WorldWideScience

Sample records for situ x-ray investigation

  1. 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.

  2. 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)

  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. 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.

  5. 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....

  6. 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...

  7. 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

  8. 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.

  9. 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...

  10. 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.

  11. 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

  12. 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

  13. 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

  14. 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....

  15. 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.)

  16. 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.

  17. 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.

  18. 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.

  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. 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.

  1. 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.

  2. 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.

  3. 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

  4. 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.

  5. 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

  6. 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.

  7. 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

  8. 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.)

  9. 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...

  10. 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.

  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. 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.

  13. 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

  14. 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.

  15. 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.)

  16. 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.

  17. 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

  18. 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...

  19. 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.

  20. 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.

  1. 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

  2. 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...

  3. 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.

  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. 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.

  6. 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.

  7. X-ray investigations of the hot ISM

    Science.gov (United States)

    Sanders, W. T.

    1993-01-01

    At energies less than one keV, the intensity of the galactic x-ray background dominates that of the extragalactic background in almost every direction on the sky. Below 1/4 keV, the galactic x-ray background has a galactic stellar component, but the dominant emitter seems to be hot interstellar matter. The origin of the general 3/4 keV x-ray background remains uncertain, but one component must also be the contribution from hot interstellar matter. An overview is given of recent x-ray investigations of the hot interstellar medium using data from the ROSAT X-ray Telescope/Position-Sensitive Proportional Counter (XRT/PSPC) instrument. Several prominent features in the low energy x-ray background that are interpreted as fossil supernova remnants are discussed.

  8. 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

    system during charge and discharge. The in situ XRD technique was used by Reimers, Li,and Dahn to study the LiCoO 2 , LiNiO 2 , and LiMn 2 O 4 systems. Their results of these studies have demonstrated that in situ XRD can provide more detailed information about the cathode material structural changes during charge-discharge. Conventional x-ray sources were used in these studies and the beryllium windows were used in the in situ cells. Provisions were made to prevent corrosion of the beryllium windows during charge-discharge. For this reason, the in situ cells were often designed quite differently than a real battery. More seriously, the problem of beryllium corrosion restricted the voltage range of the cell below 4.5 V. This limited the use of this technique to study the effects of overcharge which is very important to the thermal stability of the cathodes. Using the plastic lithium battery technology, Amatucci, Tarascon, and Klein constructed an in situ XRD cell, which allows structural investigations at voltages greater than 5 V without any beryllium window corrosion. However, all of these in situ XRD studies using conventional x-ray sources probe the cell in reflection geometry. Therefore, the observed structural changes are predominantly from the top few microns of the electrode coating, which might not be representative for the whole coating during charge-discharge especially when the rate is high

  9. 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.

  10. 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.

  11. 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

  12. 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

  13. 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

  14. 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.

  15. 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.

  16. 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.

  17. 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.

  18. Experimental investigations of the dosimetric features of x-ray radiation used in x-ray diagnosis

    Energy Technology Data Exchange (ETDEWEB)

    Prostyakova, M A

    1975-10-01

    For radiation hygiene estimates of the extent of the irradiation of various organs and tissues in roentgenological investigations, the quality and quantity of the primary radiation beam and its behaviour in the irradiated medium are assessed. It is shown that the effective energy of x-rays generated at 50-100 kV and with different radiation field dimensions at different depths in a tissue-equivalent irradiated medium is more or less constant, varying within the range 25 to 32 keV. The constancy of effective x-ray energies in a tissue-equivalent medium enables one to use, for different x-ray tube regimes, constant values of the roentgen-rad conversion factor for soft tissue and bone tissue. The investigations confirm the desirability of using high voltages across the x-ray tube in practical x-ray work.

  19. New developments for the investigation of hard X-rays emitted by peeling adhesive tapes.

    Science.gov (United States)

    Krämer, D; Lützenkirchen-Hecht, D; Lühmann, B; Keite-Telgenbüscher, K; Frahm, R

    2013-05-01

    We realized an advanced apparatus for the investigation of emitted X-rays produced by peeling adhesive tape rolls under vacuum conditions. Two stepper motors can unwind and rewind a tape roll, and an additional roller with an optical encoder provides measurement and control of the tape speed. This way reproducible and consecutive experiments are feasible without having to change the tape or break the vacuum. The dependence of the X-ray emission on tape speed, gas pressure, type of adhesive tape, and detector angle has been investigated. The resulting spectra are continuous and span an X-ray energy range of typically 2-60 keV with high intensity. Furthermore, the new apparatus allows the in situ metalization of adhesive tape rolls by a gold sputter source. A significantly increased X-ray emission was observed for adhesive tapes with a metal coating. Thin metal foils have been placed between the tape and the detector, different K- and L-absorption edges could be measured. A considerable enhancement of the emission was achieved under the influence of the magnetic field of an NdFeB permanent magnet.

  20. 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.

  1. 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...

  2. 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.

  3. 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.

  4. 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...

  5. 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.

  6. 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.

  7. 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.

  8. 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)

  9. 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.

  10. 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

  11. 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...

  12. 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.

  13. 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

  14. Investigation of the reversible sodiation of Sn foil by ex-situ X-ray diffractometry and Mössbauer effect spectroscopy

    Energy Technology Data Exchange (ETDEWEB)

    Du, Zhijia [Department of Physics and Atmospheric Science, Dalhousie University, P.O. Box 15000, Halifax, Nova Scotia B3H 4R2 (Canada); Dunlap, R.A. [Department of Physics and Atmospheric Science, Dalhousie University, P.O. Box 15000, Halifax, Nova Scotia B3H 4R2 (Canada); Institute for Research in Materials, Dalhousie University, P.O. Box 15000, Halifax, Nova Scotia B3H 4R2 (Canada); College of Sustainability, Dalhousie University, P.O. Box 15000, Halifax, Nova Scotia B3H 4R2 (Canada); Obrovac, M.N., E-mail: mobrovac@dal.ca [Department of Physics and Atmospheric Science, Dalhousie University, P.O. Box 15000, Halifax, Nova Scotia B3H 4R2 (Canada); Institute for Research in Materials, Dalhousie University, P.O. Box 15000, Halifax, Nova Scotia B3H 4R2 (Canada); Department of Chemistry, Dalhousie University, P.O. Box 15000, Halifax, Nova Scotia B3H 4R2 (Canada)

    2014-12-25

    Highlights: • Mössbauer spectra of all phases formed during sodiation measured for the first time. • Center shifts correlated with metallurgically prepared samples. • Center shift correlated with Na content in Na–Sn. - Abstract: The reversible sodiation of Sn foil was investigated using ex-situ X-ray diffractometry (XRD) and Mössbauer effect spectroscopy. The measured voltage profile indicated that the sodiation process of Sn foil proceeded in three stages. Ex-situ XRD patterns demonstrated that Na{sub 4}Sn{sub 4}, Na{sub 5}Sn{sub 2} and Na{sub 15}Sn{sub 4} phases were formed at the end of each discharge plateau. Na{sub 5}Sn{sub 2}, Na{sub 4}Sn{sub 4} and β-Sn were formed at the end of each charge plateau. Three single-phase alloys, Na{sub 4}Sn{sub 4}, Na{sub 9}Sn{sub 4} and Na{sub 15}Sn{sub 4}, were prepared by annealing stoichiometric ratios of Na and Sn. The Mössbauer spectra of ex-situ samples at the end of each discharge plateau were collected and compared with the Mössbauer spectra of the three single phase alloys. The measured parameters for the Mössbauer effect spectra were consistent with an analysis of the crystal structures. The center shift became less positive with an increase of the sodium content in Na–Sn phases and this was shown to be a useful indicator of the degree of sodiation of Sn electrodes.

  15. 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

  16. 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

  17. 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.

  18. 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.

  19. Thermally stimulated investigations on diamond X-Ray detectors

    International Nuclear Information System (INIS)

    Tromson, D.; Bergonzo, P.; Brambilla, A.; Mer, C.; Foulon, F.; Amosov, V.N.

    1999-01-01

    Intrinsic diamond material is increasingly used for the fabrication of radiation detectors. However, the presence of inherent defects has a strong impact on the detector characteristics such as the time dependent stability of the detection signal. In order to draw better insights into this effect, comparative investigations of the X-ray responses with thermally stimulated current (TSC) measurements were carried out on natural diamond detectors. TSC revealed the presence of four peaks or shoulders on natural samples in the 200 to 500 K domain. Three energy levels were identified at about 0.7, 0.71 and 0.95 eV. Time dependent X-ray detector sensitivity was investigated for various initial conditions. The results give evidence of the improvement of the detection properties after having filled traps in the material by X-ray irradiation. The comparison between the X-ray response and the TSC spectra indicate that trapping levels emptied at room temperature appear to significantly affect the performance of radiation detectors. (authors)

  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. 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...

