained. Developments in theory in understanding the XANES spectra are described. The application of X-ray absorption spectroscopy to the study of the Mn4Ca cluster in Photosystem II is presented.

  19. X-ray filtration apparatus

    International Nuclear Information System (INIS)

    Thompson, G.

    1992-01-01

    This invention relates to an X-ray shielding support device. In spite of considerable development in X-ray taking techniques, a need still exists for effective shielding, inter alia, to compensate for variations in the thickness, density and the absorption properties of the object being studied. By appropriate shielding, the X-ray image produced is of sufficient detail, contrast and intensity over its entire area to constitute a useful diagnostic aid. It is also desirable to subject the patient to the smallest possible X-ray dosage. 4 figs

  20. Radiobiological studies using gamma and x rays.

    Energy Technology Data Exchange (ETDEWEB)

    Potter, Charles Augustus; Longley, Susan W.; Scott, Bobby R.; Lin, Yong; Wilder, Julie; Hutt, Julie A.; Padilla, Mabel T.; Gott, Katherine M.

    2013-02-01

    There are approximately 500 self-shielded research irradiators used in various facilities throughout the U.S. These facilities use radioactive sources containing either 137Cs or 60Co for a variety of biological investigations. A report from the National Academy of Sciences[1] described the issues with security of particular radiation sources and the desire for their replacement. The participants in this effort prepared two peer-reviewed publications to document the results of radiobiological studies performed using photons from 320-kV x rays and 137Cs on cell cultures and mice. The effectiveness of X rays was shown to vary with cell type.

  1. Coherent X-ray diffraction studies of mesoscopic materials

    International Nuclear Information System (INIS)

    Shabalin, Anatoly

    2015-12-01

    This thesis is devoted to three separate projects, which can be considered as independent. First, the dynamical scattering effects in the Coherent X-ray Diffractive Imaging (CXDI) method are discussed. Based on the simulation results, a straightforward method for correction for the refraction and absorption artifacts in the Bragg CXDI reconstruction is suggested. The second part summarizes the results of an Coherent X-ray Diffractive Imaging experiment with a single colloidal crystal grain. A remarkable result is that positions of individual particles in the crystal lattice have been resolved in three dimensions. The third project is devoted to X-ray diffraction experimental studies of structural evolution of colloidal crystalline films upon incremental heating. Based on the results of the analysis a model of structural evolution of a colloidal crystal upon heating on nanoscopic and mesoscopic length scales is suggested.

  2. X-ray apparatus

    International Nuclear Information System (INIS)

    Bernstein, S.; Stagg, L.; Lambert, T.W.; Griswa, P.J.

    1976-01-01

    A patient support system for X-ray equipment in arteriographic studies of the heart is described in detail. The support system has been designed to overcome many of the practical problems encountered in using previous types of arteriographic X-ray equipment. The support system is capable of horizontal movement and, by a series of shafts attached to the main support system, the X-ray source and image intensifier or detector may be rotated through the same angle. The system is highly flexible and details are given of several possible operational modes. (U.K.)

  3. X-ray filter for chest x-rays

    International Nuclear Information System (INIS)

    Ferlic, D.J.

    1984-01-01

    Filter for use in medical x-ray apparatus to permit higher intensity x-ray exposure in the heart and mediastinum area while maintaining a normal level of x-ray exposure in other areas of the body, particlarly in the lung area. The filter comprises a sheet of radiation absorbing material having an opening therein, said opening corresponding to the spine and central portion of the heart. Accordingly, the upper portion of the filter exhibits a relatively narrow opening which becomes gradually wider toward the lower portion of the filter

  4. Future planetary X-ray and gamma-ray remote sensing system and in situ requirements for room temperature solid state detectors

    CERN Document Server

    Trombka, J I; Starr, R; Clark, P E; Floyd, S R

    1999-01-01

    X-Ray and gamma-ray remote sensing observations find important applications in the study of the development of the planets. Orbital measurements can be carried out on solar-system bodies whose atmospheres and trapped radiation environments do not interfere significantly with the emissions. Elemental compositions can be inferred from observations of these line emissions. Future planetary missions also will involve landing both stationery and roving probes on planetary surfaces. Both X-ray and gamma-ray spectrometers will be used for performing elemental analysis of surface samples. These future planetary missions will impose a number of constraints: the flight instruments must be significantly reduced in weight from those previously flown; for many missions, gravity assist will be required, greatly increasing mission duration, resulting in the passage of several years before the first scientific measurement of a solar system body. The detector systems must operate reliably after years of cosmic-ray irradiation...

  5. Topological X-Rays Revisited

    Science.gov (United States)

    Lynch, Mark

    2012-01-01

    We continue our study of topological X-rays begun in Lynch ["Topological X-rays and MRI's," iJMEST 33(3) (2002), pp. 389-392]. We modify our definition of a topological magnetic resonance imaging and give an affirmative answer to the question posed there: Can we identify a closed set in a box by defining X-rays to probe the interior and without…

  6. High energy x-ray scattering studies of strongly correlated oxides

    International Nuclear Information System (INIS)

    Hatton, Peter D; Wilkins, S B; Spencer, P D; Zimmermann, M v; D'Almeida, T

    2003-01-01

    Many transition metal oxides display strongly correlated charge, spin, or orbital ordering resulting in varied phenomena such as colossal magnetoresistance, high temperature superconductivity, metal-insulator transitions etc. X-ray scattering is one of the principle techniques for probing the structural response to such effects. In this paper, we discuss and review the use of synchrotron radiation high energy x-rays (50-200 keV) for the study of transition metal oxides such as nickelates (La 2-x Sr x NiO 4 ) and manganites (La 2-2x Sr 1+2x Mn 2 O 7 ). High energy x-rays have sufficient penetration to allow us to study large flux-grown single crystals. The huge increase in sample scattering volume means that extremely weak peaks can be observed. This allows us to study very weak charge ordering. Measurements of the intensity, width and position of the charge ordering satellites as a function of temperature provide us with quantitative measures of the charge amplitude, inverse correlation length and wavevector of the charge ordering

  7. X-ray geometrical smoothing effect in indirect x-ray-drive implosion

    International Nuclear Information System (INIS)

    Mochizuki, Takayasu; Sakabe, Shuji; Yamanaka, Chiyoe

    1983-01-01

    X-ray geometrical smoothing effect in indirect X-ray drive pellet implosion for inertial confinement fusion has been numerically analyzed. Attainable X-ray driven ablation pressure has been found to be coupled with X-ray irradiation uniformity. (author)

  8. Energy-dispersive X-ray reflectivity and GID for real-time growth studies of pentacene thin films

    International Nuclear Information System (INIS)

    Kowarik, S.; Gerlach, A.; Leitenberger, W.; Hu, J.; Witte, G.; Woell, C.; Pietsch, U.; Schreiber, F.

    2007-01-01

    We use energy-dispersive X-ray reflectivity and grazing incidence diffraction (GID) to follow the growth of the crystalline organic semiconductor pentacene on silicon oxide in-situ and in real-time. The technique allows for monitoring Bragg reflections and measuring X-ray growth oscillations with a time resolution of 1 min in a wide q-range in reciprocal space extending over 0.25-0.80 A -1 , i.e. sampling a large number of Fourier components simultaneously. A quantitative analysis of growth oscillations at several q-points yields the evolution of the surface roughness, showing a marked transition from layer-by-layer growth to strong roughening after four monolayers of pentacene have been deposited

  9. Theory-driven design of high-valence metal sites for water oxidation confirmed using in situ soft X-ray absorption

    Science.gov (United States)

    Zheng, Xueli; Zhang, Bo; de Luna, Phil; Liang, Yufeng; Comin, Riccardo; Voznyy, Oleksandr; Han, Lili; García de Arquer, F. Pelayo; Liu, Min; Dinh, Cao Thang; Regier, Tom; Dynes, James J.; He, Sisi; Xin, Huolin L.; Peng, Huisheng; Prendergast, David; Du, Xiwen; Sargent, Edward H.

    2018-02-01

    The efficiency with which renewable fuels and feedstocks are synthesized from electrical sources is limited at present by the sluggish oxygen evolution reaction (OER) in pH-neutral media. We took the view that generating transition-metal sites with high valence at low applied bias should improve the activity of neutral OER catalysts. Here, using density functional theory, we find that the formation energy of desired Ni4+ sites is systematically modulated by incorporating judicious combinations of Co, Fe and non-metal P. We therefore synthesized NiCoFeP oxyhydroxides and probed their oxidation kinetics with in situ soft X-ray absorption spectroscopy (sXAS). In situ sXAS studies of neutral-pH OER catalysts indicate ready promotion of Ni4+ under low overpotential conditions. The NiCoFeP catalyst outperforms IrO2 and retains its performance following 100 h of operation. We showcase NiCoFeP in a membrane-free CO2 electroreduction system that achieves a 1.99 V cell voltage at 10 mA cm-2, reducing CO2 into CO and oxidizing H2O to O2 with a 64% electricity-to-chemical-fuel efficiency.

  10. Theory-driven design of high-valence metal sites for water oxidation confirmed using in situ soft X-ray absorption.

    Science.gov (United States)

    Zheng, Xueli; Zhang, Bo; De Luna, Phil; Liang, Yufeng; Comin, Riccardo; Voznyy, Oleksandr; Han, Lili; García de Arquer, F Pelayo; Liu, Min; Dinh, Cao Thang; Regier, Tom; Dynes, James J; He, Sisi; Xin, Huolin L; Peng, Huisheng; Prendergast, David; Du, Xiwen; Sargent, Edward H

    2018-02-01

    The efficiency with which renewable fuels and feedstocks are synthesized from electrical sources is limited at present by the sluggish oxygen evolution reaction (OER) in pH-neutral media. We took the view that generating transition-metal sites with high valence at low applied bias should improve the activity of neutral OER catalysts. Here, using density functional theory, we find that the formation energy of desired Ni 4+ sites is systematically modulated by incorporating judicious combinations of Co, Fe and non-metal P. We therefore synthesized NiCoFeP oxyhydroxides and probed their oxidation kinetics with in situ soft X-ray absorption spectroscopy (sXAS). In situ sXAS studies of neutral-pH OER catalysts indicate ready promotion of Ni 4+ under low overpotential conditions. The NiCoFeP catalyst outperforms IrO 2 and retains its performance following 100 h of operation. We showcase NiCoFeP in a membrane-free CO 2 electroreduction system that achieves a 1.99 V cell voltage at 10 mA cm -2 , reducing CO 2 into CO and oxidizing H 2 O to O 2 with a 64% electricity-to-chemical-fuel efficiency.

  11. Study of properties of chemically modified samples of halloysite mineral with X-ray fluorescence and X-ray powder diffraction methods

    International Nuclear Information System (INIS)

    Banaś, D.; Kubala-Kukuś, A.; Braziewicz, J.; Majewska, U.; Pajek, M.; Wudarczyk-Moćko, J.; Czech, K.; Garnuszek, M.; Słomkiewicz, P.; Szczepanik, B.

    2013-01-01

    Elemental and chemical composition of raw and activated samples of halloysite mineral using wavelength dispersive X-ray fluorescence (WDXRF), total reflection X-ray fluorescence (TXRF) and X-ray powder diffraction (XRPD) methods were determined. As the result, it has been shown that application of the complementary X-ray spectrometry techniques allows very precise observation of changes in composition of halloysite mineral samples caused by its chemical modifications. Sample preparation procedure and usability of the research methods applied are described in details. Procedure of activation of raw halloysite mineral samples by etching them in sulfuric acid of various concentrations has been described and discussed. The ability of the samples to adsorb lead from intentionally contaminated water was tested and confirmed. - Author-Highlights: • We measured elemental and chemical composition of raw and activated halloysite mineral samples. • We showed that X-ray techniques allow precise study of changes in the sample composition. • We describe procedure of activation of the samples by etching them in sulfuric acid. • We tested ability of halloysite mineral to absorb lead from contaminated water

  12. In situ investigation by X-ray tomography of the overall and local microstructural changes occurring during partial remelting of an Al-15.8 wt.% Cu alloy

    International Nuclear Information System (INIS)

    Limodin, Nathalie; Salvo, Luc; Suery, Michel; DiMichiel, Marco

    2007-01-01

    The paper is concerned with the study of the microstructural changes occurring during holding of an Al-15.8 wt.% Cu alloy in the semi-solid state. These changes are investigated in 3D by in situ X-ray tomography carried out at the temperature of the treatment. The studies are classified in two categories: overall changes by measuring average values of characteristic parameters, and local changes by considering the evolution of individual necks between particles. It is shown in particular that the size of the solid particles or the surface area of the solid-liquid interfaces do not follow the classical power laws but rather evolve in a slower manner. Local observations confirm that these results are due to the competition of two coarsening mechanisms of the solid particles that occur simultaneously: dissolution of a small particle to the benefit of one or several bigger ones by an Ostwald-type mechanism and the growth of necks between solid particles due to their coalescence. Complex variations of neck size result from these mechanisms which can be explained only by considering the neighbourhood of the particles under investigation. These observations confirm that in situ X-ray tomography is a very powerful tool to provide data that are representative of the semi-solid state and to observe in real time the mechanisms that act on the microstructure

  13. X-ray survey of the Pleiades: dependence of X-ray luminosity on stellar age

    International Nuclear Information System (INIS)

    Micela, G.; Sciortino, S.; Serio, S.; Vaiana, G.S.; Golub, L.; Harnden, F.R.; Rosner, R.

    1984-01-01

    The study of X-ray emission of stellar clusters, allows to decouple the influence of some individual stellar parameters, as initial conditions, composition and age, on the stellar X-ray function. The authors report preliminary results from an Einstein X-ray survey of the Pleiades. (Auth.)

  14. Different X-ray spectral evolution for black hole X-ray binaries in dual tracks of radio-X-ray correlation

    International Nuclear Information System (INIS)

    Cao, Xiao-Feng; Wu, Qingwen; Dong, Ai-Jun

    2014-01-01

    Recently, an 'outlier' track of radio-X-ray correlation was found, which is much steeper than the former universal correlation, where dual tracks were speculated to be triggered by different accretion processes. In this work, we test this issue by exploring hard X-ray spectral evolution in four black-hole X-ray binaries with multiple, quasi-simultaneous radio and X-ray observations. First, we find that hard X-ray photon indices, Γ, are negatively and positively correlated with X-ray fluxes when the X-ray flux, F 3-9 keV , is below and above a critical flux, F X, crit , which are consistent with predictions of the advection-dominated accretion flow and the disk-corona model, respectively. Second, and most importantly, we find that the radio-X-ray correlations are also clearly different when the X-ray fluxes are higher and lower than the critical flux as defined by X-ray spectral evolution. The data points with F 3-9 keV ≳ F X, crit have a steeper radio-X-ray correlation (F X ∝F R b and b ∼ 1.1-1.4), which roughly forms the ''outlier'' track. However, the data points with anti-correlation of Γ – F 3-9 keV either stay in the universal track with b ∼ 0.61 or stay in the transition track (from the universal to 'outlier' tracks or vice versa). Therefore, our results support that the universal and ''outlier'' tracks of radio-X-ray correlations are regulated by radiatively inefficient and radiatively efficient accretion model, respectively.