  2. 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.

  3. Application of X-ray fluorescence in investigation of historical monuments

    International Nuclear Information System (INIS)

    Cechak, Tomas; Trojek, Tomas; Musilek, Ladislav; Paulusova, Hana

    2008-01-01

    Full text: Nuclear techniques represent invaluable tools in non-destructive diagnostics applied to archaeological findings and objects of arts, mainly for dating and determining the composition of materials used in the production of artefacts. In this work we present the application of X-ray fluorescence analysis (XRFA). The X-ray fluorescence apparatus built and operated in the Laboratory of Quantitative Methods in Research of Ancient Monuments, constituent part of the Department of Dosimetry and Application of Ionizing Radiation, FNSPE, was used for the purpose of old relics measurements. The X-ray sources (radionuclides) generate the characteristic X-ray photons from the sample. After processing the resulting signal, we obtain information about the chemical composition of the tested sample. 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.) and X-ray tube with Mo anode were used. Narrow collimation of the exciting beam makes it possible to select the measured area of e.g. pigments in old manuscripts. X-ray fluorescence analysis, both in its energy form and in its wave dispersive form, is one of the most widespread methods using ionising radiation to study the elemental composition of materials. It is frequently used for studies of various cultural and historic relicts and objects of art. This work summarizes the author's experience with X-ray fluorescence analysis in investigating historical relicts namely by means of portable spectroscopic devices. Utilization of these methods is demonstrated in the investigation of fresco paintings, metal objects and old manuscripts. The results of these measurements provide the information on the composition of

  4. 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.

  5. 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

  6. 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...

  7. 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.

  8. 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

  9. 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).

  10. 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

  11. 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.

  12. 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.

  13. 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.

  14. 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.

  15. 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...

  16. 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.

  17. 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.

  18. Investigation on diagnostic techniques of X-ray radiation characteristic from slit target

    International Nuclear Information System (INIS)

    Cheng Jinxiu; Miao Wenyong; Sun Kexu; Wang Hongbin; Cao Leifeng; Yang Jiamin; Chen Zhenglin

    2001-01-01

    On the Xingguang-II facility, X-ray transport process in a cavity target was simulated in a long cylindrical cavity with slits. High temporally and spatially resolved Microchannel Plate (MCP) gated X-ray picosecond frame camera and soft X-ray steak camera were used to investigate the temporal and spatial distribution of the soft X-ray emitted from the cavity wall through the slit. X-ray transport velocity, X-ray emission time and amount of intensity decay was obtained. X-ray CCD pinhole transmission grating spectrometer was used to investigate the spectrum change of the emitted X-ray versus its location. The change characteristic of the spectrum of X-ray absorbed and emitted again and again in transport was obtained. X-ray diodes and Dante spectrometer were used to measure X-ray flux and radiation temperature in the slit, the source and the transport end, respectively. The typical results in the experiment were given. A brief and essential analysis and discussion were made

  19. 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.

  20. 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

  1. 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.

  2. 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.

  3. 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...

  4. 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.

  5. 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...

  6. Accelerators and x-rays in cultural heritage investigations

    International Nuclear Information System (INIS)

    Heinz-Eberhard, Mahnke; Salomon, J.; Heinz-Eberhard, Mahnke; Denker, A.; Heinz-Eberhard, Mahnke

    2009-01-01

    In the following article a review is given on the use of accelerators in studies connected to our cultural heritage. It focuses on making use of the production and detection of x-rays as a general tool. At 'small accelerators', the proton induced x-ray emission (PIXE), especially when combined with Rutherford backscattering spectroscopy (RBS), has been developed to a very versatile and powerful technique for near-surface investigations. It is well complemented by larger facilities, synchrotron radiation sources as well as medium energy ion accelerators for high energy PIXE. With the development of small compact electron accelerators, a new generation of mono-energetic high-energy high-intensity x-ray sources will add a very comfortable complement in cultural heritage studies

  7. 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

  8. 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

  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. Thermal behaviour of molecular sieves (SAPO-11/AIPO-11 type) investigated by synchrotron radiation X-ray diffraction (SRXD)

    International Nuclear Information System (INIS)

    Neissendorfer, F.; Jahn, E.; Gusenko, S.N.; Sheromov, M.A.

    1991-01-01

    The structure of molecular sieves is important for a successful application as a catalyzer. The final structure of the synthetic product depends on the technological steps. This process was investigated by in-situ Synchrotron radiation X-ray diffraction. Structural changes in the molecular sieves exist not only during the heating process but also during the following cooling process. (author) 3 figs., 2 refs

  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. 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.

  13. Combining x-ray diffraction contrast tomography and mesoscale grain growth simulations in strontium titanate: An integrated approach for the investigation of microstructure evolution

    DEFF Research Database (Denmark)

    Syha, Melanie; Baürer, Michael; Rheinheimer, Wolfgang

    2013-01-01

    Motivated by the recently reported a growth anomaly in strontium titatate bulk samples1, the microstructure of bulk strontium titanate has been investigated by an integrated approach comprising conventional metallography, three dimensional X-ray diffraction contrast tomography (DCT)2, and the obs......Motivated by the recently reported a growth anomaly in strontium titatate bulk samples1, the microstructure of bulk strontium titanate has been investigated by an integrated approach comprising conventional metallography, three dimensional X-ray diffraction contrast tomography (DCT)2......, and the observation of pore shapes in combination with mesoscale grain growth simulations. The microstructural evolution in strontium titanate has been characterized alternating ex-situ annealing and high energy X-ray DCT measurements, resulting in three dimensional microstructure reconstructions which...

  14. 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.

  15. 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.

  16. In situ investigation of the surface silvering of late Roman coins by combined use of high energy broad-beam and low energy micro-beam X-ray fluorescence techniques

    Energy Technology Data Exchange (ETDEWEB)

    Romano, F.P., E-mail: romanop@lns.infn.it [IBAM, CNR, Via Biblioteca 4, 95124 Catania (Italy); LNS, INFN, Via S. Sofia 62, 95123 Catania (Italy); Garraffo, S. [ITABC, CNR, Via Salaria km 29.300, 00016 Monterotondo, Roma (Italy); Pappalardo, L. [IBAM, CNR, Via Biblioteca 4, 95124 Catania (Italy); LNS, INFN, Via S. Sofia 62, 95123 Catania (Italy); Rizzo, F. [LNS, INFN, Via S. Sofia 62, 95123 Catania (Italy); Dipartimento di Fisica e Astronomia, Universita di Catania, Via S. Sofia 64, 95123 Catania (Italy)

    2012-07-15

    The compositional analysis of archeological metals performed with the X-ray Fluorescence technique (XRF) provides information on the ancient technology. One of the most interesting case-study concerns the techniques used by Romans for silvering the surface of coins. Different metallurgical processes have been suggested in previous studies. Recently the investigation has been addressed to the mercury-silvering and to its possible use in the mass-production of coins minted during the late period (after 294 AD). In the present paper the non-destructive investigation of the silvering process used for manufacturing the Roman nummi - the important typology of coin introduced by Diocletian in his monetary reform - is approached by the combined use of the standard X-Ray Fluorescence (XRF) and the low energy micro-X-Ray Fluorescence (LE-{mu}XRF) portable methods. The research was focused on the systematic determination of the mercury presence in a large number of samples and on its correlation with silver in the surface of the coins. 1041 Roman nummi belonging to the Misurata Treasure were analyzed in situ, at the Leptis Magna Museum (Al Khums, Libya). The treasure, composed of about 108 thousand silvered coins, gives the unique opportunity to study the Roman coinage in a wide interval of time (about 40 years in the period 294-333 AD) and in almost all the imperial mints operating in the Roman world. - Highlights: Black-Right-Pointing-Pointer Custom-building of a high energy broad-beam and a low energy micro-beam XRF Black-Right-Pointing-Pointer In situ analysis of the silvering methods in late Roman nummi with plated surfaces Black-Right-Pointing-Pointer The broad-beam XRF was applied for the detection of mercury traces in the coin alloy. Black-Right-Pointing-Pointer The low energy micro-XRF was used to scan the surface patina of the coins. Black-Right-Pointing-Pointer The correlation between mercury and silver at the coin surface was evidenced.

  17. 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.

  18. Bone structure investigation using X-ray and neutron radiography techniques

    International Nuclear Information System (INIS)

    Kamali Moghaddam, K.; Taheri, T.; Ayubian, M.

    2008-01-01

    In this paper we report a study of the periodic variation of bone tissue humidity immediately after death using both neutron and X-ray radiography techniques. After death, bone tissue experiences sequential change over time. This change consists of organic and inorganic phase variations of the bone structure, as well as gradual reduction of the bone's water content. These variations are investigated by periodically imaging dead bone using X-ray and neutron radiography. Chemical separation techniques such as calcification and decalcification were used to separate the organic and inorganic phases of the bone. Comparison between X-ray and neutron radiographs of bone following phase separation can be potentially used to investigate the bone disease or to determine a cause of death. In our experiments, we use adult rat femur bones, and the interpretations of these results are presented based on our understanding of bone structure and images produced by neutron and X-ray photon interactions

  19. Bone structure investigation using X-ray and neutron radiography techniques

    Energy Technology Data Exchange (ETDEWEB)

    Kamali Moghaddam, K. [Nuclear Research Center (NRC), Atomic Energy Organization of Iran (AEOI), P.O. Box 11365-8486, Tehran (Iran, Islamic Republic of)], E-mail: kkamali@aeoi.org.ir; Taheri, T.; Ayubian, M. [Nuclear Research Center (NRC), Atomic Energy Organization of Iran (AEOI), P.O. Box 11365-8486, Tehran (Iran, Islamic Republic of)

    2008-01-15

    In this paper we report a study of the periodic variation of bone tissue humidity immediately after death using both neutron and X-ray radiography techniques. After death, bone tissue experiences sequential change over time. This change consists of organic and inorganic phase variations of the bone structure, as well as gradual reduction of the bone's water content. These variations are investigated by periodically imaging dead bone using X-ray and neutron radiography. Chemical separation techniques such as calcification and decalcification were used to separate the organic and inorganic phases of the bone. Comparison between X-ray and neutron radiographs of bone following phase separation can be potentially used to investigate the bone disease or to determine a cause of death. In our experiments, we use adult rat femur bones, and the interpretations of these results are presented based on our understanding of bone structure and images produced by neutron and X-ray photon interactions.

  20. 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

  1. 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.

  2. 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.

  3. 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

  4. X-ray investigations in intensive care units

    Energy Technology Data Exchange (ETDEWEB)

    Pokieser, H.

    1981-10-01

    From special care following surgery and from arteficial respiration of polio patients the modern and very special intensive medical care has developed. At the same time the provisional bedside radiology was improved to one branch of clinical radiology with special organisation and methods of investigation. Importance and urgency of radiological information are requiring close cooperation of all medical branches. Functions of these different groups have to be defined. The movable X-ray apparatus of 20 kV output is necessary for every intensive care unit. Hard beam technique for lung X-rays, scattered radiation grids and adequate positioning of the patient are important to get the same high quality pictures than from the radiological department.

  5. X-ray investigations in intensive care units

    International Nuclear Information System (INIS)

    Pokieser, H.

    1981-01-01

    From special care following surgery and from arteficial respiration of polio patients the modern and very special intensive medical care has developed. At the same time the provisional bedside radiology was improved to one branch of clinical radiology with special organisation and methods of investigation. Importance and urgency of radiological information are requiring close cooperation of all medical branches. Functions of these different groups have to be defined. The movable X-ray apparatus of 20 kV output is necessary for every intensive care unit. Hard beam technique for lung X-rays, scattered radiation grids and adequate positioning of the patient are important to get the same high quality pictures than from the radiological department. (orig.) [de

  6. 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.

  7. 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.

  8. 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.

  9. 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...

  10. 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)

  11. 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.

  12. 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}).

  13. Structural investigation of GaInP nanowires using X-ray diffraction

    DEFF Research Database (Denmark)

    Kriegner, D.; Persson, Johan Mikael; Etzelstorfer, T.

    2013-01-01

    In this work the structure of ternary GaxIn1−xP nanowires is investigated with respect to the chemical composition and homogeneity. The nanowires were grown by metal–organic vapor-phase epitaxy. For the investigation of ensemble fluctuations on several lateral length scales, X-ray diffraction...... gradients along the sample by recording diffraction patterns at different positions. In addition, compositional variations were found also within single nanowires in X-ray energy dispersive spectroscopy measurements....

  14. Investigations of time resolved x-ray wide-angle scattering and x-ray small-angle scattering at DESY

    International Nuclear Information System (INIS)

    Zachmann, H.G.; Gehrke, R.; Prieske, W.; Riekel, C.

    1985-01-01

    Instrumentation is described for the simultaneous wide-angle and small-angle x-ray scattering. The method was applied to the study of the isothermal crystallization of polyethylene terephthalates. In agreement with the classical theories of crystallization, the data showed that the density difference between the crystals and the non-crystalline regions does not change with time. The mechanisms of melting, recrystallization, and crystal thickening were investigated by small-angle x-ray scattering with stepwise changes and continuous changes of temperature using polyethylene terephthalate

  15. 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...

  16. 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.

  17. 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.

  18. 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

  19. 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.

  20. 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

  1. 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.

  2. 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

  3. 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.

  4. 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

  5. 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.

  6. 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.

  7. 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....

  8. Structural Investigation of Sodium Layered Oxides Via in Situ Synchrotron X-Ray Diffraction

    DEFF Research Database (Denmark)

    Jung, Young Hwa; Christiansen, Ane Sælland; Johnsen, Rune

    2015-01-01

    electrochemical reaction is generally considered to be a pivotal feature for understanding the relationship between layered structures and electrochemical properties. Here the structure, phase stability, and electrochemical properties of two kinds of layered oxides, P2 and O3, are investigated through in......-situ synchrotron XRD experiments. A capillary Na-based cell is designed to minimize interference in other substances such as a separator or external battery parts. This approach could give us to obtain clear diffraction patterns with high intensity during electrochemical reaction in a short period of time without...... further relaxation step. We carefully scrutinized reversible structural phase transformations during electrochemical reaction of P2 and O3-layered compounds based on in situ analysis, and detailed results will be discussed....

  9. A quasi-monochromatic X-rays source for art painting pigments investigation

    Energy Technology Data Exchange (ETDEWEB)

    Albertin, F.; Franconieri, A.; Gambaccini, M.; Petrucci, F.; Chiozzi, S. [University of Ferrara, Department of Physics and INFN, Ferrara (Italy); Moro, D. [University of Padova, Department of Physics, Padova (Italy); LNL - INFN, Legnaro, Padova (Italy)

    2009-08-15

    Monochromatic X-ray sources can be used for several applications, like in medicine or in studying our cultural heritage. We are investigating imaging systems based on a tuneable energy band X-ray source, to obtain an element mapping of painting layers using the K-edge technique. The narrow energy band beams are obtained with conventional X-ray source via Bragg diffraction on a mosaic crystal; such an analysis has been performed at different diffraction angles, tuning the energy to investigate spectra of interest from the artistic point of view, like zinc and copper. In this paper the characteristics of the system in terms of fluence rate are reported, and first results of this technique on canvas samples and painting are presented. (orig.)

  10. 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

  11. X-Ray diffraction Investigation of Electrochemically Deposited Copper

    DEFF Research Database (Denmark)

    Pantleon, Karen; Jensen, Jens Dahl; Somers, Marcel A.J.

    2004-01-01

    by the determination of X-ray diffraction (XRD) pole figures and the calculation of the orientation distribution functions. XRD results are discussed in relation to the morphologies of the electrodeposits as investigated with light optical microscopy and correlated with the process parameters during electrodeposition....

  12. 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

  13. 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).

  14. 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.

  15. Investigation of Pink Tourmalines by X-ray Fluorescent Technique

    International Nuclear Information System (INIS)

    Sangariyavanich, A.; Na Songkhla, S.; Pimjum, S.