  15. In situ analysis of the Zn(S,O) buffer layer preparation for chalcopyrite solar cells by Zn L-edge X-ray absorption spectroscopy.

    Science.gov (United States)

    Lauermann, Iver; Kropp, Timo; Vottier, Damien; Ennaoui, Ahmed; Eberhardt, Wolfgang; Aziz, Emad F

    2009-02-23

    Bridging the gap between high-vacuum soft X-ray absorption spectroscopy and real systems under ambient conditions probes chemical reactions in situ during deposition and annealing processes. The origin of highly efficient buffer layers in Zn(S,O) is the complex formation between Zn(2+) and the S=C group of thiourea (see schematic), which allows ligand-to-metal and metal-to-ligand charge transfer (LMCT and MLCT).

  16. Final Report - X-ray Studies of Highly Correlated Systems

    Energy Technology Data Exchange (ETDEWEB)

    Burns, Clement [Western Michigan Univ., Kalamazoo MI (United States)

    2017-11-27

    The overall goal of the research was to improve the capabilities of x-ray synchrotron instrumentation to enable cutting-edge research in condensed matter physics. The main goal of the current grant cycle was to find a method to measure the polarization of the scattered x-ray in resonant inelastic x-ray scattering. To do this, we developed a polarization analysis apparatus using a thin, toroidally bent single crystal, which could be set to reflect one or the other of the two polarization components in the scattered x-ray beam. Resonant x-ray scattering measurements were also carried out on interfaces and the charge density wave in high temperature superconducting materials.

  17. Higher coherent x-ray laser

    International Nuclear Information System (INIS)

    Hasegawa, Noboru; Nagashima, Keisuke; Kawachi, Tetsuya

    2001-01-01

    X-ray lasers generated by an ultra short pulse laser have advantages such as monochromatic, short pulse duration, small beam divergence, high intensity, and coherence. Spatial coherence is most important for applications, we have investigated the transient collisional excitation (TCE) scheme x-ray laser lasing from Ne-like titanium (31.6 nm), Ne-like silver (13.9 nm) and tin (11.9 nm). However, the spatial coherence was not so good with this scheme. We have been studying to improve the spatial coherence of the x-ray laser and have proposed to use coherent seed light tuned to the x-ray laser wavelength generated from higher harmonics generation (HHG), which is introduced to the x-ray laser medium (Ne-like titanium, Ni-like silver plasmas). We present about the theoretical study of the coupling efficiency HHG light with x-ray laser medium. (author)

  18. X-ray transparent Microfluidics for Protein Crystallization and Biomineralization

    Science.gov (United States)

    Opathalage, Achini

    Protein crystallization demands the fundamental understanding of nucleation and applying techniques to find the optimal conditions to achieve the kinetic pathway for a large and defect free crystal. Classical nucleation theory predicts that the nucleation occurs at high supersaturation conditions. In this dissertation we sought out to develop techniques to attain optimal supersaturation profile to a large defect free crystal and subject it to in-situ X-ray diffraction using microfluidics. We have developed an emulsion-based serial crystallographic technology in nanolitre-sized droplets of protein solution encapsulated in to nucleate one crystal per drop. Diffraction data are measured, one crystal at a time, from a series of room temperature crystals stored on an X-ray semi-transparent microfluidic chip, and a 93% complete data set is obtained by merging single diffraction frames taken from different un-oriented crystals. As proof of concept, the structure of Glucose Isomerase was solved to 2.1 A. We have developed a suite of X-ray semi-transparent micrfluidic devices which enables; controlled evaporation as a method of increasing supersaturation and manipulating the phase space of proteins and small molecules. We exploited the inherently high water permeability of the thin X-ray semi-transparent devices as a mean of increasing the supersaturation by controlling the evaporation. We fabricated the X-ray semi-transparent version of the PhaseChip with a thin PDMS membrane by which the storage and the reservoir layers are separated, and studies the phase transition of amorphous CaCO3.

  19. X-ray Studies of Unidentified Galactic TeV Gamma-ray Sources

    Science.gov (United States)

    Pühlhofer, Gerd

    2009-05-01

    Many of the recently discovered Galactic TeV sources remain unidentified to date. A large fraction of the sources is possibly associated with relic pulsar wind nebula (PWN) systems. One key question here is the maximum energy (beyond TeV) attained in the compact PWNe. Hard X-ray emission can trace those particles, but current non-focussing X-ray instruments above 10 keV have difficulties to deconvolve the hard pulsar spectrum from its surrounding nebula. Some of the new TeV sources are also expected to originate from middle-aged and possibly even from old supernova remnants (SNR). But no compelling case for such an identification has been found yet. In established young TeV-emitting SNRs, X-ray imaging above 10 keV could help to disentangle the leptonic from the hadronic emission component in the TeV shells, if secondary electrons produced in hadronic collisions can be effectively detected. As SNRs get older, the high energy electron component is expected to fade away. This may allow to verify the picture through X-ray spectral evolution of the source population. Starting from the lessons we have learned so far from X-ray follow-up observations of unidentified TeV sources, prospects for Simbol-X to resolve open questions in this field will be discussed.

  20. X-ray Studies of Unidentified Galactic TeV Gamma-ray Sources

    International Nuclear Information System (INIS)

    Puehlhofer, Gerd

    2009-01-01

    Many of the recently discovered Galactic TeV sources remain unidentified to date. A large fraction of the sources is possibly associated with relic pulsar wind nebula (PWN) systems. One key question here is the maximum energy (beyond TeV) attained in the compact PWNe. Hard X-ray emission can trace those particles, but current non-focussing X-ray instruments above 10 keV have difficulties to deconvolve the hard pulsar spectrum from its surrounding nebula.Some of the new TeV sources are also expected to originate from middle-aged and possibly even from old supernova remnants (SNR). But no compelling case for such an identification has been found yet. In established young TeV-emitting SNRs, X-ray imaging above 10 keV could help to disentangle the leptonic from the hadronic emission component in the TeV shells, if secondary electrons produced in hadronic collisions can be effectively detected. As SNRs get older, the high energy electron component is expected to fade away. This may allow to verify the picture through X-ray spectral evolution of the source population.Starting from the lessons we have learned so far from X-ray follow-up observations of unidentified TeV sources, prospects for Simbol-X to resolve open questions in this field will be discussed.

  1. Comparison of x-ray output of inverter-type x-ray equipment

    International Nuclear Information System (INIS)

    Asano, Hiroshi; Miyake, Hiroyuki; Yamamoto, Keiichi

    2000-01-01

    The x-ray output of 54 inverter-type x-ray apparatuses used at 18 institutions was investigated. The reproducibility and linearity of x-ray output and variations among the x-ray equipment were evaluated using the same fluorescence meter. In addition, the x-ray apparatuses were re-measured using the same non-invasive instrument to check for variations in tube voltage, tube current, and irradiation time. The non-invasive instrument was calibrated by simultaneously obtaining measurements with an invasive instrument, employing the tube voltage and current used for the invasive instrument, and the difference was calculated. Reproducibility of x-ray output was satisfactory for all x-ray apparatuses. The coefficient of variation was 0.04 or less for irradiation times of 5 ms or longer. In 84.3% of all x-ray equipment, variation in the linearity of x-ray output was 15% or less for an irradiation time of 5 ms. However, for all the apparatuses, the figure was 50% when irradiation time was the shortest (1 to 3 ms). Variation in x-ray output increased as irradiation time decreased. Variation in x-ray output ranged between 1.8 and 2.5 compared with the maximum and minimum values, excluding those obtained at the shortest irradiation time. The relative standard deviation ranged from ±15.5% to ±21.0%. The largest variation in x-ray output was confirmed in regions irradiated for the shortest time, with smaller variations observed for longer irradiation times. The major factor responsible for variation in x-ray output in regions irradiated for 10 ms or longer, which is a relatively long irradiation time, was variation in tube current. Variation in tube current was slightly greater than 30% at maximum, with an average value of 7% compared with the preset tube current. Variations in x-ray output in regions irradiated for the shortest time were due to photographic effects related to the rise and fall times of the tube voltage waveform. Accordingly, in order to obtain constant x-ray

  2. Chest X-Ray

    Medline Plus

    Full Text Available ... about chest radiography also known as chest x-rays. Chest x-rays are the most commonly performed x-ray exams and use a very small dose of ... of the inside of the chest. A chest x-ray is used to evaluate the lungs, heart and ...

  3. Assessment of a synchrotron X-ray method for quantitative analysis of calcium hydroxide

    International Nuclear Information System (INIS)

    Williams, P. Jason; Biernacki, Joseph J.; Bai Jianming; Rawn, Claudia J.

    2003-01-01

    Thermogravimetric analysis (TGA) and quantitative X-ray diffraction (QXRD) are widely used to determine the calcium hydroxide (CH) content in cementitious systems containing blends of Portland cement, fly ash, blast furnace slag, silica fume and other pozzolanic and hydraulic materials. These techniques, however, are destructive to cement samples and subject to various forms of error. While precise weight losses can be measured by TGA, extracting information from samples with multiple overlapping thermal events is difficult. And, however, while QXRD can offer easier deconvolution, the accuracy for components below about 5 wt.% is typically poor when a laboratory X-ray source is used. Furthermore, the destructive nature of both techniques prevents using them to study the in situ hydration of a single contiguous sample for kinetic analysis. In an attempt to overcome these problems, the present research evaluated the use of synchrotron X-rays for quantitative analysis of CH. A synchrotron X-ray source was used to develop calibration data for quantification of the amount of CH in mixtures with fly ash. These data were compared to conventional laboratory XRD data for like samples. While both methods were found to offer good quantification, synchrotron XRD (SXRD) provided a broader range of detectability and higher accuracy than laboratory diffraction and removed the subjectivity as compared to TGA analysis. Further, the sealed glass capillaries used with the synchrotron source provided a nondestructive closed, in situ environment for tracking hydrating specimens from zero to any desired age

  4. A study on the measurement of effective energy of scattering X-rays

    International Nuclear Information System (INIS)

    Oogama, Noboru; Fujimoto, Nobuhisa; Nishitani, Motohiro; Yamada, Katsuhiko

    1995-01-01

    Only a few studies have been reported on the measurement and evaluation of the effective energy of scattering X-rays using an ionization chamber. The reason for this is due to the difficulty in accurately measuring attenuation curve in scattering X-rays lacking any directional properties. We could come up with a new method for calculating the effective energy of scattering X-rays by utilizing their spectra data. First, for analysing the accuracy of our calculation method with using primary X-rays, a comparison was made of calculated values of the effective energy obtained by our calculation method with the measurement values obtained using an ionization chamber. The results gave the calculated values agreeing with the measurement values within a maximum error of 2%, and this method was very helpful in measuring the effective energy of the scattering X-rays. Consequently, this method was capable of measuring the effective energy of scattering X-rays in the following parameters: X-ray tube voltage, scattering angle and size of scatterer. In conclusion, it is considered that our method could solve the present difficulty regarding the measurement of effective energy of the scattering X-rays, and provided a useful procedure concerning the study of radiation protection. (author)

  5. A hard X-ray study of the ultraluminous X-ray source NGC 5204 X-1 with NuSTAR and XMM-Newton

    DEFF Research Database (Denmark)

    Mukherjee, E. S.; Walton, D. J.; Bachetti, M.

    2015-01-01

    We present the results from coordinated X-ray observations of the ultraluminous X-ray source NGC 5204 X-1 performed by the Nuclear Spectroscopic Telescope Array and XMM-Newton in early 2013. These observations provide the first detection of NGC 5204 X-1 above 10 keV, extending the broadband cover...

  6. In-situ X-ray diffraction : a useful tool to investigate hydride-formation reactions

    NARCIS (Netherlands)

    Notten, P.H.L.; Daams, J.L.C.; Veirman, de A.E.M.; Staals, A.A.

    1994-01-01

    A high-pressure X-ray diffraction (XRD) cell has been designed which allowed us to study simultaneously hydrogen absorption/desorption isotherms and XRD powder diffraction patterns on (de)hydrided intermetallic compounds. The hydride formation reaction was investigated in the case of LaNi5 under

  7. Study of X-rays and nuclear gamma -rays in muonic thallium

    CERN Document Server

    Backe, H; Jahnke, U; Kankeleit, E; Pearce, R M; Petitjean, C; Schellenberg, L; Schneuwly, H; Schröder, W U; Walter, H K; Zehnder, A

    1972-01-01

    Energies and intensities of muonic X-rays, nuclear gamma -rays and mu -capture gamma -rays were measured in natural muonic thallium with Ge (Li) detectors. The absolute intensities of higher mu X-rays were reproduced by a cascade calculation starting with a statistical population at n=20 including K-, L- and M-conversion. The electron screening effect was deduced from energies of higher mu X-rays. Eight prompt nuclear gamma -rays were found. This excitation explains the anomalous intensity ratios of the 2p-1s and 3d-2p fine structure components. From the nuclear gamma -rays of the first excited states were deduced: the magnetic h.f. splittings, muonic isomer shifts E2/M1 mixing ratios and the half-life in the presence of the muon in /sup 205/Tl. Evidence for a magnetic nuclear polarization was found. An isotope shift of Delta E=10.35+or-0.25 keV was measured for the 1s/sub 1/2/ state which is compared with data from optical spectroscopy. From an analysis of the time distribution of delayed gamma -rays from mu...

  8. The effect of water on the stability of iron oxide and iron carbide nanoparticles in hydrogen and syngas followed by in situ X-ray absorption spectroscopy

    NARCIS (Netherlands)

    Thuene, P.C.; Moodley - Gengan, P.; Scheijen, F.J.E.; Fredriksson, H.O.A.; Lancee, R.J.; Kropf, J.; Miller, J.T.; Niemantsverdriet, J.W.

    2012-01-01

    The effect of water on iron-based nanoparticles under hydrogen and syngas was investigated by in situ X-ray absorption spectroscopy. The iron oxide (¿-Fe2O3) nanoparticles, dispersed as a monolayer on flat silica surfaces, were readily converted into metallic iron in dry hydrogen at 350 °C and into

  9. Characterization of Metalloproteins and Biomaterials by X-ray Absorption Spectroscopy and X-ray Diffraction

    DEFF Research Database (Denmark)

    Frankær, Christian Grundahl

    This thesis presents thework on combining complementary X-rays techniques for studying the structures of proteins and other biomaterials, and consists of three different projects: (i) Characterization of protein powders with X-ray powder diffraction (XRPD). (ii) The combination of X-ray...... crystallography and X-ray absorption spectroscopy (XAS) applied to studying different hexameric insulin conformations. (iii) The structures of polymorphs of strontium ranelate and the distribution of strontium in bone tissue. A procedure for fast identification and verification of protein powders using XRPD...... was correction for disordered bulk-solvent, but also correction for background and optimization of unit cell parameters have to be taken into account. A sample holder was designed for collecting powder diffraction data on a standard laboratory X-ray powder diffractometer. The background was reduced by use...