    1998-01-01

    X-ray fluorescent technique has been employed in the study of trace elements in six samples of gamma irradiated pink tourmalines, namely, red-pink (rubellite), light-pink, orange-pink, brownish orange-pink, purple red and purple orange-pink. The analysis of their characteristic X-ray indicated the existence of manganese in all samples. Trace amounts of iron, zinc, lead, bismuth or gallium were also investigated in certain samples. Since these elements were not present in red-pink tourmaline, therefore, we believed that manganese is the major cause of pink color in tourmaline while other elements produce various types of pink color

  16. X-ray electron investigation of technetium compounds

    International Nuclear Information System (INIS)

    Gerasimov, V.N.; Kryuchkov, S.V.; Kuzina, A.F.; Kulakov, V.M.; Pirozhkov, S.V.; Spitsyn, V.I.; Gosudarstvennyj Komitet po Ispol'zovaniyu Atomnoj Ehnergii SSSR, Moscow. Inst. Atomnoj Ehnergii)

    1982-01-01

    Investigation results of a number of technetium compounds using the method of X-ray electron spectroscopy have been presented for the first time. Calculation of effective charge for compounds without Tc-Tc bond and cluster complexes with strong Tc-Tc bond is made. Strong interdependence of effective charge and properties of technetium clusters is shown. Binding energies for certain cluster complexes of technetium with halides are given

  17. Monte Carlo Investigation of Phosphor Screens for X-ray Imaging

    International Nuclear Information System (INIS)

    Lim, Chang Hwy; Cheong, Min Ho; Cho, Min Kook; Shon, Choel Soon; Kim, Ho Kyung

    2006-01-01

    In order to detect X rays with pixel detectors, there are two technical methods; a direct detection using photoconductive material that permits the conversion of the incident X rays into the signal charges, and an indirect detection using scintillation material that converts the incident X rays into the optical photons. Therefore, two-dimensional (2D) photosensitive pixel array is necessary for the indirect-detection scheme. Terbium-doped gadolinium oxysulfide (Gd 2 O 2 S:Tb) phosphor screen is the most popular X-ray converter, and often employed to the digital radiographic system owing to its well-known technology and easy handling in size, thickness, and flexibility. Furthermore, the cost is effective. In cascaded imaging chains of the indirect-detection system, the phosphor screen is served as the first stage. Since the image signal-to-noise ratio (SNR) is irreversible through the cascaded system, the phosphor screen is largely responsible for the eventual image quality. For the various radiation qualities suggested by IEC (International Electrotechnical Commission, Report 1267), we have investigated important physical quantities of Gd 2 O 2 S:Tb screen with a wide range of coverages (34 . 135 mg/cm 2 ) by using Monte Carlo calculations. The results will be useful for the optimal design of digital X-ray imaging systems

  18. 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.

  19. 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

  20. 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

  1. 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...

  2. 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.

  3. 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.

  4. 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

  5. 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

    For decades the optimization of polycrystalline absorbers has been done using an Edisonian approach, where trial and error and complex design of experiments in large parameter spaces have driven efficiencies to the record values we see today – CIGS at 22.5%, 22.1% for CdTe, 21.3% for high purity multi-crystalline silicon. Appropriate growth parameters are critical to ensure good quality crystals with low concentration of structural defects - low dislocation density and large grain sizes. However, to bridge the gap between the efficiencies today and the fundamental Shockley-Queisser limit for these materials a much more fundamental understanding of the role and interaction between composition, structure, defect density and electrical properties is required. In recent years multiple novel characterization techniques have shown the potential that nanoscale characterization can have in deciphering the composition of grain boundaries in materials like CIGS and CdTe. However, high resolution has come at the cost of small sampling areas and number of specimens, making it extremely difficult to draw conclusions based on the characteristic small sampling sizes. The missing links thus far have been: (1) the lack of statistical meaningfulness of the nanosclae studies and (2) the direct correlation of compositional variations to electrical performance with nanoscale resolution. In this work we present the use of synchrotron-based nano-X-ray fluorescence microscopy (nano-XRF), x-ray absorption nanospectroscopy (nano-XAS) coupled with nano-x-ray beam induced current (nano-XBIC) as ideal tools for investigating elemental, chemical and electrical properties of large areas of solar cell materials at the sub-micron scale with very high sensitivity. We show how the technique can provide statistical valuable information regarding the elemental segregation in CIGS and the direct correlation to current collection. For example, we demonstrate that Cu and Ga (and with that, CGI and GGI

  6. 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.

  7. 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

  8. Repeated sorption of water in SBA-15 investigated by means of in situ small-angle x-ray scattering

    International Nuclear Information System (INIS)

    Erko, M; Paris, O; Wallacher, D; Findenegg, G H

    2012-01-01

    The effect of repeated cycles of water adsorption/desorption on the structural stability of ordered mesoporous silica SBA-15 is studied by small-angle x-ray scattering (SAXS). In situ sorption measurements are conducted using a custom-built sorption apparatus in connection with a laboratory SAXS setup. Two striking irreversible changes are observed in the sorption isotherms as derived from the integrated SAXS intensity. First, the capillary condensation pressure shifts progressively to lower relative pressure values with increasing number of sorption cycles. This effect is attributed to chemisorption of water at the silica walls, resulting in a change of the fluid-wall interaction. Second, the sorption cycles do not close completely at vanishing vapour pressure, suggesting that progressively more water remains trapped within the porous material after each cycle. This effect is interpreted to be the result of an irreversible collapse of parts of mesopores, originating from pore wall deformation due to the large Laplace pressure of water acting on the pore walls at capillary condensation and capillary evaporation. (paper)

  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 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.

  11. 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.

  12. 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.

  13. X-rays Provide a New Way to Investigate Exploding Stars

    Science.gov (United States)

    2007-05-01

    exhausted. The duration of this X-ray emission traces the amount of material left on the white dwarf after the nova explosion. Optical Image of Andromeda Galaxy (M31) Optical Image of Andromeda Galaxy (M31) A well determined start time of the optical nova outburst and the X-ray turn-on and turn-off times are therefore important benchmarks for replication in computer models of novae. Whilst monitoring the M31 novae, frequently over several months, for the appearance and subsequent disappearance of the X-rays, Pietsch made an important discovery. Some novae start to emit X-rays and then turn them off again within just a few months. "These novae are a new class. They would have been overlooked before," says Pietsch. That's because previous surveys looked only every six months or so. Within that time, the fast X-ray novae could have blinked both on and off. In addition to discovering the short-lived ones, the new survey also confirms that other novae generate X-rays over a much longer time. XMM-Newton detected seven novae that were still shining X-rays into space, up to a decade after the original eruption. The differing lengths of times are thought to reflect the masses of the white dwarfs at the heart of the nova explosion. The fastest evolving novae are thought to be those coming from the most massive white dwarfs. To investigate further, the team have been awarded more XMM-Newton and Chandra observing time. They now plan to monitor M31's novae every ten days for several months, starting in November 2007 to glean more information about these puzzling stellar explosions. Notes for editors: X-ray monitoring of optical novae in M31 from July 2004 to February 2005 by W. Pietsch et al. is published in Astronomy and Astrophysics, 465, 375-392 (2007). For more information: Wolfgang Pietsch wnp@mpe.mpg.de Norbert Schartel Norbert.Schartel@sciops.esa.int

  14. In situ investigation of catalysts for alcohol synthesis

    DEFF Research Database (Denmark)

    Duchstein, Linus Daniel Leonhard; Sharafutdinov, Irek; Wu, Qiongxiao

    consists of three complimentary in situ techniques: (1) Activity measurements based on a reactor connected to a gas chromatograph (GC), (2) In situ x-ray diffractometer (XRD) measurements based on a reactor cell connected to a mass spectrometer (MS), and (3) environmental TEM (ETEM) that allows...... distribution, measured both macroscopically (XRD) and microscopically (ETEM), with the catalytic activity....

  15. 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)

  16. 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

  17. 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.

  18. 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...

  19. Investigation of HF-plasma-treated soft x-ray optical elements

    Science.gov (United States)

    Eggenstein, F.; Krivenkov, M.; Rudolph, I.; Sertsu, M. G.; Sokolov, A.; Varykhalov, A.; Wolf, J.; Zeschke, T.; Schäfers, F.

    2017-09-01

    The contamination of optical elements (mirrors and gratings) with carbon still is an issue when using soft x-ray synchrotron radiation. With an in-house developed HF-plasma treatment we are able to decontaminate our optics in-situ from carbon very efficiently. The cleaning device, a simple Al-antenna, is mounted in situ inside the mirror- and grating vacuum chambers. A systematic study of the HF-plasma cleaning efficiency was performed acquired with in-situ and exsitu methods for monitoring: An atomic force microscope (AFM) and a scanning tunneling microscope (STM) were used before and after the cleaning process to determine the surface morphology and roughness. Reflectivity angular scans using the reflectometer at the BESSY-II Metrology Station [1-3] allowed to estimate the thickness of the remaining Clayer after different cleaning steps and thereby helped us to determine the etching rate. Reflection spectra measurements in the range of 200 eV - 900 eV show the complete removal of Carbon from the optics without contaminating it with any other elements due to the plasma treatment. The data show that the plasma process improves the reflectivity and reduces the roughness of the surface. In addition to that, the region of the optical surface where the carbon has been removed becomes passivated.