  10. X-Ray Source Heights in a Solar Flare: Thick-Target Versus Thermal Conduction Front Heating

    Science.gov (United States)

    Reep, J. W.; Bradshaw, S. J.; Holman, G. D.

    2016-01-01

    Observations of solar flares with RHESSI have shown X-ray sources traveling along flaring loops, from the corona down to the chromosphere and back up. The 2002 November 28 C1.1 flare, first observed with RHESSI by Sui et al. and quantitatively analyzed by O'Flannagain et al., very clearly shows this behavior. By employing numerical experiments, we use these observations of X-ray source height motions as a constraint to distinguish between heating due to a non-thermal electron beam and in situ energy deposition in the corona. We find that both heating scenarios can reproduce the observed light curves, but our results favor non-thermal heating. In situ heating is inconsistent with the observed X-ray source morphology and always gives a height dispersion with photon energy opposite to what is observed.

  11. Direct analysis of biological samples by total reflection X-ray fluorescence

    International Nuclear Information System (INIS)

    Lue M, Marco P.; Hernandez-Caraballo, Edwin A.

    2004-01-01

    The technique of total reflection X-ray fluorescence (TXRF) is well suited for the direct analysis of biological samples due to the low matrix interferences and simultaneous multi-element nature. Nevertheless, biological organic samples are frequently analysed after digestion procedures. The direct determination of analytes requires shorter analysis time, low reactive consumption and simplifies the whole analysis process. On the other hand, the biological/clinical samples are often available in minimal amounts and routine studies require the analysis of large number of samples. To overcome the difficulties associated with the analysis of organic samples, particularly of solid ones, different procedures of sample preparation and calibration to approach the direct analysis have been evaluated: (1) slurry sampling, (2) Compton peak standardization, (3) in situ microwave digestion, (4) in situ chemical modification and (5) direct analysis with internal standardization. Examples of analytical methods developed by our research group are discussed. Some of them have not been previously published, illustrating alternative strategies for coping with various problems that may be encountered in the direct analysis by total reflection X-ray fluorescence spectrometry

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

    Science.gov (United States)

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

    2008-07-01

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

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

    Energy Technology Data Exchange (ETDEWEB)

    Nakano, S [National Institute for Materials Science, Tsukuba, Ibaraki 305-0044 (Japan); Nakayama, A [Department of Materials Science and Engineering, Meijo University, Nagoya 468-8502 (Japan); Kikegawa, T [Photon Factory (PF), Institute of Materials Structure Science, High Energy Accelerator Research Organization (KEK), Ibaraki 305-0801 (Japan)], E-mail: NAKANO.Satoshi@nims.go.jp

    2008-07-15

    Lithium borohydride (LiBH{sub 4}) was compressed up to 10 GPa using a diamond-anvil-cell to investigate its high-pressure structure. In-situ x-ray diffraction profiles indicated a pressure-induced transformation at 1.1 GPa, which was consistent with the previous experimental observation such as Raman scattering spectroscopy. The high-pressure phase was indexed on a tetragonal symmetry of P4{sub 2}/mmc, which was not corresponding some structural models proposed by previous calculation studies. An unknown substance (presumably another Li-B-H compound), which was contained in the starting material, also transformed into its high-pressure phase at 0.6 GPa without any relation to the transformation of LiBH{sub 4}.

  14. X-ray Micro Tomography as a Tool for Studying Localized Damage / Deformation in Clay Rock

    International Nuclear Information System (INIS)

    Viggiani, Gioacchino; Besuelle, Pierre; Desrues, Jacques

    2013-01-01

    Deformation in geo-materials (soils, rocks, concrete, etc.) is often localized, e.g., in the form of shear bands or fractures. In experimental analysis of the mechanical behavior of such materials, standard laboratory methods are insufficient as the majority of measurements are made at the sample scale and rarely at a local scale. X-ray tomography monitoring during loading allows high-resolution full-field observation of the development of deformation. However, such images only indicate clearly the de-formation when there are significant changes in material density (i.e., volume changes) that produce a change in x-ray absorption. As such 3D Digital Image Correlation (DIC) approaches have been developed that allow quantification of the full strain tensor field throughout the imaged volume. This paper presents results from triaxial compression tests on a clay rock (Callovo-Oxfordian argillite) with in situ synchrotron x-ray micro tomography imaging providing complete 3D images of the specimen at several stages throughout the test. These images have been analyzed using 3D DIC to provide full-field displacement and strain measurements, which allowed the detection of the onset of strain localization and its timing relative to the load peak plus insight into the 3D structure of the localized zone. The paper concludes with a few general remarks concerning the lessons learned from this study and perspectives for current and future work. (authors)

  15. Study of characteristic X-ray source and its applications

    International Nuclear Information System (INIS)

    Li Fuquan

    1994-11-01

    The law of characteristic X-rays emitted by target element under the radiation of isotope source in a range of low energy is discussed. Both the way of improving the rate of γ-X conversion and the method to eliminate the influence of scatter rays are introduced. The influence of the variation of isotopes source, targets and the relative position of source-target to the output of X-rays is also discussed and then the conditions of improving signal-to-noise radio is presented. The X-ray source based on these results can produce different energy X-rays, and so can be broadly used on nuclear instruments and other fields as a low energy source. The thickness gauge, as one of the applications, has succeeded in thickness measuring of the different materials in large range, and it presents a new application field for characteristic X-ray source. (11 figs., 10 tabs.)

  16. X-ray study of bow shocks in runaway stars

    Science.gov (United States)

    De Becker, M.; del Valle, M. V.; Romero, G. E.; Peri, C. S.; Benaglia, P.

    2017-11-01

    Massive runaway stars produce bow shocks through the interaction of their winds with the interstellar medium, with the prospect for particle acceleration by the shocks. These objects are consequently candidates for non-thermal emission. Our aim is to investigate the X-ray emission from these sources. We observed with XMM-Newton a sample of five bow shock runaways, which constitutes a significant improvement of the sample of bow shock runaways studied in X-rays so far. A careful analysis of the data did not reveal any X-ray emission related to the bow shocks. However, X-ray emission from the stars is detected, in agreement with the expected thermal emission from stellar winds. On the basis of background measurements we derive conservative upper limits between 0.3 and 10 keV on the bow shocks emission. Using a simple radiation model, these limits together with radio upper limits allow us to constrain some of the main physical quantities involved in the non-thermal emission processes, such as the magnetic field strength and the amount of incident infrared photons. The reasons likely responsible for the non-detection of non-thermal radiation are discussed. Finally, using energy budget arguments, we investigate the detectability of inverse Compton X-rays in a more extended sample of catalogued runaway star bow shocks. From our analysis we conclude that a clear identification of non-thermal X-rays from massive runaway bow shocks requires one order of magnitude (or higher) sensitivity improvement with respect to present observatories.

  17. In situ X-ray investigations of oxygen precipitation in semiconductor silicon; In-situ-Roentgenuntersuchungen der Sauerstoffpraezipitation in Halbleitersilizium

    Energy Technology Data Exchange (ETDEWEB)

    Grillenberger, Hannes

    2011-03-04

    The precipitation of oxygen in Czochralski grown semiconductor silicon is investigated in situ during thermal treatments up to 1000 C with high energy X-rays. All investigations are performed with a focusing Laue diffractometer. The parameters of the diffraction curve are the relative full width at half maximum (rFHWM) and the enhancement of the integral intensity (EII). A readout software has been developed to extract these automatically from the detector image for the measured 220, -220 and 040 Bragg peaks. The sample thickness is set to 15 mm as this enhances the sensitivity of the method and the samples are processed after the strain-field diffraction (SFD) experiments to wafers for an ex situ characterization demanding wafers. Three experimental series with a total of 21 in situ SFD experiments with different thermal treatments have been performed. The slope of the initial temperature ramp is set to 1 K/min in the first and the third series to generate a high precipitate (Bulk Micro Defect, BMD) density. In the second series the slope is chosen as 10 K/min to generate a lower density in the same silicon material. It is shown with all experiments and with preliminary works that the built up of strain during the heat treatment is caused by BMDs during the high temperature period of the treatment. The detection limit of series 1 is found at 7 nm at a density of 10{sup 13}/cm{sup 3}, of series 2 at 40 nm at a density of 2 x 10{sup 8}/cm{sup 3}, and at 8 nm at a density of 4.8 x 10{sup 12}/cm{sup 3} for series 3. The local maximum of the EII at 450 C, which emerges coincident with a local minimum of the rFWHM in series 2 may be caused by thermal donors (TD). With the experiments is shown that SFD operates in the infrared-laser scattering tomography detection range, but also reaches in a region covered only by transmission electron microscopy (TEM) so far. In contrast to these methods SFD is not limited to low temperatures and in situ experiments can be done. Thus

  18. Wide field X-ray telescopes: Detecting X-ray transients/afterglows related to gamma ray bursts

    International Nuclear Information System (INIS)

    Hudec, Rene; Pina, Ladislav; Inneman, Adolf; Gorenstein, Paul; Rezek, Tomas

    1999-01-01

    The recent discovery of X-ray afterglows of GRBs opens the possibility of analyses of GRBs by their X-ray detections. However, imaging X-ray telescopes in current use mostly have limited field of view. Alternative X-ray optics geometries achieving very large fields of view have been theoretically suggested in the 70ies but not constructed and used so far. We review the geometries and basic properties of the wide-field X-ray optical systems based on one- and two-dimensional lobster-eye geometry and suggest technologies for their development and construction. First results of the development of double replicated X-ray reflecting flats for use in one-dimensional X-ray optics of lobster eye type are presented and discussed. Optimum strategy for locating GRBs upon their X-ray counterparts is also presented and discussed

  19. Analysis of fresco paintings by X-ray fluorescence method

    International Nuclear Information System (INIS)

    Cechak, T.; Gerndt, J.; Musilek, L.; Kopecka, I.

    2000-01-01

    In this work we present the application of X-ray fluorescence analysis (XRFA) to examine fresco paintings from the Karlstejn castle. The X-ray fluorescence apparatus built and operated in the Laboratory of Quantitative Methods in Research of Ancient Monuments was used for the purpose of fresco paintings measurements. The X-ray sources (radionuclides) generate the characteristic X-ray photons from the sample. The Si(Li) detector measures numbers and energies of photons emitted from the specimen. The energy and number of photons detected can be converted into kind and amount of measured atoms. These results give data for qualitative and quantitative analysis of samples. XRFA is relatively simple and non-destructive method. Capability of in-situ measurement is one of big advantages of this method. The radionuclide sources of exciting radiation (e.g. 55 Fe enables the excitation of elements with Z up to 23, 238 Pu is used in interval of Z from 20 to 39 etc.) were used. An Si(Li) semiconductor detector with a 5 l Dewar vessel and portable spectroscopy system enable the in situ measurement. Narrow collimation of the exciting beam makes it possible to select the measured area of fresco painting. The valuable fresco paintings from the Karlstejn castle were investigated in this way. The measurements were carried out in collaboration with the Analytical Laboratory of the State Institute for the Preservation of Historic Monuments. A suitable analysis of paintings makes it possible to detect the kind of colours and evaluate changes in the surface colour of paintings and suggest useful and timely procedures for their conservation and restoration. (author)

  20. X-ray microscopy in Aarhus

    International Nuclear Information System (INIS)

    Uggerhoej, Erik; Abraham-Peskir, Joanna V.

    2000-01-01

    The Aarhus imaging soft X-ray microscope is now a busy multi-user facility. The optical set-up will be described and project highlights discussed. a) Metal-induced structural changes in whole cells in solution. The effects of aluminum, copper, nickel and zinc on protozoa investigated by using a combination of light microscopy, confocal scanning laser microscopy and X-ray microscopy. b) Botanical studies by X-ray microscopy used to compliment electron microscopy studies. c) Sludge morphology and iron precipitation in Danish freshwater plants by combining X-ray, scanning electron and transmission electron microscopy

  1. Facile Low Temperature Hydrothermal Synthesis of BaTiO3 Nanoparticles Studied by In Situ X-ray Diffraction

    Directory of Open Access Journals (Sweden)

    Ola G. Grendal

    2018-06-01

    Full Text Available Ferroelectric materials are crucial for today’s technological society and nanostructured ferroelectric materials are important for the downscaling of devices. Controlled and reproducible synthesis of these materials are, therefore, of immense importance. Hydrothermal synthesis is a well-established synthesis route, with a large parameter space for optimization, but a better understanding of nucleation and growth mechanisms is needed for full utilization and control. Here we use in situ X-ray diffraction to follow the nucleation and growth of BaTiO3 formed by hydrothermal synthesis using two different titanium precursors, an amorphous titania precipitate slurry and a Ti-citric acid complex solution. Sequential Rietveld refinement was used to extract the time dependency of lattice parameters, crystallite size, strain, and atomic displacement parameters. Phase pure BaTiO3 nanoparticles, 10–15 nm in size, were successfully synthesized at different temperatures (100, 125, and 150 °C from both precursors after reaction times, ranging from a few seconds to several hours. The two precursors resulted in phase pure BaTiO3 with similar final crystallite size. Finally, two different growth mechanisms were revealed, where the effect of surfactants present during hydrothermal synthesis is discussed as one of the key parameters.

  2. X-ray bursts observed with JEM-X

    DEFF Research Database (Denmark)

    Brandt, Søren Kristian; Chenevez, Jérôme; Lund, Niels

    2006-01-01

    We report on the search for X-ray bursts in the JEM-X X-ray monitor on INTEGRAL during the first two years of operations. More than 350 bursts from 25 different type-I X-ray burst sources were found.......We report on the search for X-ray bursts in the JEM-X X-ray monitor on INTEGRAL during the first two years of operations. More than 350 bursts from 25 different type-I X-ray burst sources were found....

  3. Intrinsic stress in ZrN thin films: Evaluation of grain boundary contribution from in situ wafer curvature and ex situ x-ray diffraction techniques

    International Nuclear Information System (INIS)

    Koutsokeras, L. E.; Abadias, G.

    2012-01-01

    Low-mobility materials, like transition metal nitrides, usually undergo large residual stress when sputter-deposited as thin films. While the origin of stress development has been an active area of research for high-mobility materials, atomistic processes are less understood for low-mobility systems. In the present work, the contribution of grain boundary to intrinsic stress in reactively magnetron-sputtered ZrN films is evaluated by combining in situ wafer curvature measurements, providing information on the overall biaxial stress, and ex situ x-ray diffraction, giving information on elastic strain (and related stress) inside crystallites. The thermal stress contribution was also determined from the in situ stress evolution during cooling down, after deposition was stopped. The stress data are correlated with variations in film microstructure and growth energetics, in the 0.13-0.42 Pa working pressure range investigated, and discussed based on existing stress models. At low pressure (high energetic bombardment conditions), a large compressive stress is observed due to atomic peening, which induces defects inside crystallites but also promotes incorporation of excess atoms in the grain boundary. Above 0.3-0.4 Pa, the adatom surface mobility is reduced, leading to the build-up of tensile stress resulting from attractive forces between under-dense neighbouring column boundary and possible void formation, while crystallites can still remain under compressive stress.

  4. Stress-dependent crystal structure of lanthanum strontium cobalt ferrite by in situ synchrotron X-ray diffraction

    Science.gov (United States)

    Geiger, Philipp T.; Khansur, Neamul H.; Riess, Kevin; Martin, Alexander; Hinterstein, Manuel; Webber, Kyle G.

    2018-02-01

    Lanthanum strontium cobalt ferrite La1-xSrxCo1-yFeyO3-δ (LSCF) is one of the most studied mixed ionic-electronic conductor materials due to electrical and transport properties, which are attractive for intermediate temperature solid oxide fuel cells (SOFCs), oxygen permeation membranes, and catalysis. The integration of such materials, however, depends on the thermal as well as mechanical behavior. LSCF exhibits nonlinear hysteresis during compressive stress-strain measurements, marked by a remanent strain and coercive stress, i.e., ferroelasticity. However, the origin of ferroelastic behavior has not been investigated under high compressive stress. This study, therefore, investigates the microscopic origin of stress-induced mechanical behavior in polycrystalline (La0.6Sr0.4)0.95Co0.2Fe0.8O3-δ using in situ synchrotron x-ray diffraction. The data presented here reveals that the strain response originates from the intrinsic lattice strain as well as the extrinsic domain switching strain without any apparent change in crystallographic symmetry. A comparison of the calculated microscopic strain contribution with that of a macroscopic measurement indicates a significant change in the relative contributions of intrinsic and extrinsic strain depending on the applied stress state, i.e., under maximum stress and after unloading. Direct evidence of the microscopic origin of stress-strain response outlined in this paper may assist in guiding materials design with the improved mechanical reliability of SOFCs.

  5. Application of X-ray CCD camera in X-ray spot diagnosis of rod-pinch diode

    International Nuclear Information System (INIS)

    Song Yan; Zhou Ming; Song Guzhou; Ma Jiming; Duan Baojun; Han Changcai; Yao Zhiming

    2015-01-01

    The pinhole imaging technique is widely used in the measurement of X-ray spot of rod-pinch diode. The X-ray CCD camera, which was composed of film, fiber optic taper and CCD camera, was employed to replace the imaging system based on scintillator, lens and CCD camera in the diagnosis of X-ray spot. The resolution of the X-ray CCD camera was studied. The resolution is restricted by the film and is 5 lp/mm in the test with Pb resolution chart. The frequency is 1.5 lp/mm when the MTF is 0.5 in the test with edge image. The resolution tests indicate that the X-ray CCD camera can meet the requirement of the diagnosis of X-ray spot whose scale is about 1.5 mm when the pinhole imaging magnification is 0.5. At last, the image of X-ray spot was gained and the restoration was implemented in the diagnosis of X-ray spot of rod-pinch diode. (authors)

  6. X-Ray and Near-Infrared Spectroscopy of Dim X-Ray Point Sources Constituting the Galactic Ridge X-Ray Emission

    Directory of Open Access Journals (Sweden)

    Kumiko Morihana

    2014-12-01

    Full Text Available We present the results of X-ray and Near-Infrared observations of the Galactic Ridge X-ray Emission (GRXE. We extracted 2,002 X-ray point sources in the Chandra Bulge Field (l =0°.113, b = 1°.424 down to ~10-14.8 ergscm-2s-1 in 2-8 keV band with the longest observation (900 ks of the GRXE. Based on X-ray brightness and hardness, we classied the X-ray point sources into three groups: A (hard, B (soft and broad spectrum, and C (soft and peaked spectrum. In order to know populations of the X-ray point sources, we carried out NIR imaging and spectroscopy observation. We identied 11% of X-ray point sources with NIR and extracted NIR spectra for some of them. Based on X-ray and NIR properties, we concluded that non-thermal sources in the group A are mostly active galactic nuclei and the thermal sources are mostly white dwarf binaries such as cataclysmic variables (CVs and Pre-CVs. We concluded that the group B and C sources are X-ray active stars in flare and quiescence, respectively.

  7. Commercial Applications of X Ray Spectrometric Techniques

    International Nuclear Information System (INIS)

    Wegrzynek, D.

    2013-01-01

    In the 21st century, the X-ray fluorescence (XRF) technique is widely used in process control, industrial applications and for routine elemental analysis. The technique has a multielement capability capable of detecting elements with Z ≥ 10, with a few instruments capable of detecting also elements with Z ≥ 5. It is characterized by a non-destructive analysis process and relatively good detection limits, typically one part per million, for a wide range of elements. The first commercial XRF instruments were introduced to the market about 50 years ago. They were the wavelength dispersive X ray fluorescence (WDXRF) spectrometers utilizing Bragg’s law and reflection on crystal lattices for sequential elemental analysis of sample composition. The advances made in radiation detector technology, especially the introduction of semiconductor detectors, improvements in signal processing electronics, availability and exponential growth of personal computer market led to invention of energy dispersive X ray fluorescence (EDXRF) technique. The EDXRF is more cost effective as compared to WDXRF. It also allows for designing compact instruments. Such instruments can be easily tailored to the needs of different customers, integrated with industrial installations, and also miniaturized for the purpose of in-situ applications. The versatility of the technique has been confirmed in a spectacular way by using the XRF and X-ray spectrometric techniques, among few others, during the NASA and ESA missions in search for the evidence of life and presence of water on the surface of Mars. The XRF technique has achieved its strong position within the atomic spectroscopy group of analytical techniques not only due to its versatility but also due to relatively low running costs, as compared to the commonly used methods, e.g., atomic absorption spectrometry (AAS) or inductively coupled plasma atomic emission/mass spectrometry (ICP-AES/MS). Presently, the XRF technique together with X ray

  8. Cone beam x-ray luminescence computed tomography: a feasibility study.

    Science.gov (United States)

    Chen, Dongmei; Zhu, Shouping; Yi, Huangjian; Zhang, Xianghan; Chen, Duofang; Liang, Jimin; Tian, Jie

    2013-03-01

    The appearance of x-ray luminescence computed tomography (XLCT) opens new possibilities to perform molecular imaging by x ray. In the previous XLCT system, the sample was irradiated by a sequence of narrow x-ray beams and the x-ray luminescence was measured by a highly sensitive charge coupled device (CCD) camera. This resulted in a relatively long sampling time and relatively low utilization of the x-ray beam. In this paper, a novel cone beam x-ray luminescence computed tomography strategy is proposed, which can fully utilize the x-ray dose and shorten the scanning time. The imaging model and reconstruction method are described. The validity of the imaging strategy has been studied in this paper. In the cone beam XLCT system, the cone beam x ray was adopted to illuminate the sample and a highly sensitive CCD camera was utilized to acquire luminescent photons emitted from the sample. Photons scattering in biological tissues makes it an ill-posed problem to reconstruct the 3D distribution of the x-ray luminescent sample in the cone beam XLCT. In order to overcome this issue, the authors used the diffusion approximation model to describe the photon propagation in tissues, and employed the sparse regularization method for reconstruction. An incomplete variables truncated conjugate gradient method and permissible region strategy were used for reconstruction. Meanwhile, traditional x-ray CT imaging could also be performed in this system. The x-ray attenuation effect has been considered in their imaging model, which is helpful in improving the reconstruction accuracy. First, simulation experiments with cylinder phantoms were carried out to illustrate the validity of the proposed compensated method. The experimental results showed that the location error of the compensated algorithm was smaller than that of the uncompensated method. The permissible region strategy was applied and reduced the reconstruction error to less than 2 mm. The robustness and stability were then

  9. X-ray diffraction studies of NbTe2 single crystal

    Indian Academy of Sciences (India)

    Unknown

    X-ray (EDAX) and remaining structural characterization was also accomplished by X-ray diffraction (XRD) studies. Lattice parameters, volume and ... The layered structure compound, NbTe2, is one of the typical materials which lead to charge .... financial assistance to carry out this work. References. Brown B E 1966 Acta ...

  10. Bone X-Ray (Radiography)

    Medline Plus

    Full Text Available ... Resources Professions Site Index A-Z X-ray (Radiography) - Bone Bone x-ray uses a very small ... X-ray (Radiography)? What is Bone X-ray (Radiography)? An x-ray (radiograph) is a noninvasive medical ...

  11. Bone X-Ray (Radiography)

    Medline Plus

    Full Text Available ... Professions Site Index A-Z X-ray (Radiography) - Bone Bone x-ray uses a very small dose ... limitations of Bone X-ray (Radiography)? What is Bone X-ray (Radiography)? An x-ray (radiograph) is ...

  12. Bone X-Ray (Radiography)

    Science.gov (United States)

    ... News Physician Resources Professions Site Index A-Z X-ray (Radiography) - Bone Bone x-ray uses a very small ... of Bone X-ray (Radiography)? What is Bone X-ray (Radiography)? An x-ray (radiograph) is a noninvasive ...

  13. Abdomen X-Ray (Radiography)

    Science.gov (United States)

    ... News Physician Resources Professions Site Index A-Z X-ray (Radiography) - Abdomen Abdominal x-ray uses a very small ... of an abdominal x-ray? What is abdominal x-ray? An x-ray (radiograph) is a noninvasive medical ...

  14. CRL X-ray tube

    International Nuclear Information System (INIS)

    Kolchevsky, N.N.; Petrov, P.V.

    2015-01-01

    A novel types of X-ray tubes with refractive lenses are proposed. CRL-R X-ray tube consists of Compound Refractive Lens- CRL and Reflection X-ray tube. CRL acts as X-ray window. CRL-T X-ray consists of CRL and Transmission X-ray tube. CRL acts as target for electron beam. CRL refractive lens acts as filter, collimator, waveguide and focusing lens. Properties and construction of the CRL X-ray tube are discussed. (authors)

  15. A preliminary study of synchrotron light sources for x-ray lithography

    International Nuclear Information System (INIS)

    Hoffmann, C.R.; Bigham, C.B.; Ebrahim, N.A.; Sawicki, J.A.; Taylor, T.

    1989-02-01

    A preliminary study of synchrotron light sources has been made, primarily oriented toward x-ray lithography. X-ray lithography is being pursued vigorously in several countries, with a goal of manufacturing high-density computer chips (0.25 μm feature sizes), and may attain commercial success in the next decade. Many other applications of soft x-rays appear worthy of investigation as well. The study group visited synchrotron radiation facilities and had discussions with members of the synchrotron radiation community, particularly Canadians. It concluded that accelerator technology for a conventional synchrotron light source appropriate for x-ray lithography is well established and is consistent with skills and experience at Chalk River Nuclear Laboratories. Compact superconducting systems are being developed also. Their technical requirements overlap with capabilities at Chalk River. (32 refs)

  16. Studies of oxide-based thin-layered heterostructures by X-ray scattering methods

    Energy Technology Data Exchange (ETDEWEB)

    Durand, O. [Thales Research and Technology France, Route Departementale 128, F-91767 Palaiseau Cedex (France)]. E-mail: olivier.durand@thalesgroup.com; Rogers, D. [Nanovation SARL, 103 bis rue de Versailles 91400 Orsay (France); Universite de Technologie de Troyes, 10-12 rue Marie Curie, 10010 (France); Teherani, F. Hosseini [Nanovation SARL, 103 bis rue de Versailles 91400 Orsay (France); Andrieux, M. [LEMHE, ICMMOCNRS-UMR 8182, Universite d' Orsay, Batiment 410, 91410 Orsay (France); Modreanu, M. [Tyndall National Institute, Lee Maltings, Prospect Row, Cork (Ireland)

    2007-06-04

    Some X-ray scattering methods (X-ray reflectometry and Diffractometry) dedicated to the study of thin-layered heterostructures are presented with a particular focus, for practical purposes, on the description of fast, accurate and robust techniques. The use of X-ray scattering metrology as a routinely working non-destructive testing method, particularly by using procedures simplifying the data-evaluation, is emphasized. The model-independent Fourier-inversion method applied to a reflectivity curve allows a fast determination of the individual layer thicknesses. We demonstrate the capability of this method by reporting X-ray reflectometry study on multilayered oxide structures, even when the number of the layers constitutive of the stack is not known a-priori. Fast Fourier transform-based procedure has also been employed successfully on high resolution X-ray diffraction profiles. A study of the reliability of the integral-breadth methods in diffraction line-broadening analysis applied to thin layers, in order to determine coherent domain sizes, is also reported. Examples from studies of oxides-based thin-layers heterostructures will illustrate these methods. In particular, X-ray scattering studies performed on high-k HfO{sub 2} and SrZrO{sub 3} thin-layers, a (GaAs/AlOx) waveguide, and a ZnO thin-layer are reported.

  17. A filter based analyzer for studies of X-ray Raman scattering

    CERN Document Server

    Seidler, G T

    2001-01-01

    Non-resonant X-ray Raman scattering (XRS) with hard X-rays holds the potential for measuring local structure and local electronic properties around low-Z atoms in environments where traditional soft X-ray techniques are inapplicable. However, the small cross-section for XRS requires that experiments must simultaneously achieve high detection efficiency, large collection solid angles, and good energy resolution. We report here that a simple X-ray analyzer consisting of an absorber and a point-focusing spatial filter can be used to study some X-ray Raman near-edge features. This apparatus has greater than 10% detection efficiency, has an energy resolution of 8 eV, and can be readily extended to collection angles of more than 1 sr. We present preliminary measurements of the XRS from the nitrogen 1 s shell in pyrolitic boron nitride.

  18. In Situ X-ray Diffraction Study of the Formation of Fe(Se,Te) from Various Precursors

    DEFF Research Database (Denmark)

    Grivel, Jean-Claude; Yue, Zhao; Wulff, Anders Christian

    2012-01-01

    The formation of the FeSe0.5Te0.5 phase was studied by means of high energy synchrotron x-ray diffraction. The precursors consisted of Fe, Se and Te or Se0.5Te0.5 powder mixtures and were encased in a metal (Cu/Nb) composite sheath to prevent evaporation of Se and Te during high temperature...... equilibria of the Se – Te system. The grain size of the starting Fe powder has no influence on the reaction path for the grain sizes used in the present study. However, the reaction rate for Fe(Se,Te) formation is clearly sensitive to this parameter....

  19. Bone X-Ray (Radiography)

    Medline Plus

    Full Text Available ... News Physician Resources Professions Site Index A-Z X-ray (Radiography) - Bone Bone x-ray uses a very ... of Bone X-ray (Radiography)? What is Bone X-ray (Radiography)? An x-ray (radiograph) is a noninvasive ...

  20. Bone X-Ray (Radiography)

    Medline Plus

    Full Text Available ... News Physician Resources Professions Site Index A-Z X-ray (Radiography) - Bone Bone x-ray uses a very small ... of Bone X-ray (Radiography)? What is Bone X-ray (Radiography)? An x-ray (radiograph) is a noninvasive ...