  20. X-ray Pump–Probe Investigation of Charge and Dissociation Dynamics in Methyl Iodine Molecule

    Directory of Open Access Journals (Sweden)

    Li Fang

    2017-05-01

    Full Text Available Molecular dynamics is of fundamental interest in natural science research. The capability of investigating molecular dynamics is one of the various motivations for ultrafast optics. We present our investigation of photoionization and nuclear dynamics in methyl iodine (CH3I molecule with an X-ray pump X-ray probe scheme. The pump–probe experiment was realized with a two-mirror X-ray split and delay apparatus. Time-of-flight mass spectra at various pump–probe delay times were recorded to obtain the time profile for the creation of high charge states via sequential ionization and for molecular dissociation. We observed high charge states of atomic iodine up to 29+, and visualized the evolution of creating these high atomic ion charge states, including their population suppression and enhancement as the arrival time of the second X-ray pulse was varied. We also show the evolution of the kinetics of the high charge states upon the timing of their creation during the ionization-dissociation coupled dynamics. We demonstrate the implementation of X-ray pump–probe methodology for investigating X-ray induced molecular dynamics with femtosecond temporal resolution. The results indicate the footprints of ionization that lead to high charge states, probing the long-range potential curves of the high charge states.

  1. Investigation of pulse shape analyzers for phoswich detectors in space-borne hard X-ray experiments

    Energy Technology Data Exchange (ETDEWEB)

    Bleeker, J A.M.; Overtoom, J M [Huygens Lab., Leiden (Netherlands). Cosmic Ray Working Group

    1979-12-01

    A low-background telescope for hard X-ray astronomy (15-250 keV), comprising arrays of NaI(Tl)/CsI(Na) phoswiches as photon collectors, was recently developed. The background rejection efficiency of such a telescope, and hence the minimum source in a given time, critically depends on the performance of the phoswich pulse shape analyzer (PSA) in a space radiation environment. Results from theoretical and experimental work on analyzer configurations based on zero-crossing detection are presented. This led to the selection of an optimum configuration for space application. The in-situ performance of this analyzer was evaluated in a balloon-borne hard X-ray experiment, showing excellent discrimination efficiency throughout the entire energy regime.

  2. 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.

  3. In situ X-ray and neutron diffraction of the Ruddlesden-Popper compounds (RE2-xSrx)0.98(Fe0.8Co0.2)1-yMgyO4-δ (RE=La, Pr): Structure and CO2 stability

    DEFF Research Database (Denmark)

    Chatzichristodoulou, Christodoulos; Hauback, B.C.; Hendriksen, Peter Vang

    2013-01-01

    The crystal structure of the Ruddlesden-Popper compounds (La 1.0Sr1.0)0.98Fe0.8Co 0.2O4-δ and (La1.2Sr0.8) 0.98(Fe0.8Co0.2)0.8Mg 0.2O4-δ was investigated at 1000 °C in N 2 (aO2=1×10-4) by in-situ powder neutron diffraction. In-situ powder X-ray diffraction (PXD) was also employed to investigate....... The equivalent pseudo-cubic thermal and chemical expansion coefficients are in agreement with values determined by dilatometry. The chemical stability in CO2 containing environments of various Ruddlesden-Popper compounds with chemical formula (RE2-xSr x)0.98(Fe0.8Co0.2) 1-yMgyO4-δ (RE=La, Pr), as well...

  4. 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.

  5. Investigation of electronic order using resonant soft X-ray diffraction

    Energy Technology Data Exchange (ETDEWEB)

    Schlappa, J.

    2006-12-01

    The aim of this PhD work was the application of resonant soft X-ray diffraction technique for the investigation of electronic order in transition metal oxides at the TM L{sub 2,3}-edge, trying to obtain a quantitative understanding of the data. The method was first systematically explored through application to a model system in order to test the feasibility of the technique and to understand of how X-ray optical effects have to be taken into account. Two more complex systems were investigated; stripe order in La{sub 1.8}Sr{sub 0.2}NiO{sub 4} and charge and orbital order in Fe{sub 3}O{sub 4}. The main focus of the work was on the spectroscopic potential of the technique, trying to obtain a level of quantitative description of the data. For X-ray absorption spectroscopy (XAS) from transition metal oxides, cluster configuration interaction calculation provides a powerful and realistic microscopic theory. In the frame work of this thesis cluster theory, considering explicit hybridization effects between the TM-ion and the surrounding oxygen ligands, has been applied for the first time to describe resonant diffraction data. (orig.)

  6. Investigation of electronic order using resonant soft X-ray diffraction

    International Nuclear Information System (INIS)

    Schlappa, J.

    2006-01-01

    The aim of this PhD work was the application of resonant soft X-ray diffraction technique for the investigation of electronic order in transition metal oxides at the TM L 2,3 -edge, trying to obtain a quantitative understanding of the data. The method was first systematically explored through application to a model system in order to test the feasibility of the technique and to understand of how X-ray optical effects have to be taken into account. Two more complex systems were investigated; stripe order in La 1.8 Sr 0.2 NiO 4 and charge and orbital order in Fe 3 O 4 . The main focus of the work was on the spectroscopic potential of the technique, trying to obtain a level of quantitative description of the data. For X-ray absorption spectroscopy (XAS) from transition metal oxides, cluster configuration interaction calculation provides a powerful and realistic microscopic theory. In the frame work of this thesis cluster theory, considering explicit hybridization effects between the TM-ion and the surrounding oxygen ligands, has been applied for the first time to describe resonant diffraction data. (orig.)

  7. 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)

  8. Electronic properties of Nd2−xCexCuO4+δ: A hard X-ray photoemission investigation

    International Nuclear Information System (INIS)

    Guarino, A.; Panaccione, G.; Offi, F.; Monaco, G.; Fondacaro, A.; Torelli, P.; Fittipaldi, R.; Vecchione, A.; Pace, S.; Nigro, A.

    2016-01-01

    Highlights: • We grow and characterize Nd 2−x Ce x CuO 4+δ samples as thin film and single crystal. • We study the Cu 2p levels of our samples by hard X-ray photoemission spectroscopy. • We investigate bulk features of the Nd 2−x Ce x CuO 4+δ samples. • Signature of the bulk response is correlated with the crystallinity of the samples. - Abstract: Cu 2p core levels spectra measured by X-ray photoemission spectroscopy of selected as-grown Nd 2−x Ce x CuO 4+δ samples are presented and discussed. The presence of a satellite peak in the 2p core level of Nd 2−x Ce x CuO 4+δ single crystal by hard X-ray photoemission is confirmed in all non-superconducting samples, films and single crystals investigated in this work. The comparison of the spectral features of the different samples suggests that the presence and the intensity of this satellite peak is not related to the electric transport properties, but to the texture characteristics.

  9. Instability of cyclic superelastic deformation of NiTi investigated by synchrotron X-ray diffraction

    Czech Academy of Sciences Publication Activity Database

    Sedmák, P.; Šittner, Petr; Pilch, Jan; Curfs, C.

    2015-01-01

    Roč. 94, Aug (2015), s. 257-270 ISSN 1359-6454 R&D Projects: GA ČR GB14-36566G; GA ČR GPP108/12/P111; GA ČR GA14-15264S; GA ČR GAP107/12/0800 Institutional support: RVO:68378271 Keywords : shape memory alloy * NiTi * superelasticity * cyclic deformation * in situ X-ray diffraction Subject RIV: JG - Metallurgy Impact factor: 5.058, year: 2015

  10. 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.

  11. 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.

  12. 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

  13. 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

  14. 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.

  15. 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)

  16. 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.