  1. Perfect-crystal x-ray optics to treat x-ray coherence

    International Nuclear Information System (INIS)

    Yamazaki, Hiroshi; Ishikawa, Tetsuya

    2007-01-01

    X-ray diffraction of perfect crystals, which serve as x-ray monochromator and collimator, modifies coherence properties of x-ray beams. From the time-dependent Takagi-Taupin equations that x-ray wavefields obey in crystals, the reflected wavefield is formulated as an integral transform of a general incident wavefield with temporal and spatial inhomogeneity. A reformulation of rocking-curve profiles from the field solution of the Takagi-Taupin equations allows experimental evaluation of the mutual coherence function of x-ray beam. The rigorous relationship of the coherence functions between before and after reflection clarifies how the coherence is transferred by a crystal. These results will be beneficial to developers of beamline optics for the next generation synchrotron sources. (author)

  2. Stellar X-ray sources

    International Nuclear Information System (INIS)

    Katz, J.I.; Washington Univ., St. Louis, MO

    1988-01-01

    I Review some of the salient accomplishments of X-rap studies of compact objects. Progress in this field has closely followed the improvement of observational methods, particularly in angular resolution and duration of exposure. Luminous compact X-ray sources are accreting neutron stars or black holes. Accreting neutron stars may have characteristic temporal signatures, but the only way to establish that an X-ray source is a black hole is to measure its mass. A rough phenomenological theory is succesful, but the transport of angular momentum in accretion flows is not onderstood. A number of interesting complications have been observed, including precessing accretion discs, X-ray bursts, and the acceleration of jets in SS433. Many puzzles remain unsolved, including the excitation of disc precession, the nature of the enigmatic A- and gamma-ray source Cyg X-3, the mechanism by which slowly spinning accreting neutron stars lose angular momentum, and the superabundance of X-ray sources in globular clusters. 41 refs.; 5 figs

  3. Interdiffusion in nanometer-scale multilayers investigated by in situ low-angle x-ray diffraction

    Science.gov (United States)

    Wang, Wei-Hua; Bai, Hai Yang; Zhang, Ming; Zhao, J. H.; Zhang, X. Y.; Wang, W. K.

    1999-04-01

    An in situ low-angle x-ray diffraction technique is used to investigate interdiffusion phenomena in various metal-metal and metal-amorphous Si nanometer-scale compositionally modulated multilayers (ML's). The temperature-dependent interdiffusivities are obtained by accurately monitoring the decay of the first-order modulation peak as a function of annealing time. Activation enthalpies and preexponential factors for the interdiffusion in the Fe-Ti, Ag-Bi, Fe-Mo, Mo-Si, Ni-Si, Nb-Si, and Ag-Si ML's are determined. Activation enthalpies and preexponential factors for the interdiffusion in the ML's are very small compared with that in amorphous alloys and crystalline solids. The relation between the atomic-size difference and interdiffusion in the ML's are investigated. The observed interdiffusion characteristics are compared with that in amorphous alloys and crystalline α-Zr, α-Ti, and Si. The experimental results suggest that a collective atomic-jumping mechanism govern the interdiffusion in the ML's, the collective proposal involving 8-15 atoms moving between extended nonequilibrium defects by thermal activation. The role of the interdiffusion in the solid-state reaction in the ML's is also discussed.

  4. In situ time-resolved X-ray near-edge absorption spectroscopy of selenite reduction by siderite

    International Nuclear Information System (INIS)

    Badaut, V.; Schlegel, M.L.; Descostes, M.; Moutiers, G.

    2012-01-01

    The reduction oxidation-reaction between aqueous selenite (SeO 3 2- ) and siderite (FeCO 3 (s)) was monitored by in situ, time-resolved X-ray absorption near-edge structure (XANES) spectroscopy at the selenium K edge in a controlled electrochemical environment. Spectral evolutions showed that more than 60% of selenite was reduced at the siderite surface after 20 h of experiment, at which time the reaction was still incomplete. Fitting of XANES spectra by linear combination of reference spectra showed that selenite reaction with siderite is essentially a two-step process, selenite ions being immobilized on siderite surface prior to their reduction. A kinetic model of the reduction step is proposed, allowing to identify the specific contribution of surface reduction. These results have strong implications for the retention of selenite by corrosion products in nuclear waste repositories and in a larger extent for the fate of selenium in the environment. (authors)

  5. A laboratory-based hard x-ray monochromator for high-resolution x-ray emission spectroscopy and x-ray absorption near edge structure measurements

    Energy Technology Data Exchange (ETDEWEB)

    Seidler, G. T., E-mail: seidler@uw.edu; Mortensen, D. R.; Remesnik, A. J.; Pacold, J. I.; Ball, N. A.; Barry, N.; Styczinski, M.; Hoidn, O. R. [Physics Department, University of Washington, Seattle, Washington 98195-1560 (United States)

    2014-11-15

    We report the development of a laboratory-based Rowland-circle monochromator that incorporates a low power x-ray (bremsstrahlung) tube source, a spherically bent crystal analyzer, and an energy-resolving solid-state detector. This relatively inexpensive, introductory level instrument achieves 1-eV energy resolution for photon energies of ∼5 keV to ∼10 keV while also demonstrating a net efficiency previously seen only in laboratory monochromators having much coarser energy resolution. Despite the use of only a compact, air-cooled 10 W x-ray tube, we find count rates for nonresonant x-ray emission spectroscopy comparable to those achieved at monochromatized spectroscopy beamlines at synchrotron light sources. For x-ray absorption near edge structure, the monochromatized flux is small (due to the use of a low-powered x-ray generator) but still useful for routine transmission-mode studies of concentrated samples. These results indicate that upgrading to a standard commercial high-power line-focused x-ray tube or rotating anode x-ray generator would result in monochromatized fluxes of order 10{sup 6}–10{sup 7} photons/s with no loss in energy resolution. This work establishes core technical capabilities for a rejuvenation of laboratory-based hard x-ray spectroscopies that could have special relevance for contemporary research on catalytic or electrical energy storage systems using transition-metal, lanthanide, or noble-metal active species.

  6. Experimental observation of G banding verifying X-ray workers' chromosome translocation detected by FISH

    International Nuclear Information System (INIS)

    Sun Yuanming; Li Jin; Wang Qin; Tang Weisheng; Wang Zhiquan

    2002-01-01

    Objective: FISH is the most effective way of detecting chromosome aberration and many factors affect its accuracy. G-banding is used to verify the results of early X-ray workers' chromosome translocation examined by FISH. Methods: The chromosome translocations of early X-ray workers have been analysed by FISH (fluorescence in situ hybridization) and G-banding, yields of translocation treated with statistics. Results: The chromosome aberrations frequencies by tow methods are closely related. Conclusion: FISH is a feasible way to analyse chromosome aberrations of X-ray workers and reconstruct dose

  7. X-ray scattering in X-ray fluorescence spectra with X-ray tube excitation - Modelling, experiment, and Monte-Carlo simulation

    International Nuclear Information System (INIS)

    Hodoroaba, V.-D.; Radtke, M.; Vincze, L.; Rackwitz, V.; Reuter, D.

    2010-01-01

    X-ray scattering may contribute significantly to the spectral background of X-ray fluorescence (XRF) spectra. Based on metrological measurements carried out with a scanning electron microscope (SEM) having attached a well characterised X-ray source (polychromatic X-ray tube) and a calibrated energy dispersive X-ray spectrometer (EDS) the accuracy of a physical model for X-ray scattering is systematically evaluated for representative samples. The knowledge of the X-ray spectrometer efficiency, but also of the spectrometer response functions makes it possible to define a physical spectral background of XRF spectra. Background subtraction relying on purely mathematical procedures is state-of-the-art. The results produced by the analytical model are at least as reliable as those obtained by Monte-Carlo simulations, even without considering the very challenging contribution of multiple scattering. Special attention has been paid to Compton broadening. Relevant applications of the implementation of the analytical model presented in this paper are the prediction of the limits of detection for particular cases or the determination of the transmission of X-ray polycapillary lenses.

  8. X-Ray Scattering Applications Using Pulsed X-Ray Sources

    Energy Technology Data Exchange (ETDEWEB)

    Larson, B.C.

    1999-05-23

    Pulsed x-ray sources have been used in transient structural phenomena investigations for over fifty years; however, until the advent of synchrotrons sources and the development of table-top picosecond lasers, general access to ligh temporal resolution x-ray diffraction was relatively limited. Advances in diffraction techniques, sample excitation schemes, and detector systems, in addition to IncEased access to pulsed sources, have ld tO what is now a diverse and growing array of pulsed-source measurement applications. A survey of time-resolved investigations using pulsed x-ray sources is presented and research opportunities using both present and planned pulsed x-ray sources are discussed.

  9. X-ray diagnostic installation for X-ray tomographic images

    International Nuclear Information System (INIS)

    Haendle, J.; Sklebitz, H.

    1984-01-01

    An exemplary embodiment includes at least one x-ray tube for the generation of an x-ray beam, a patient support, an image detector, and a control generator-connected with the x-ray tube and the image detector-for the purpose of moving the x-ray beam, and in opposition thereto, the image field of the image detector. There is connected to the control generator a layer height computer which calculates the enlargement from the geometric data for the tomogram. The image detector has a circuit-connected with the layer height computer-for the purpose of fading-in a marking for the dimensions in the layer plane

  10. Nanoparticle-Assisted Scanning Focusing X-Ray Therapy with Needle Beam X Rays.

    Science.gov (United States)

    Davidson, R Andrew; Guo, Ting

    2016-01-01

    In this work, we show a new therapeutic approach using 40-120 keV X rays to deliver a radiation dose at the isocenter located many centimeters below the skin surface several hundred times greater than at the skin and how this dose enhancement can be augmented with nanomaterials to create several thousand-fold total dose enhancement effect. This novel approach employs a needle X-ray beam directed at the isocenter centimeters deep in the body while continuously scanning the beam to cover a large solid angle without overlapping at the skin. A Monte Carlo method was developed to simulate an X-ray dose delivered to the isocenter filled with X-ray absorbing and catalytic nanoparticles in a water phantom. An experimental apparatus consisting of a moving plastic phantom irradiated with a stationary 1 mm needle X-ray beam was built to test the theoretical predictions. X-ray films were used to characterize the dose profiles of the scanning X-ray apparatus. Through this work, it was determined that the X-ray dose delivered to the isocenter in a treatment voxel (t-voxel) underneath a 5 cm deep high-density polyethylene (HDPE) phantom was 295 ± 48 times greater than the surface dose. This measured value was in good agreement with the theoretical predicted value of 339-fold. Adding X-ray-absorbing nanoparticles, catalytic nanoparticles or both into the t-voxel can further augment the dose enhancement. For example, we predicted that adding 1 weight percentage (wp) of gold into water could increase the effective dose delivered to the target by onefold. Dose enhancement using 1 mm X-ray beam could reach about 1,600-fold in the t-voxel when 7.5 wp of 88 nm diameter silica-covered gold nanoparticles were added, which we showed in a previously published study can create a dose enhancement of 5.5 ± 0.46-fold without scanning focusing enhancement. Based on the experimental data from that study, mixing 0.02 wp 2.5 nm diameter small tetrakis hydroxymethyl phosphonium chloride (THPC

  11. X-ray emission spectroscopy. X-ray fluorescence

    International Nuclear Information System (INIS)

    Despujols, J.

    1992-01-01

    Principles of X-ray emission spectrometry are first recalled, then wave-length dispersive and energy dispersive X-ray fluorescence spectrometer are described. They are essentially designed for qualitative and quantitative analysis of elements (Z>10). Sample preparation, calibration, corrections, interferences, accuracy are reviewed. Examples of use in different industries are given. (71 refs.)

  12. Providing x-rays

    International Nuclear Information System (INIS)

    Mallozzi, P.J.; Epstein, H.M.

    1985-01-01

    This invention provides an apparatus for providing x-rays to an object that may be in an ordinary environment such as air at approximately atmospheric pressure. The apparatus comprises: means (typically a laser beam) for directing energy onto a target to produce x-rays of a selected spectrum and intensity at the target; a fluid-tight enclosure around the target; means for maintaining the pressure in the first enclosure substantially below atmospheric pressure; a fluid-tight second enclosure adjoining the first enclosure, the common wall portion having an opening large enough to permit x-rays to pass through but small enough to allow the pressure reducing means to evacuate gas from the first enclosure at least as fast as it enters through the opening; the second enclosure filled with a gas that is highly transparent to x-rays; the wall of the second enclosure to which the x-rays travel having a portion that is highly transparent to x-rays (usually a beryllium or plastic foil), so that the object to which the x-rays are to be provided may be located outside the second enclosure and adjacent thereto and thus receive the x-rays substantially unimpeded by air or other intervening matter. The apparatus is particularly suited to obtaining EXAFS (extended x-ray fine structure spectroscopy) data on a material

  13. The color of X-rays: Spectral X-ray computed tomography using energy sensitive pixel detectors

    NARCIS (Netherlands)

    Schioppa, E.J.

    2014-01-01

    Energy sensitive X-ray imaging detectors are produced by connecting a semiconductor sensor to a spectroscopic pixel readout chip. In this thesis, the applicability of such detectors to X-ray Computed Tomography (CT) is studied. A prototype Medipix based silicon detector is calibrated using X-ray

  14. Observing Solvation Dynamics with Simultaneous Femtosecond X-ray Emission Spectroscopy and X-ray Scattering

    DEFF Research Database (Denmark)

    Haldrup, Kristoffer; Gawelda, Wojciech; Abela, Rafael

    2016-01-01

    and structural changes, and local solvent structural changes are desired. We have studied the intra- and intermolecular dynamics of a model chromophore, aqueous [Fe(bpy)3]2+, with complementary X-ray tools in a single experiment exploiting intense XFEL radiation as a probe. We monitored the ultrafast structural...... rearrangement of the solute with X-ray emission spectroscopy, thus establishing time zero for the ensuing X-ray diffuse scattering analysis. The simultaneously recorded X-ray diffuse scattering atterns reveal slower subpicosecond dynamics triggered by the intramolecular structural dynamics of the photoexcited...

  15. The use of diagnostic x-ray among veterinarians. Results from a survey et guidance to regulations for veterinarian's use of diagnostic x-ray

    International Nuclear Information System (INIS)

    Solberg, M.