  17. Synchrotron-Radiation X-Ray Investigation of Li+/Na+ Intercalation into Prussian Blue Analogues

    Directory of Open Access Journals (Sweden)

    Yutaka Moritomo

    2013-01-01

    Full Text Available Prussian blue analogies (PBAs are promising cathode materials for lithium ion (LIB and sodium ion (SIB secondary batteries, reflecting their covalent and nanoporous host structure. With use of synchrotron-radiation (SR X-ray source, we investigated the structural and electronic responses of the host framework of PBAs against Li+ and Na+ intercalation by means of the X-ray powder diffraction (XRD and X-ray absorption spectroscopy (XAS. The structural investigation reveals a robust nature of the host framework against Li+ and Na+ intercalation, which is advantageous for the stability and lifetime of the batteries. The spectroscopic investigation identifies the redox processes in respective plateaus in the discharge curves. We further compare these characteristics with those of the conventional cathode materials, such as, LiCoO2, LiFePO4, and LiMn2O4.

  18. 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

  19. EPR and X-ray diffraction investigation of some Greek marbles and limestones

    International Nuclear Information System (INIS)

    Duliu, Octavian; Grecu, Maria Nicoleta; Cristea, Corina

    2009-01-01

    Twelve different marble and limestone samples collected from well-known Greek quarries have been investigated by X-ray diffraction and electron paramagnetic resonance (EPR). X-ray diffraction spectra permitted to determine both major (calcite and dolomite) and minor (quartz or magnesite) mineralogical components. EPR has been used to investigate the same samples unirradiated and after 10 kGy gamma-ray irradiation. The unirradiated samples display typical EPR spectra of Mn 2+ in calcite and dolomite as well as a superposition of these while some samples displayed EPR free radicals signals of centers (low field signal) and centers (high field signal). From X-ray diffraction and EPR spectra it was possible to extract numerical values of several numerical parameters such as dolomite to calcite ratio, EPR intensity parameter, and low field to high field EPR signals intensity ratio. These values as well as the correlation coefficients between the digital functions that described the low field Mn 2+ ions EPR line have been used as entry data for cluster analysis to quantify the resemblance and differences between analyzed samples. (authors)

  20. Center for X-Ray Optics, 1986

    International Nuclear Information System (INIS)

    1987-07-01

    The Center for X-Ray Optics has made substantial progress during the past year on the development of very high resolution x-ray technologies, the generation of coherent radiation at x-ray wavelengths, and, based on these new developments, had embarked on several scientific investigations that would not otherwise have been possible. The investigations covered in this report are topics on x-ray sources, x-ray imaging and applications, soft x-ray spectroscopy, synchrotron radiation, advanced light source and magnet structures for undulators and wigglers

  1. Frequency filter of seed x-ray by use of x-ray laser medium. Toward the generation of the temporally coherent x-ray laser

    International Nuclear Information System (INIS)

    Hasegawa, Noboru; Kawachi, Tetsuya; Kishimoto, Maki; Sukegawa, Kouta; Tanaka, Momoko; Ochi, Yoshihiro; Nishikino, Masaharu; Nagashima, Keisuke; Kato, Yoshiaki; Renzhong, Tai

    2009-01-01

    We evaluate the characteristics of a higher-order harmonics light as a seed X-ray amplified through a laser-produced X-ray amplifier. The narrow spectral bandwidth of the X-ray amplifier works as the frequency filter of the seed X-ray, resulting in that only the temporally coherent X-ray is amplified. Experimental investigation using the 29th-order harmonic light of the Ti:sapphire laser at a wavelength of 26.9 nm together with a neon-like manganese X-ray laser medium shows evident spectral narrowing of the seed X-ray and amplification without serious diffraction effects on the propagation of the amplified X-ray beam. This implies that the present combination is potential to realize temporally coherent X-ray lasers, with an expected duration of approximately 400 fs. (author)

  2. 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.

  3. 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}).

  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. 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. Soft X-ray synchrotron radiation investigations of actinide materials systems utilizing X-ray emission spectroscopy and resonant inelastic X-ray scattering

    International Nuclear Information System (INIS)

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

    2004-01-01

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

  7. Investigation of Deuterium Loaded Materials Subject to X-Ray Exposure

    Science.gov (United States)

    Benyo, Theresa L.; Steinetz, Bruce M.; Hendricks, Robert C.; Martin, Richard E.; Forsley, Lawrence P.; Daniels, Christopher C.; Chait, Arnon; Pines, Vladimir; Pines, Marianna; Penney, Nicholas; hide

    2017-01-01

    Results are presented from an exploratory study involving x-ray irradiation of select deuterated materials. Titanium deuteride plus deuterated polyethylene, deuterated polyethylene alone, and for control, hydrogen-based polyethylene samples and nondeuterated titanium samples were exposed to x-ray irradiation. These samples were exposed to various energy levels from 65 to 280 kV with prescribed electron flux from 500 to 9000 µA impinging on a tungsten braking target, with total exposure times ranging from 55 to 280 min. Gamma activity was measured using a high-purity germanium (HPGe) detector, and for all samples no gamma activity above background was detected. Alpha and beta activities were measured using a gas proportional counter, and for select samples beta activity was measured with a liquid scintillator spectrometer. The majority of the deuterated materials subjected to the microfocus x-ray irradiation exhibited postexposure beta activity above background and several showed short-lived alpha activity. The HPE and nondeuterated titanium control samples exposed to the x-ray irradiation showed no postexposure alpha or beta activities above background. Several of the samples (SL10A, SL16, SL17A) showed beta activity above background with a greater than 4s confidence level, months after exposure. Portions of SL10A, SL16, and SL17A samples were also scanned using a beta scintillator and found to have beta activity in the tritium energy band, continuing without noticeable decay for over 12 months. Beta scintillation investigation of as-received materials (before x-ray exposure) showed no beta activity in the tritium energy band, indicating the beta emitters were not in the starting materials.

  8. New Pyrazole-Hydrazone Derivatives: X-ray Analysis, Molecular Structure Investigation via Density Functional Theory (DFT) and Their High In-Situ Catecholase Activity.

    Science.gov (United States)

    Karrouchi, Khalid; Yousfi, El Bekkaye; Sebbar, Nada Kheira; Ramli, Youssef; Taoufik, Jamal; Ouzidan, Younes; Ansar, M'hammed; Mabkhot, Yahia N; Ghabbour, Hazem A; Radi, Smaail

    2017-10-25

    The development of low-cost catalytic systems that mimic the activity of tyrosinase enzymes (Catechol oxidase) is of great promise for future biochemistry technologic demands. Herein, we report the synthesis of new biomolecules systems based on hydrazone derivatives containing a pyrazole moiety ( L1 - L6 ) with superior catecholase activity. Crystal structures of L1 and L2 biomolecules were determined by X-ray single crystal diffraction (XRD). Optimized geometrical parameters were calculated by density functional theory (DFT) at B3LYP/6-31G (d, p) level and were found to be in good agreement with single crystal XRD data. Copper (II) complexes of the compounds ( L1 - L6 ), generated in-situ, were investigated for their catalytic activities towards the oxidation reaction of catechol to ortho -quinone with the atmospheric dioxygen, in an attempt to model the activity of the copper containing enzyme tyrosinase. The studies showed that the activities depend on four parameters: the nature of the ligand, the nature of counter anion, the nature of solvent and the concentration of ligand. The Cu(II)-ligands, given here, present the highest catalytic activity (72.920 μmol·L -1 ·min -1 ) among the catalysts recently reported in the existing literature.

  9. 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

  10. Identification of ginseng root using quantitative X-ray microtomography.

    Science.gov (United States)

    Ye, Linlin; Xue, Yanling; Wang, Yudan; Qi, Juncheng; Xiao, Tiqiao

    2017-07-01

    The use of X-ray phase-contrast microtomography for the investigation of Chinese medicinal materials is advantageous for its nondestructive, in situ , and three-dimensional quantitative imaging properties. The X-ray phase-contrast microtomography quantitative imaging method was used to investigate the microstructure of ginseng, and the phase-retrieval method is also employed to process the experimental data. Four different ginseng samples were collected and investigated; these were classified according to their species, production area, and sample growth pattern. The quantitative internal characteristic microstructures of ginseng were extracted successfully. The size and position distributions of the calcium oxalate cluster crystals (COCCs), important secondary metabolites that accumulate in ginseng, are revealed by the three-dimensional quantitative imaging method. The volume and amount of the COCCs in different species of the ginseng are obtained by a quantitative analysis of the three-dimensional microstructures, which shows obvious difference among the four species of ginseng. This study is the first to provide evidence of the distribution characteristics of COCCs to identify four types of ginseng, with regard to species authentication and age identification, by X-ray phase-contrast microtomography quantitative imaging. This method is also expected to reveal important relationships between COCCs and the occurrence of the effective medicinal components of ginseng.