    2010-12-01

    The use of diagnostic X-ray equipment by veterinarians in Norway is regulated by the Radiation Protection Act (Stralevernloven) as well as the Regulation for Radiation Protection and Use of Radiation (Stralevernforskriften). A revised regulation was accepted by the Norwegian government 29/10/2010; revisions relevant to veterinarians will come to force 01/01/2011. Many X-ray machines are used in veterinary clinics in Norway, and the Norwegian Radiation Protection Authority (NRPA) has therefore undertaken a study to assess their use of X-ray equipment. The main objective has been to study occupational exposure to ionizing radiation. This report summarizes data collected during a web-based survey as well as data collected from 13 inspections at veterinary clinics, including in situ measurements of scattered radiation and measurements of compliance between light field and irradiation field at a selection of veterinary clinics. The report also includes guidance to regulations that are specific for the practice of radiology in veterinary medicine. The Norwegian organization for veterinarians (Den Norske Veterinarforening) is gratefully acknowledged for distributing the web-based survey among their members and thereby enabling a large number of responses to be collected. Of 441 completed surveys, 276 (63 %) confirmed that X-ray equipment was used in their clinic. The results from the survey and inspections generally show a good approach and satisfactory daily routines with regard to the use of X-ray machines, especially concerning occupational health aspects. However, nearly 50 % of the respondents were not familiar with the regulations. During the inspection round, certain regulatory requirements were found to be less than satisfactory in most clinics. Such requirements included reporting the use of X-ray machines to the NRPA and the proper use of radiation warning symbols in rooms where X-ray equipment was situated. About 50 % of the veterinary surgeons who used X -ray

  16. Toward Adaptive X-Ray Telescopes

    Science.gov (United States)

    O'Dell, Stephen L.; Atkins, Carolyn; Button, Tim W.; Cotroneo, Vincenzo; Davis, William N.; Doel, Peer; Feldman, Charlotte H.; Freeman, Mark D.; Gubarev, Mikhail V.; Kolodziejczak, Jeffrey J.; hide

    2011-01-01

    Future x-ray observatories will require high-resolution (less than 1 inch) optics with very-large-aperture (greater than 25 square meter) areas. Even with the next generation of heavy-lift launch vehicles, launch-mass constraints and aperture-area requirements will limit the surface areal density of the grazing-incidence mirrors to about 1 kilogram per square meter or less. Achieving sub-arcsecond x-ray imaging with such lightweight mirrors will require excellent mirror surfaces, precise and stable alignment, and exceptional stiffness or deformation compensation. Attaining and maintaining alignment and figure control will likely involve adaptive (in-space adjustable) x-ray optics. In contrast with infrared and visible astronomy, adaptive optics for x-ray astronomy is in its infancy. In the middle of the past decade, two efforts began to advance technologies for adaptive x-ray telescopes: The Generation-X (Gen-X) concept studies in the United States, and the Smart X-ray Optics (SXO) Basic Technology project in the United Kingdom. This paper discusses relevant technological issues and summarizes progress toward adaptive x-ray telescopes.

  17. X-ray detector for a panoramic X-ray unit

    Energy Technology Data Exchange (ETDEWEB)

    Cowell, D; Ensslin, F H

    1976-01-15

    The discovery deals with an X-ray detector suitable for the controlling of panoramic X-ray systems. It consists of a fluorescent image screen and a semiconductor photo cell. The output signal of the detector is proportional to the intensity of the X-radiation and the response time is large enough to follow the change of amplitude of the contours of the modulated X radiation. The detector with band-pass filter regulates, via a control system, the moving rate of the X-ray source and of the film opposite it in dependence of the intensity, so that a uniform exposure is ensured.

  18. Corrosion and Corrosion-Fatigue Behavior of 7075 Aluminum Alloys Studied by In Situ X-Ray Tomography

    Science.gov (United States)

    Stannard, Tyler

    7XXX Aluminum alloys have high strength to weight ratio and low cost. They are used in many critical structural applications including automotive and aerospace components. These applications frequently subject the alloys to static and cyclic loading in service. Additionally, the alloys are often subjected to aggressive corrosive environments such as saltwater spray. These chemical and mechanical exposures have been known to cause premature failure in critical applications. Hence, the microstructural behavior of the alloys under combined chemical attack and mechanical loading must be characterized further. Most studies to date have analyzed the microstructure of the 7XXX alloys using two dimensional (2D) techniques. While 2D studies yield valuable insights about the properties of the alloys, they do not provide sufficiently accurate results because the microstructure is three dimensional and hence its response to external stimuli is also three dimensional (3D). Relevant features of the alloys include the grains, subgrains, intermetallic inclusion particles, and intermetallic precipitate particles. The effects of microstructural features on corrosion pitting and corrosion fatigue of aluminum alloys has primarily been studied using 2D techniques such as scanning electron microscopy (SEM) surface analysis along with post-mortem SEM fracture surface analysis to estimate the corrosion pit size and fatigue crack initiation site. These studies often limited the corrosion-fatigue testing to samples in air or specialized solutions, because samples tested in NaCl solution typically have fracture surfaces covered in corrosion product. Recent technological advancements allow observation of the microstructure, corrosion and crack behavior of aluminum alloys in solution in three dimensions over time (4D). In situ synchrotron X-Ray microtomography was used to analyze the corrosion and cracking behavior of the alloy in four dimensions to elucidate crack initiation at corrosion pits

  19. X-ray fluorescence spectroscopy technology applied to the materials elementary characterization

    International Nuclear Information System (INIS)

    Marambio A, Cristian Gilberto.

    1997-01-01

    A thorough study of the different applications of energy dispersive x-ray fluorescence spectrometry is presented, using different excitation sources and measurement geometries. The adaptation of these systems focuses on the analytical solution for different sample types by studying distinct parameters such as: volume of saturation for liquid samples, inter elemental effects from the matrix and the interferences associated with the measurement reading statistical parameters: as reproducibility, precision and detection limits. The application of the technique using radioisotopic sources gave satisfactory results in the analysis of geologic samples, in analytical control of concentration processes for rare earths and for the manufacturing of fuel elements. In the case of a system with an x-ray generator two measurement geometries were studied: 45 deg geometry and total reflection. There were major results in the analysis of polymer impurities and alloy impurities, aluminums and thin semiconductor films, respectively, after non destructive in situ analysis of the material. The results show that x-ray fluorescence spectrometry is a powerful tool for analysis and process control, with prospects for the solution of analytical problems in the materials area. (author)

  20. Grain-resolved elastic strains in deformed copper measured by three-dimensional X-ray diffraction

    DEFF Research Database (Denmark)

    Oddershede, Jette; Schmidt, Søren; Poulsen, Henning Friis

    2011-01-01

    This X-ray diffraction study reports the grain-resolved elastic strains in about 1000 randomly oriented grains embedded in a polycrystalline copper sample. Diffraction data were collected in situ in the undeformed state and at a plastic strain of 1.5% while the sample was under tensile load...

  1. A Study of the Resolution of Dental Intraoral X-Ray Machines

    International Nuclear Information System (INIS)

    Kim, Seon Ju; Chung, Hyon De

    1990-01-01

    The purpose of this study was to assess the resolution and focal spot size of dental X-ray machines. Fifty dental X-ray machines were selected for measuring resolution and focal spot size. These machines were used in general dental clinics. The time on installation of the X-ray machine varies from 1 years to 10 years. The resolution of these machines was measured with the test pattern. The focal spot size of these machines was measured with the star test pattern. The following results were obtained: 1. The resolution of dental intraoral X-ray machines was not significantly changed in ten years. 2. The focal spot size of dental intraoral X-ray machines was not significantly increased in ten years. The statistical analysis between the mean focal spot size and nominal focal spot size was significant at the 0.05 level about the more than 3 years used machines.

  2. Abdominal x-ray

    Science.gov (United States)

    Abdominal film; X-ray - abdomen; Flat plate; KUB x-ray ... There is low radiation exposure. X-rays are monitored and regulated to provide the minimum amount of radiation exposure needed to produce the image. Most ...

  3. Magnetic x-ray microdiffraction

    Energy Technology Data Exchange (ETDEWEB)

    Evans, Paul G [Computer-Aided Engineering Center, University of Wisconsin, Madison, WI 53706 (United States); Isaacs, Eric D [Center for Nanoscale Materials, Argonne National Laboratory, Argonne, IL 60439 (United States)

    2006-08-07

    Magnetic x-ray microdiffraction uses the structural specificity of x-ray diffraction to probe complex magnetic structures at the length scales relevant to physical phenomena including domain dynamics and phase transitions. Conventional magnetic crystallography techniques such as neutron or x-ray diffraction lack this spatial resolution. The combination of both reciprocal space and real space resolution with a rich magnetic cross section allows new microscopy techniques to be developed and applied to magnetism at the scale of single domains. Potential applications include a wide range of magnetic problems in nanomagnetism, the interaction of strain, polarization and magnetization in complex oxides and spatially resolved studies of magnetic phase transitions. We present the physical basis for x-ray microdiffraction and magnetic scattering processes, review microdiffraction domain imaging techniques in antiferromagnetic and ferromagnetic materials and discuss potential directions for studies. (topical review)

  4. In situ determination of K, Ca, S and Si in fresh sugar cane leaves by handheld Energy Dispersive X-Ray Fluorescence Spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Guerra, Marcelo B.B.; Adame, Andressa; Almeida, Eduardo de; Brasil, Marcos A.S.; Krug, Francisco J., E-mail: fjkrug@cena.usp.br [Centro de Energia Nuclear na Agricultura, Piracicaba, SP (Brazil); Schaefer, Carlos E.G.R. [Departamento de Solos, Universidade Federal de Viçosa, MG (Brazil)

    2018-05-01

    A portable energy dispersive X-ray fluorescence spectrometer was evaluated in the in situ analysis of fresh sugar cane leaves for real time plant nutrition diagnosis. Fresh leaf fragments (n = 10 sugar cane varieties; 20 fragments per leaf; 2 measurement sites per fragment) were irradiated and the averaged data from X-ray characteristic emission lines intensities (for K, Ca, S and Si Kα lines) were in close agreement with mass fraction data obtained by a validated comparative method. The linear correlation coefficients (r) ranged from 0.9575 for Ca to 0.9851 for Si. The obtained limits of detection were at least two-fold lower than the critical nutrient levels. Manganese can also be properly determined, but validation still requires more robust calibration models. The proposed method is a straightforward approach towards the fast evaluation of the nutritional profile of plants avoiding time-consuming steps, which involve drying, grinding, weighing, and acid digestion. (author)

  5. Resonance magnetic x-ray scattering study of erbium

    DEFF Research Database (Denmark)

    Sanyal, M.K.; Gibbs, D.; Bohr, J.

    1994-01-01

    The magnetic phases of erbium have been studied by resonance x-ray-scattering techniques. When the incident x-ray energy is tuned near the L(III) absorption edge, large resonant enhancements of the magnetic scattering are observed above 18 K. We have measured the energy and polarization dependence...... of this magnetic scattering and analyzed it using a simple model based on electric dipole and quadrupole transitions among atomic orbitals. The line shapes can be fitted to a magnetic structure combining both c-axis-modulated and basal-plane components. Below 18 K, we have observed unusual behavior of the magnetic...

  6. X-ray diffraction study of surface-layer structure in parallel grazing rays

    International Nuclear Information System (INIS)

    Shtypulyak, N.I.; Yakimov, I.I.; Litvintsev, V.V.

    1989-01-01

    An x-ray diffraction method is described for study of thin polycrystalline and amorphous films and surface layers in an extremely asymmetrical diffraction system in parallel grazing rays using a DRON-3.0 diffractometer. The minimum grazing angles correspond to diffraction under conditions of total external reflection and a layer depth of ∼ 2.5-8 nm

  7. Magneto x-ray study of a gadolinium-iron amorphous alloy

    International Nuclear Information System (INIS)

    Keller, E.N.

    1985-01-01

    This work reports the measurement of the magnetic x-ray absorption of an amorphous Gd-Fe ferrimagnetic thin film. The Gd to Fe concentration in the sample was 1:4. The magnetic x-ray effect is the x-ray analog of magneto-optic absorption effects. Magneto x-ray effects arise when a solid has different indices of refraction for right and left circularly polarized x-rays. The difference in absorption of left and right circularly polarized x-rays is called the magneto x-ray absorption. This absorption is proportional to the net spin of the final state density of states. At the L3 edge, the main x-ray transition is from initial Gd(2p) core states to final Gd(5d) unoccupied states. Since the 5d states have a net spin polarization in ferromagnetic Gd, this experiment hoped to directly observe how that polarization changes for Gd in the alloy. The magneto x-ray absorption at the Gd L3 edge will be proportional to the sign and amount of the net spin polarization of the 5d electrons. The magnetic x-ray absorption coefficient was found to be at least 0.0005 smaller than the linear absorption coefficient at the Gd white line energy. This was measured for the amorphous alloy at room temperature. Lock-in techniques were used to obtain the small limit to the absorption. A simple model for the size of the magnetic x-ray absorption coefficient in Gd suggests that the Gd(5d) net spin polarization is less than 0.01 Bohr magnetons per atom

  8. Chest X-Ray

    Medline Plus

    Full Text Available ... talk with you about chest radiography also known as chest x-rays. Chest x-rays are the ... treatment for a variety of lung conditions such as pneumonia, emphysema and cancer. A chest x-ray ...

  9. Modern X-ray spectroscopy 3. X-ray fluorescence holography

    International Nuclear Information System (INIS)

    Hayashi, Kouichi

    2008-01-01

    X-ray fluorescence holography (XFH) provides three dimensional atomic images around specified elements. The XFH uses atoms as a wave source or monitor of interference field within a crystal sample, and therefore it can record both intensity and phase of scattered X-rays. Its current performance makes it possible to apply to ultra thin film, impurity and quasicrystal. In this article, I show the theory including solutions for twin image problem, advanced measuring system, data processing for reconstruction of the atomic images and for obtaining accurate atomic positions, applications using resonant X-ray scattering and X-ray excited optical luminescence, and an example of XFH result on the local structure around copper in silicon steal. (author)

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

    Science.gov (United States)

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

    2016-03-01

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

  11. Combined X-ray and Raman Studies on the Effect of Cobalt Additives on the Decomposition of Magnesium Borohydride

    Directory of Open Access Journals (Sweden)

    Olena Zavorotynska

    2015-08-01

    Full Text Available Magnesium borohydride (Mg(BH42 is one of the most promising hydrogen storage materials. Its kinetics of hydrogen desorption, reversibility, and complex reaction pathways during decomposition and rehydrogenation, however, present a challenge, which has been often addressed by using transition metal compounds as additives. In this work the decomposition of Mg(BH42 ball-milled with CoCl2 and CoF2 additives, was studied by means of a combination of several in-situ techniques. Synchrotron X-ray diffraction and Raman spectroscopy were used to follow the phase transitions and decomposition of Mg(BH42. By comparison with pure milled Mg(BH42, the temperature for the γ → ε phase transition in the samples with CoF2 or CoCl2 additives was reduced by 10–45 °C. In-situ Raman measurements showed the formation of a decomposition phase with vibrations at 2513, 2411 and 766 cm−1 in the sample with CoF2. Simultaneous X-ray absorption measurements at the Co K-edge revealed that the additives chemically transformed to other species. CoF2 slowly reacted upon heating till ~290 °C, whereas CoCl2 transformed drastically at ~180 °C.