  11. X-ray Topographic Investigations of Domain Structure in Czochralski Grown PrxLa1-xAlO3 Crystals

    International Nuclear Information System (INIS)

    Wieteska, K.; Wierzchowski, W.; Malinowska, A.; Turczynski, S.; Pawlak, D.A.; Lukasiewicz, T.; Lefeld-Sosnowska, M.; Graeff, W.

    2010-01-01

    In the present paper X-ray diffraction topographic techniques were applied to a number of samples cut from Czochralski grown Pr x La 1-x AlO 3 crystals with different ratio of praseodymium and lanthanum. Conventional and synchrotron X-ray topographic investigations revealed differently developed domain structures dependent on the composition of mixed praseodymium lanthanum aluminium perovskites. Some large mosaic blocks were observed together with the domains. In the best crystals, X-ray topographs revealed striation fringes and individual dislocations inside large domains. Synchrotron topographs allowed us to indicate that the domains correspond to three different crystallographic planes, and to evaluate the lattice misorientation between domains in the range of 20-50 arc min (authors)

  12. Duodenal X-ray diagnostics

    International Nuclear Information System (INIS)

    Scheppach, W.

    1982-01-01

    The publication provides an overview of duodenal X-ray diagnostics with the aid of barium meals in 1362 patients. The introducing paragraphs deal with the topographic anatomy of the region and the methodics of X-ray investigation. The chapter entitled ''processes at the duodenum itself'' describes mainly ulcers, diverticula, congenital anomalies, tumors and inflammations. The neighbourhood processes comprise in the first place diseases having their origin at the pancreas and bile ducts. As a conclusion, endoscopic rectograde cholangio-pancreaticography and percutaneous transhepatic cholangiography are pointed out as advanced X-ray investigation methods. In the annex of X-ray images some of the described phenomena are shown in exemplary manner. (orig./MG) [de

  13. X-ray interferometers

    International Nuclear Information System (INIS)

    Franks, A.

    1980-01-01

    An improved type of amplitude-division x-ray interferometer is described. The wavelength at which the interferometer can operate is variable, allowing the instrument to be used to measure x-ray wavelength, and the angle of inclination is variable for sample investigation. (U.K.)

  14. 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)

  15. Electronic properties of Nd{sub 2−x}Ce{sub x}CuO{sub 4+δ}: A hard X-ray photoemission investigation

    Energy Technology Data Exchange (ETDEWEB)

    Guarino, A., E-mail: guarino@sa.infn.it [CNR-SPIN-Salerno, Fisciano, SA (Italy); Dipartimento di Fisica “E. R. Caianiello” Università di Salerno, Fisciano, SA (Italy); Panaccione, G. [CNR-IOM Laboratorio TASC, AREA Science Park, 34012 Basovizza, TS (Italy); Offi, F. [CNISM and Dipartimento di Scienze, Università Roma Tre, Roma (Italy); Monaco, G. [Dipartimento di Fisica, Università di Trento, Trento (Italy); Fondacaro, A. [European Synchrotron Radiation Facility, BP 220, F-38042 Grenoble (France); Torelli, P. [CNR-IOM Laboratorio TASC, AREA Science Park, 34012 Basovizza, TS (Italy); Fittipaldi, R.; Vecchione, A. [CNR-SPIN-Salerno, Fisciano, SA (Italy); Pace, S.; Nigro, A. [CNR-SPIN-Salerno, Fisciano, SA (Italy); Dipartimento di Fisica “E. R. Caianiello” Università di Salerno, Fisciano, SA (Italy)

    2016-10-15

    Highlights: • We grow and characterize Nd{sub 2−x}Ce{sub x}CuO{sub 4+δ} samples as thin film and single crystal. • We study the Cu 2p levels of our samples by hard X-ray photoemission spectroscopy. • We investigate bulk features of the Nd{sub 2−x}Ce{sub x}CuO{sub 4+δ} samples. • Signature of the bulk response is correlated with the crystallinity of the samples. - Abstract: Cu 2p core levels spectra measured by X-ray photoemission spectroscopy of selected as-grown Nd{sub 2−x}Ce{sub x}CuO{sub 4+δ} samples are presented and discussed. The presence of a satellite peak in the 2p core level of Nd{sub 2−x}Ce{sub x}CuO{sub 4+δ} single crystal by hard X-ray photoemission is confirmed in all non-superconducting samples, films and single crystals investigated in this work. The comparison of the spectral features of the different samples suggests that the presence and the intensity of this satellite peak is not related to the electric transport properties, but to the texture characteristics.

  16. 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...

  17. 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.

  18. 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....

  19. In situ x-ray diffraction investigations during low energy ion nitriding of austenitic stainless steel grade 1.4571

    International Nuclear Information System (INIS)

    Manova, D; Mändl, S; Gerlach, J W; Hirsch, D; Neumann, H; Rauschenbach, B

    2014-01-01

    Insertion of nitrogen into austenitic stainless steel leads to anomalously fast nitrogen diffusion and the formation of an expanded face-centred cubic phase which is known to contain a large amount of mechanical stress. In situ x-ray diffraction (XRD) measurements during low energy nitrogen ion implantation into steel 316Ti at 300–550 °C allow a direct view into diffusion and phase formation. While the layer growth is directly observable from the decreasing substrate reflection intensity, the time evolution of the intensities for the expanded phase reflection is much more complex: several mechanisms including at least formation and annealing of defects, twinning, reduction of the crystal symmetry, or grain rotation may be active inside the expanded phase, besides the thermally activated decay of the metastable expanded phase. This locally varying coherence length or scattering intensity from the expanded phase is furthermore a function of temperature and time, additionally complicating the deconvolution of XRD spectra for stress and concentration gradients. As no concise modelling of this coherence length is possible at present, a simple qualitative model assuming a dependence of the scattering intensity on the depth, influence by stress and plastic flow during the nitriding process is proposed for understanding the underlying processes. (paper)

  20. 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

  1. 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.)

  2. Hazard and efficiency of X-ray diagnostic investigations

    International Nuclear Information System (INIS)

    1984-01-01

    This symposium deals with the hazards and efficiency of biomedical X-ray examinations. The first articles are devoted to the effects of radiation on the human body. Special attention is paid to low dose irradiation. Later on the efficiency and necessity of X-ray examinations are discussed. Reference is made to the diagnosis of colon- and mammacarcinoma. (Auth.)

  3. 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...

  4. 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.

  5. Investigation of the hard x-ray background in backlit pinhole imagers

    Energy Technology Data Exchange (ETDEWEB)

    Fein, J. R., E-mail: jrfein@umich.edu; Holloway, J. P. [Department of Nuclear Engineering and Radiological Sciences, University of Michigan, Ann Arbor, Michigan 48109-2143 (United States); Peebles, J. L. [Center for Energy Research, University of California, San Diego, La Jolla, California 92093 (United States); Keiter, P. A.; Klein, S. R.; Kuranz, C. C.; Manuel, M. J.-E.; Drake, R. P. [Department of Atmospheric, Oceanic and Space Sciences, University of Michigan, Ann Arbor, Michigan 48109-2143 (United States)

    2014-11-15

    Hard x-rays from laser-produced hot electrons (>10 keV) in backlit pinhole imagers can give rise to a background signal that decreases signal dynamic range in radiographs. Consequently, significant uncertainties are introduced to the measured optical depth of imaged plasmas. Past experiments have demonstrated that hard x-rays are produced when hot electrons interact with the high-Z pinhole substrate used to collimate the softer He-α x-ray source. Results are presented from recent experiments performed on the OMEGA-60 laser to further study the production of hard x-rays in the pinhole substrate and how these x-rays contribute to the background signal in radiographs. Radiographic image plates measured hard x-rays from pinhole imagers with Mo, Sn, and Ta pinhole substrates. The variation in background signal between pinhole substrates provides evidence that much of this background comes from x-rays produced in the pinhole substrate itself. A Monte Carlo electron transport code was used to model x-ray production from hot electrons interacting in the pinhole substrate, as well as to model measurements of x-rays from the irradiated side of the targets, recorded by a bremsstrahlung x-ray spectrometer. Inconsistencies in inferred hot electron distributions between the different pinhole substrate materials demonstrate that additional sources of hot electrons beyond those modeled may produce hard x-rays in the pinhole substrate.

  6. 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

  7. 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

  8. 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

  9. 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

  10. 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.