  12. Development of confocal micro X-ray fluorescence instrument using two X-ray beams

    International Nuclear Information System (INIS)

    Tsuji, Kouichi; Nakano, Kazuhiko; Ding Xunliang

    2007-01-01

    A new confocal micro X-ray fluorescence instrument was developed. This instrument has two independent micro X-ray tubes with Mo targets. A full polycapillary X-ray lens was attached to each X-ray tube. Another half polycapillary lens was attached to a silicon drift X-ray detector (SDD). The focal spots of the three lenses were adjusted to a common position. The effects of the excitation of two X-ray beams were investigated. The instrument enabled highly sensitive three-dimensional X-ray fluorescence analysis. We confirmed that the X-ray fluorescence intensity from the sample increased by applying the two independent X-ray tubes in confocal configuration. Elemental depth profiling of black wheat was demonstrated with the result that each element in the surface coat of a wheat grain showed unique distribution

  13. Overview of the ARGOS X-ray framing camera for Laser MegaJoule

    Energy Technology Data Exchange (ETDEWEB)

    Trosseille, C., E-mail: clement.trosseille@cea.fr; Aubert, D.; Auger, L.; Bazzoli, S.; Brunel, P.; Burillo, M.; Chollet, C.; Jasmin, S.; Maruenda, P.; Moreau, I.; Oudot, G.; Raimbourg, J.; Soullié, G.; Stemmler, P.; Zuber, C. [CEA, DAM, DIF, F-91297 Arpajon (France); Beck, T. [CEA, DEN, CADARACHE, F-13108 St Paul lez Durance (France); Gazave, J. [CEA, DAM, CESTA, F-33116 Le Barp (France)

    2014-11-15

    Commissariat à l’Énergie Atomique et aux Énergies Alternatives has developed the ARGOS X-ray framing camera to perform two-dimensional, high-timing resolution imaging of an imploding target on the French high-power laser facility Laser MegaJoule. The main features of this camera are: a microchannel plate gated X-ray detector, a spring-loaded CCD camera that maintains proximity focus in any orientation, and electronics packages that provide remotely-selectable high-voltages to modify the exposure-time of the camera. These components are integrated into an “air-box” that protects them from the harsh environmental conditions. A miniaturized X-ray generator is also part of the device for in situ self-testing purposes.

  14. X-Ray Study of Variable Gamma-Ray Pulsar PSR J2021+4026

    Science.gov (United States)

    Wang, H. H.; Takata, J.; Hu, C.-P.; Lin, L. C. C.; Zhao, J.

    2018-04-01

    PSR J2021+4026 showed a sudden decrease in the gamma-ray emission at the glitch that occurred around 2011 October 16, and a relaxation of the flux to the pre-glitch state at around 2014 December. We report X-ray analysis results of the data observed by XMM-Newton on 2015 December 20 in the post-relaxation state. To examine any change in the X-ray emission, we compare the properties of the pulse profiles and spectra at the low gamma-ray flux state and at the post-relaxation state. The phase-averaged spectra for both states can be well described by a power-law component plus a blackbody component. The former is dominated by unpulsed emission and probably originated from the pulsar wind nebula as reported by Hui et al. The emission property of the blackbody component is consistent with the emission from the polar cap heated by the back-flow bombardment of the high-energy electrons or positrons that were accelerated in the magnetosphere. We found no significant change in the X-ray emission properties between two states. We suggest that the change of the X-ray luminosity is at an order of ∼4%, which is difficult to measure with the current observations. We model the observed X-ray light curve with the heated polar cap emission, and we speculate that the observed large pulsed fraction is owing to asymmetric magnetospheric structure.

  15. Modern X-ray difraction. X-ray diffractometry for material scientists, physicists, and chemicists

    International Nuclear Information System (INIS)

    Spiess, L.; Schwarzer, R.; Behnken, H.; Teichert, G.

    2005-01-01

    The book yields a comprehensive survey over the applications of X-ray diffraction in fields like material techniques, metallurgy, electrotechniques, machine engineering, as well as micro- and nanotechniques. The necessary fundamental knowledge on X-ray diffraction are mediated foundedly and illustratively. Thereby new techniques and evaluation procedures are presented as well as well known methods. The content: Production and properties of X radiation, diffraction of X radiation, hardware for X-ray diffraction, methods of X-ray diffraction, lattice-constant determination, phase analysis, X-ray profile analysis, crystal structure analysis, X-ray radiographic stress analysis, X-ray radiographic texture analysis, crystal orientation determination, pecularities at thin films, small angle scattering

  16. X-Ray Exam: Pelvis

    Science.gov (United States)

    ... Staying Safe Videos for Educators Search English Español X-Ray Exam: Pelvis KidsHealth / For Parents / X-Ray Exam: ... Ray Exam: Hip Broken Bones Getting an X-ray (Video) X-Ray (Video) View more Partner Message About Us ...

  17. Some considerations on X-ray fluorescence use in museum measurements - The case of medieval silver coins

    International Nuclear Information System (INIS)

    Constantinescu, B.; Bugoi, R.; Oberlaender-Tarnoveanu, E.; Parvan, K.

    2005-01-01

    The purpose of this paper is to give a general layout for the potential applications of Energy-Dispersive X-Ray Fluorescence (ED-XRF) technique for ancient silver coin characterization, using in-situ (in museums) measurements. Examples concerning originality testing, provenance (mines, workshops) identification, counterfeits selection, historical studies (manufacturing technologies, commercial, military and political relationships) are given. Two study cases of medieval coins are described: German brakteaten pfennige and Moldavian groschen. Other analysis methods and their use in the study of medieval coins are illustrated with the example of Particle Induced X-ray Emission (PIXE) technique. (authors)

  18. Extragalactic Hard X-ray Surveys: From INTEGRAL to Simbol-X

    Science.gov (United States)

    Paltani, S.; Dwelly, T.; Walter, R.; McHardy, I. M.; Courvoisier, T. J.-L.

    2009-05-01

    We present some results of the deepest extragalactic survey performed by the INTEGRAL satellite. The fraction of very absorbed AGN is quite large. The sharp decrease in the absorption fraction with X-ray luminosity observed at lower-energy X-rays is not observed. The current lack of truly Compton-thick objects, with an upper limit of 14% to the size of this population, is just compatible with recent modeling of the cosmic X-ray background. We also study the prospects for a future hard X-ray serendipitous survey with Simbol-X. We show that Simbol-X will easily detect a large number of serendipitous AGN, allowing us to study the evolution of AGN up to redshifts about 2, opening the door to the cosmological study of hard X-ray selected AGN, which is barely possible with existing satellites like Swift and INTEGRAL.

  19. X-ray scattering measurements from thin-foil x-ray mirrors

    DEFF Research Database (Denmark)

    Christensen, Finn Erland; BYRNAK, BP; Hornstrup, Allan

    1992-01-01

    Thin foil X-ray mirrors are to be used as the reflecting elements in the telescopes of the X-ray satellites Spectrum-X-Gamma (SRG) and ASTRO-D. High resolution X-ray scattering measurements from the Au coated and dip-lacquered Al foils are presented. These were obtained from SRG mirrors positioned...... in a test quadrant of the telescope structure and from ASTRO-D foils held in a simple fixture. The X-ray data is compared with laser data and other surface structure data such as STM, atomic force microscopy (AFM), TEM, and electron micrography. The data obtained at Cu K-alpha(1), (8.05 keV) from all...

  20. X-ray examination apparatus

    NARCIS (Netherlands)

    2000-01-01

    The invention relates to an X-ray apparatus which includes an adjustable X-ray filter. In order to adjust an intensity profile of the X-ray beam, an X-ray absorbing liquid is transported to filter elements of the X-ray filter. Such transport is susceptible to gravitational forces which lead to an

  1. Development of x-ray laminography under an x-ray microscopic condition

    International Nuclear Information System (INIS)

    Hoshino, Masato; Uesugi, Kentaro; Takeuchi, Akihisa; Suzuki, Yoshio; Yagi, Naoto

    2011-01-01

    An x-ray laminography system under an x-ray microscopic condition was developed to obtain a three-dimensional structure of laterally-extended planar objects which were difficult to observe by x-ray tomography. An x-ray laminography technique was introduced to an x-ray transmission microscope with zone plate optics. Three prototype sample holders were evaluated for x-ray imaging laminography. Layered copper grid sheets were imaged as a laminated sample. Diatomite powder on a silicon nitride membrane was measured to confirm the applicability of this method to non-planar micro-specimens placed on the membrane. The three-dimensional information of diatom shells on the membrane was obtained at a spatial resolution of sub-micron. Images of biological cells on the membrane were also obtained by using a Zernike phase contrast technique.

  2. In situ study on the formation of FeTe

    DEFF Research Database (Denmark)

    Grivel, Jean-Claude; Wulff, Anders Christian; Yue, Zhao

    2011-01-01

    The formation of the FeTe compound from a mixture of Fe and Te powders was studied in situ by means of high-energy synchrotron X-ray diffraction. FeTe does not form directly from the starting elements; instead, FeTe2 forms as an intermediate product. During a 2 °C/min heating ramp, Te first reacts...

  3. Chest X-Ray

    Medline Plus

    Full Text Available ... by Image/Video Gallery Your Radiologist Explains Chest X-ray Transcript Welcome to Radiology Info dot org! Hello, ... you about chest radiography also known as chest x-rays. Chest x-rays are the most commonly performed ...

  4. Small-angle X-ray scattering studies on the X-ray induced aggregation of ribonnuclease, lactate dehydrogenase, glyceraldehyde-3-phosphate dehydrogenase and serum albumin. A comparison with malate synthase

    International Nuclear Information System (INIS)

    Zipper, P.; Gatterer, H.G.; Schutz, J.; Durchschlag, H.

    1980-01-01

    The X-ray induced aggregation of ribonuclease, lactate dehydrogenase (LDH), glyceraldehyde-3-phosphate dehydrogenase (GAPDH) and serum albumin in aqueous solution was monitored in situ by means of small-angle X-ray scattering. Measurements carried out with ribonuclease, LDH and serum albumin in the absence of dithiothreitol (DTT) and with GAPDH in the presence of 0.2mM DTT established the following series for the rates of aggregation of the proteins under these conditions: ribonuclease >LDH> >GAPDH> serum albumin. Within six hours from the beginning of irradiation (i.e. about the time required for the exposure of one complete scattering curve under the conditions of our experiments) the following increases of R tilde resulted: ribonuclease 9%, LDH 7%, GAPDH 4%, serum albumin <1%. Changes of R tilde exceeding 1% are, of course, too high to be tolerated in conventional scattering experiments. Measurements carried out with LDH and GAPDH in the presence of 2mM DTT established a strong protective effect of DTT against the X-ray induced aggregation of these enzymes. The initial increase of R tilde upon irradiation of LDH and GAPDH in the presence of 2mM DTT was found to be even lower than the increase of R tilde observed when serum albumin was irradiated in the absence of DTT. However, the observed decrease of anti x of LDH and GAPDH at the early stages of irradiation suggested the occurrence of fragmentation of the enzymes as another consequence of radiation damage. This finding is discussed in context with the results from previous scattering experiments and electrophoretic studies on malate synthase. (author)

  5. Possibilities and Challenges of Scanning Hard X-ray Spectro-microscopy Techniques in Material Sciences

    Directory of Open Access Journals (Sweden)

    Andrea Somogyi

    2015-06-01

    Full Text Available Scanning hard X-ray spectro-microscopic imaging opens unprecedented possibilities in the study of inhomogeneous samples at different length-scales. It gives insight into the spatial variation of the major and minor components, impurities and dopants of the sample, and their chemical and electronic states at micro- and nano-meter scales. Measuring, modelling and understanding novel properties of laterally confined structures are now attainable. The large penetration depth of hard X-rays (several keV to several 10 keV beam energy makes the study of layered and buried structures possible also in in situ and in operando conditions. The combination of different X-ray analytical techniques complementary to scanning spectro-microscopy, such as X-ray diffraction, X-ray excited optical luminescence, secondary ion mass spectrometry (SIMS and nano-SIMS, provides access to optical characteristics and strain and stress distributions. Complex sample environments (temperature, pressure, controlled atmosphere/vacuum, chemical environment are also possible and were demonstrated, and allow as well the combination with other analysis techniques (Raman spectroscopy, infrared imaging, mechanical tensile devices, etc. on precisely the very same area of the sample. The use of the coherence properties of X-rays from synchrotron sources is triggering emerging experimental imaging approaches with nanometer lateral resolution. New fast analytical possibilities pave the way towards statistically significant studies at multi- length-scales and three dimensional tomographic investigations. This paper gives an overview of these techniques and their recent achievements in the field of material sciences.

  6. Synchrotron-based X-ray microscopic studies for bioeffects of nanomaterials.

    Science.gov (United States)

    Zhu, Ying; Cai, Xiaoqing; Li, Jiang; Zhong, Zengtao; Huang, Qing; Fan, Chunhai

    2014-04-01

    There have been increasing interests in studying biological effects of nanomaterials, which are nevertheless faced up with many challenges due to the nanoscale dimensions and unique chemical properties of nanomaterials. Synchrotron-based X-ray microscopy, an advanced imaging technology with high spatial resolution and excellent elemental specificity, provides a new platform for studying interactions between nanomaterials and living systems. In this article, we review the recent progress of X-ray microscopic studies on bioeffects of nanomaterials in several living systems including cells, model organisms, animals and plants. We aim to provide an overview of the state of the art, and the advantages of using synchrotron-based X-ray microscopy for characterizing in vitro and in vivo behaviors and biodistribution of nanomaterials. We also expect that the use of a combination of new synchrotron techniques should offer unprecedented opportunities for better understanding complex interactions at the nano-biological interface and accounting for unique bioeffects of nanomaterials. Synchrotron-based X-ray microscopy is a non-destructive imaging technique that enables high resolution spatial mapping of metals with elemental level detection methods. This review summarizes the current use and perspectives of this novel technique in studying the biology and tissue interactions of nanomaterials. Copyright © 2014 Elsevier Inc. All rights reserved.

  7. Low energy (soft) x rays

    International Nuclear Information System (INIS)

    Hoshi, Masaharu; Antoku, Shigetoshi; Russell, W.J.; Miller, R.C.; Nakamura, Nori; Mizuno, Masayoshi; Nishio, Shoji.

    1987-05-01

    Dosimetry of low-energy (soft) X rays produced by the SOFTEX Model CMBW-2 was performed using Nuclear Associates Type 30 - 330 PTW, Exradin Type A2, and Shonka-Wyckoff ionization chambers with a Keithley Model 602 electrometer. Thermoluminescent (BeO chip) dosimeters were used with a Harshaw Detector 2000-A and Picoammeter-B readout system. Beam quality measurements were made using aluminum absorbers; exposure rates were assessed by the current of the X-ray tube and by exposure times. Dose distributions were established, and the average factors for non-uniformity were calculated. The means of obtaining accurate absorbed and exposed doses using these methods are discussed. Survival of V79 cells was assessed by irradiating them with soft X rays, 200 kVp X rays, and 60 Co gamma rays. The relative biological effectiveness (RBE) values for soft X rays with 0, 0.2, 0.7 mm added thicknesses of aluminum were 1.6, which were compared to 60 Co. The RBE of 200 kVp X rays relative to 60 Co was 1.3. Results of this study are available for reference in future RERF studies of cell survival. (author)

  8. X-ray diagnostic in gas discharge

    International Nuclear Information System (INIS)

    Chen Suhe; Wang Dalun; Cui Gaoxian; Wang Mei; Fu Yibei; Zhang Xinwei; Zhang Wushou

    1995-01-01

    X rays were observed when the anomalous phenomenon in the metal loaded with deuterium studied by the gas-discharge method. Therefore the X-ray energy spectra were measured by the absorption method, the specific X-ray approach and the NaI scintillation counter, while X-ray intensity was estimated by using 7 Li thermoluminescent foils. The X-ray average energy measured by the absorption method is 27.6 +- 2.1 keV, which is fitted within the error extent to 26.0 +-2.4 keV monoenergetic X rays measured by the NaI scintillation counter

  9. Multiwavelength study of Chandra X-ray sources in the Antennae

    Science.gov (United States)

    Clark, D. M.; Eikenberry, S. S.; Brandl, B. R.; Wilson, J. C.; Carson, J. C.; Henderson, C. P.; Hayward, T. L.; Barry, D. J.; Ptak, A. F.; Colbert, E. J. M.

    2011-01-01

    We use Wide-field InfraRed Camera (WIRC) infrared (IR) images of the Antennae (NGC 4038/4039) together with the extensive catalogue of 120 X-ray point sources to search for counterpart candidates. Using our proven frame-tie technique, we find 38 X-ray sources with IR counterparts, almost doubling the number of IR counterparts to X-ray sources that we first identified. In our photometric analysis, we consider the 35 IR counterparts that are confirmed star clusters. We show that the clusters with X-ray sources tend to be brighter, Ks≈ 16 mag, with (J-Ks) = 1.1 mag. We then use archival Hubble Space Telescope (HST) images of the Antennae to search for optical counterparts to the X-ray point sources. We employ our previous IR-to-X-ray frame-tie as an intermediary to establish a precise optical-to-X-ray frame-tie with <0.6 arcsec rms positional uncertainty. Due to the high optical source density near the X-ray sources, we determine that we cannot reliably identify counterparts. Comparing the HST positions to the 35 identified IR star cluster counterparts, we find optical matches for 27 of these sources. Using Bruzual-Charlot spectral evolutionary models, we find that most clusters associated with an X-ray source are massive, and young, ˜ 106 yr.

  10. In-situ X-ray tomographic study of the morphological changes of a Si/C paper anode for Li-ion batteries

    Science.gov (United States)

    Vanpeene, V.; Etiemble, A.; Bonnin, A.; Maire, E.; Roué, L.

    2017-05-01

    The evolution of the three-dimensional (3D) morphology of a Si-based electrode upon cycling (1st discharge, 1st charge and 2nd discharge) is studied by in-situ synchrotron X-ray tomography. The Si-based electrode is constituted of silicon/carbon black/carboxymethylcellulose (Si/CB/CMC) embedded in a commercial carbon fiber paper, acting as a flexible 3D current collector. Its initial areal discharge capacity is 4.9 mAh cm-2. A reconstructed volume of 293 × 293 × 137 μm3 is analyzed with a resolution of ∼0.3 μm. Three phases are identified: (i) the solid phase (C fibers + Si + CB + CMC), (ii) the electrolyte phase (pores filled with electrolyte) and (iii) the gas phase (electrolyte-free pores). Their respective volume fraction, size distribution and connectivity, and also the dimensional changes of the electrode along the three axes are quantified during cycling. At the beginning of the 1st discharge (lithiation), the formation of gas channels attributed to the reductive electrolyte decomposition is observed. During the 1st charge, large cracks are formed through the electrode, which reclose during the subsequent discharge. The electrode expansion/contraction due to the Si volume change is partially irreversible, occurs mainly in the transverse direction and is much larger in the bottom part of the electrode.

  11. Feasibility study for PTV measurement using x-ray holography

    International Nuclear Information System (INIS)

    Uemura, Tomomasa; Yamamoto, Yasufumi; Murata, Shigeru; Nishio, Shigeru; Iguchi, Manabu; Uesugi, Kentaro

    2005-01-01

    Some X-ray imaging techniques are examined for a feasibility study for micro-PIV in this study. There are three X-ray imaging method, the absorption contrast method, the refraction contrast method, and the phase contrast method. The first one is a common method but its spatial resolution is rather poor. The 2nd method corresponds to the Schlieren method that utilizes refraction of parallel light. The characteristics of the method, edge enhancement, can be effective in extracting tracer images. The third method is a kind of holography methods, and this method can record fine tracer particles. Among the three methods, the second and the third method are seemed to be applicable to PIV imaging, and those methods need a parallel X-ray. The SPring-8, the synchrotron radiation facility in Harima, is utilized. There are some methods to realize phase contrast image, most of them requires ultra-high precision in optical alignment. In the present study, though a coherent source is indispensable, the simplest and robust holography method, the inline holography, is used to take phase contrast pictures. (author)

  12. Basic studies in X-ray radiography and imaging techniques

    International Nuclear Information System (INIS)

    Vaidya, Paresh R.

    2000-01-01

    The aim of this research was to study the basic characteristics related to a new branch of radiography viz. the micro-focal radiography. The most important among them was to find methods of measurement of focal spot size of these X-ray sources. It is important to accomplish this because the design of such units is specifically meant to produce very fine source size. To this end. first the process of radiography test was introduced. Among other things. various properties of an image and image forming systems (like PSF, LSF, MTF etc.) were introduced and explained. Methods used for microfocus measurement of focal spot size in conventional units were reviewed. It was shown how they are not suitable for microfocal tubes. Next the microfocus X-ray unit meant for the study was installed and commissioned. Features which are different from conventional X-ray units were observed more carefully. Data was collected and analyzed for various aspects. Procedure for focussing the electron beam while getting the feed back about beam diameter from the oscilloscope was established by experiments. In addition, influence of change in tube voltage and tube current on the focal spot size was studied. Relationship between tube current and target current vis-a-vis focus size was established. Radiation zone was determined. Focal spot size was qualitatively compared with that of a conventional X-ray unit by taking radiographs of different wire meshes at different magnifications by both the units

  13. X-ray Imaging and preliminary studies of the X-ray self-emission from an innovative plasma-trap based on the Bernstein waves heating mechanism

    Science.gov (United States)

    Caliri, C.; Romano, F. P.; Mascali, D.; Gammino, S.; Musumarra, A.; Castro, G.; Celona, L.; Neri, L.; Altana, C.

    2013-10-01

    Electron Cyclotron Resonance Ion Sources (ECRIS) are based on ECR heated plasmas emitting high fluxes of X-rays. Here we illustrate a pilot study of the X-ray emission from a compact plasma-trap in which an off-resonance microwave-plasma interaction has been attempted, highlighting a possible Bernstein-Waves based heating mechanism. EBWs-heating is obtained via the inner plasma EM-to-ES wave conversion and enables to reach densities much larger than the cut-off ones. At LNS-INFN, an innovative diagnostic technique based on the design of a Pinhole Camera (PHC) coupled to a CCD device for X-ray Imaging of the plasma (XRI) has been developed, in order to integrate X-ray traditional diagnostics (XRS). The complementary use of electrostatic probes measurements and X-ray diagnostics enabled us to gain knowledge about the high energy electrons density and temperature and about the spatial structure of the source. The combination of the experimental data with appropriate modeling of the plasma-source allowed to estimate the X-ray emission intensity in different energy domains (ranging from EUV up to Hard X-rays). The use of ECRIS as X-ray source for multidisciplinary applications, is now a concrete perspective due to the intense fluxes produced by the new plasma heating mechanism.

  14. Microfocussing of synchrotron X-rays using X-ray refractive lens

    Indian Academy of Sciences (India)

    X-ray lenses are fabricated in polymethyl methacrylate using deep X-ray lithography beamline of Indus-2. The focussing performance of these lenses is evaluated using Indus-2 and Diamond Light Source Ltd. The process steps for the fabrication of X-ray lenses and microfocussing at 10 keV at moderate and low emittance ...

  15. Energy dispersive X-Ray fluorescence spectrometric study of ...

    African Journals Online (AJOL)

    Energy dispersive X-Ray fluorescence spectrometric study of compositional differences in trace elements in dried Moringa oleifera leaves grown in two different agro-ecological locations in Ebonyi State, Nigeria.

  16. Polarized X-ray excitation for scatter reduction in X-ray fluorescence computed tomography.

    Science.gov (United States)

    Vernekohl, Don; Tzoumas, Stratis; Zhao, Wei; Xing, Lei

    2018-05-25

    X-ray fluorescence computer tomography (XFCT) is a new molecular imaging modality which uses X-ray excitation to stimulate the emission of fluorescent photons in high atomic number contrast agents. Scatter contamination is one of the main challenges in XFCT imaging which limits the molecular sensitivity. When polarized X-rays are used, it is possible to reduce the scatter contamination significantly by placing detectors perpendicular to the polarization direction. This study quantifies scatter contamination for polarized and unpolarized X-ray excitation and determines the advantages of scatter reduction. The amount of scatter in preclinical XFCT is quantified in Monte Carlo simulations. The fluorescent X-rays are emitted isotropically, while scattered X-rays propagate in polarization direction. The magnitude of scatter contamination is studied in XFCT simulations of a mouse phantom. In this study, the contrast agent gold is examined as an example but a scatter reduction from polarized excitation is also expected for other elements. The scatter reduction capability is examined for different polarization intensities with a monoenergetic X-ray excitation energy of 82 keV. The study evaluates two different geometrical shapes of CZT detectors which are modeled with an energy resolution of 1 keV FWHM at an X-ray energy of 80 keV. Benefits of a detector placement perpendicular to the polarization direction are shown in iterative and analytic image reconstruction including scatter correction. The contrast to noise ratio (CNR) and the normalized mean square error (NMSE) are analyzed and compared for the reconstructed images. A substantial scatter reduction for common detector sizes was achieved for 100% and 80% linear polarization while lower polarization intensities provide a decreased scatter reduction. By placing the detector perpendicular to the polarization direction, a scatter reduction by factor up to 5.5 can be achieved for common detector sizes. The image

  17. PREFACE: Structure and dynamics determined by neutron and x-ray scattering Structure and dynamics determined by neutron and x-ray scattering

    Science.gov (United States)

    Müller-Buschbaum, Peter

    2011-06-01

    Neutron and x-ray scattering have emerged as powerful methods for the determination of structure and dynamics. Driven by emerging new, powerful neutron and synchrotron radiation sources, the continuous development of new instrumentation and novel scattering techniques gives rise to exciting possibilities. For example, in situ observations become possible via a high neutron or x-ray flux at the sample and, as a consequence, morphological transitions with small time constants can be detected. This special issue covers a broad range of different materials from soft to hard condensed matter. Hence, different material classes such as colloids, polymers, alloys, oxides and metals are addressed. The issue is dedicated to the 60th birthday of Professor Winfried Petry, scientific director of the Research Neutron Source Heinz Maier-Leibnitz (FRM-II), Germany, advisor at the physics department for the Bayerische Elite-Akademie, chair person of the Arbeitsgemeinschaft Metall- und Materialphysik of the German Physical Society (DPG) and a member of the professional council of the German Science Foundation (Deutsche Forschungsgemeinschaft, DFG). We would like to acknowledge and thank all contributors for their submissions, which made this special issue possible in the first place. Moreover, we would like to thank the staff at IOP Publishing for helping us with the administrative aspects and for coordinating the refereeing process, and Valeria Lauter for the beautiful cover artwork. Finally, to the readers, we hope that you find this special issue a valuable resource that provides insights into the present possibilities of neutron and x-ray scattering as powerful tools for the investigation of structure and dynamics. Structure and dynamics determined by neutron and x-ray scattering contents In situ studies of mass transport in liquid alloys by means of neutron radiography F Kargl, M Engelhardt, F Yang, H Weis, P Schmakat, B Schillinger, A Griesche and A Meyer Magnetic spin

  18. X-ray detector array

    International Nuclear Information System (INIS)

    Houston, J.M.

    1980-01-01

    The object of the invention (an ionization chamber X-ray detector array for use with high speed computerised tomographic imaging apparatus) is to reduce the time required to produce a tomographic image. The detector array described determines the distribution of X-ray intensities in one or more flat, coplanar X-ray beams. It comprises three flat anode sheets parallel to the X-ray beam, a plurality of rod-like cathodes between the anodes, a detector gas between the electrodes and a means for applying a potential between the electrodes. Each of the X-ray sources is collimated to give a narrow, planar section of X-ray photons. Sets of X-ray sources in the array are pulsed simultaneously to obtain X-ray transmission data for tomographic image reconstruction. (U.K.)

  19. Hydrostatic pressure cells development for X-ray and neutron experiments

    International Nuclear Information System (INIS)

    Passamai Junior, Jose Luis

    2010-01-01

    It was developed and built two pressure cell original models in order to be applied in X-ray elastic scattering (X-ray diffraction), X-ray absorption and neutron scattering experiments (neutron diffraction) under hydrostatic pressure. For the first two experimental cases, where X-ray beam is used, the pressure cell built with two B 4 C anvil mounted in a CuBe body. The B 4 C anvil was prepared at CTA research center in order to present an enhanced X-ray transparence and hardness. The special detail and advantage of the CuBe cell with B 4 C anvil is that this cell can be also used to measure de AC magnetic susceptibility in situ. This special characteristic is highlight as new concept of labeled here as multipurpose pressure cell. A second type of cell pressure was developed in order to be used in neutron elastic scattering experiments, specific in neutron diffraction experiments. The neutron cell pressure was developed using carbon fibers composite to improve the mechanical resistance a cylindrical geometry. The B 4 C pressure cells were available to researches in LNLS. The neutron pressure cell was given to research staff of IPEN Nuclear Reactor. This work show details and draws of these two types of hydrostatic pressure cells. (author)

  20. Fast photoconductor CdTe detectors for synchrotron x-ray studies

    International Nuclear Information System (INIS)

    Yoo, Sung Shik; Faurie, J.P.; Huang Qiang; Rodricks, B.

    1993-09-01

    The Advanced Photon Source will be that brightest source of synchrotron x-rays when it becomes operational in 1996. During normal operation, the ring will be filled with 20 bunches of positrons with an interbunch spacing of 177 ns and a bunch width of 119 ps. To perform experiments with x-rays generated by positrons on these time scales one needs extremely high speed detectors. To achieve the necessary high speed, we are developing MBE-grown CdTe-base photoconductive position sensitive array detectors. The arrays fabricated have 64 pixels with a gap of 100 μm between pixels. The high speed response of the devices was tested using a short pulse laser. X-ray static measurements were performed using an x-ray tube and synchrotron radiation to study the device's response to flux and wavelength changes. This paper presents the response of the devices to some of these tests and discusses different physics aspects to be considered when designing high speed detectors