  11. Laser plasma x-ray source for ultrafast time-resolved x-ray absorption spectroscopy

    Directory of Open Access Journals (Sweden)

    L. Miaja-Avila

    2015-03-01

    Full Text Available We describe a laser-driven x-ray plasma source designed for ultrafast x-ray absorption spectroscopy. The source is comprised of a 1 kHz, 20 W, femtosecond pulsed infrared laser and a water target. We present the x-ray spectra as a function of laser energy and pulse duration. Additionally, we investigate the plasma temperature and photon flux as we vary the laser energy. We obtain a 75 μm FWHM x-ray spot size, containing ∼106 photons/s, by focusing the produced x-rays with a polycapillary optic. Since the acquisition of x-ray absorption spectra requires the averaging of measurements from >107 laser pulses, we also present data on the source stability, including single pulse measurements of the x-ray yield and the x-ray spectral shape. In single pulse measurements, the x-ray flux has a measured standard deviation of 8%, where the laser pointing is the main cause of variability. Further, we show that the variability in x-ray spectral shape from single pulses is low, thus justifying the combining of x-rays obtained from different laser pulses into a single spectrum. Finally, we show a static x-ray absorption spectrum of a ferrioxalate solution as detected by a microcalorimeter array. Altogether, our results demonstrate that this water-jet based plasma source is a suitable candidate for laboratory-based time-resolved x-ray absorption spectroscopy experiments.

  12. The x-ray time of flight method for investigation of ghosting in amorphous selenium-based flat panel medical x-ray imagers

    International Nuclear Information System (INIS)

    Rau, A.W.; Bakueva, L.; Rowlands, J.A.

    2005-01-01

    Amorphous selenium (a-Se) based real-time flat-panel imagers (FPIs) are finding their way into the digital radiology department because they offer the practical advantages of digital x-ray imaging combined with an image quality that equals or outperforms that of conventional systems. The temporal imaging characteristics of FPIs can be affected by ghosting (i.e., radiation-induced changes of sensitivity) when the dose to the detector is high (e.g., portal imaging and mammography) or the images are acquired at a high frame rate (e.g., fluoroscopy). In this paper, the x-ray time-of-flight (TOF) method is introduced as a tool for the investigation of ghosting in a-Se photoconductor layers. The method consists of irradiating layers of a-Se with short x-ray pulses. From the current generated in the a-Se layer, ghosting is quantified and the ghosting parameters (charge carrier generation rate and carrier lifetimes and mobilities) are assessed. The x-ray TOF method is novel in that (1) x-ray sensitivity (S) and ghosting parameters can be measured simultaneously (2) the transport of both holes and electrons can be isolated, and (3) the method is applicable to the practical a-Se layer structure with blocking contacts used in FPIs. The x-ray TOF method was applied to an analysis of ghosting in a-Se photoconductor layers under portal imaging conditions, i.e., 1 mm thick a-Se layers, biased at 5 V/μm, were irradiated using a 6 MV LINAC x-ray beam to a total dose (ghosting dose) of 30 Gy. The initial sensitivity (S 0 ) of the a-Se layers was 63±2 nC cm -2 cGy -1 . It was found that S decreases to 30% of S 0 after a ghosting dose of 5 Gy and to 21% after 30 Gy at which point no further change in S occurs. At an x-ray intensity of 22 Gy/s (instantaneous dose rate during a LINAC x-ray pulse), the charge carrier generation rate was 1.25±0.1x10 22 ehp m -3 s -1 and, to a first approximation, independent of the ghosting dose. However, both hole and electron transport showed a

  13. High-speed X-ray topography

    International Nuclear Information System (INIS)

    Eckers, W.; Oppolzer, H.

    1977-01-01

    The investigation of lattice defects in semiconductor crystals by conventional X-ray diffraction topography is very time-consuming. Exposure times can be reduced by using high-intensity X-rays and X-ray image intensifiers. The described system comprises a high-power rotating-anode X-ray tube, a remote-controlled X-ray topography camera, and a television system operating with an X-ray sensing VIDICON. System performance is demonstrated with reference to exploratory examples. The exposure time for photographic plates is reduced to 1/20 and for the X-ray TV system (resolution of the order of 30 μm) to 1/100 relative to that required when using a conventional topography system. (orig.) [de

  14. Soft x-ray lasers

    International Nuclear Information System (INIS)

    Matthews, D.L.; Rosen, M.D.

    1988-01-01

    One of the elusive dreams of laser physicists has been the development of an x-ray laser. After 25 years of waiting, the x-ray laser has at last entered the scientific scene, although those now in operation are still laboratory prototypes. They produce soft x rays down to about five nanometers. X-ray lasers retain the usual characteristics of their optical counterparts: a very tight beam, spatial and temporal coherence, and extreme brightness. Present x-ray lasers are nearly 100 times brighter that the next most powerful x-ray source in the world: the electron synchrotron. Although Lawrence Livermore National Laboratory (LLNL) is widely known for its hard-x-ray laser program which has potential applications in the Strategic Defense Initiative, the soft x-ray lasers have no direct military applications. These lasers, and the scientific tools that result from their development, may one day have a place in the design and diagnosis of both laser fusion and hard x-ray lasers. The soft x-ray lasers now in operation at the LLNL have shown great promise but are still in the primitive state. Once x-ray lasers become reliable, efficient, and economical, they will have several important applications. Chief among them might be the creation of holograms of microscopic biological structures too small to be investigated with visible light. 5 figs

  15. 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%....

  16. 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...

  17. Electronic structure and optical properties of CdS{sub x}Se{sub 1−x} solid solution nanostructures from X-ray absorption near edge structure, X-ray excited optical luminescence, and density functional theory investigations

    Energy Technology Data Exchange (ETDEWEB)

    Murphy, M. W. [DESY (Deutsches Elektronen-Synchrotron), FS-PEX, Notkestrasse 85, 22607 Hamburg (Germany); Yiu, Y. M., E-mail: yyiu@uwo.ca; Sham, T. K. [Department of Chemistry, University of Western Ontario, London, ON N6A5B7 (Canada); Ward, M. J. [Cornell High Energy Synchrotron Source (CHESS), Cornell University, Ithaca, NY 14853 (United States); Liu, L. [Institute of Functional Nano and Soft Materials (FUNSOM) and Soochow University-Western University Center for Synchrotron Radiation Research, Soochow University, Suzhou, Jiangsu, 215123 (China); Hu, Y. [Canadian Light Source, University of Saskatchewan, Saskatoon, SK S7N2V3 (Canada); Zapien, J. A. [Center Of Super-Diamond and Advanced Films (COSDAF) and Department of Physics and Materials Science, City University of Hong Kong, Hong Kong SAR (China); Liu, Yingkai [Institute of Physics and Electronic Information, Yunnan Normal University, Kunming, Yunnan, 650500 (China)

    2014-11-21

    The electronic structure and optical properties of a series of iso-electronic and iso-structural CdS{sub x}Se{sub 1−x} solid solution nanostructures have been investigated using X-ray absorption near edge structure, extended X-ray absorption fine structure, and X-ray excited optical luminescence at various absorption edges of Cd, S, and Se. It is found that the system exhibits compositions, with variable local structure in-between that of CdS and CdSe accompanied by tunable optical band gap between that of CdS and CdSe. Theoretical calculation using density functional theory has been carried out to elucidate the observations. It is also found that luminescence induced by X-ray excitation shows new optical channels not observed previously with laser excitation. The implications of these observations are discussed.

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

    Science.gov (United States)

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

    2015-03-15

    Multiple-unit tablets consisting of polymer-coated microgranules and excipients have a number of advantageous pharmaceutical properties. Polymer-coated microgranules are known to often lose their functionality because of damage to the polymer coating caused by tableting, and the mechanism of polymer coating damage as well as the structural changes of excipients upon tableting had been investigated but without in-situ visualization and quantitative analysis. To elucidate the mechanism of coating damage, the internal structures of multiple-unit tablets were investigated by X-ray computed microtomography using synchrotron X-rays. Cross sectional images of the tablets with sub-micron spatial resolution clearly revealed that void spaces remained around the compressed excipient particles in the tablets containing an excipient composed of cellulose and lactose (Cellactose(®) 80), whereas much smaller void spaces remained in the tablets containing an excipient made of sorbitol (Parteck(®) SI 150). The relationships between the void spaces and the physical properties of the tablets such as hardness and disintegration were investigated. Damage to the polymer coating in tablets was found mainly where polymer-coated microgranules were in direct contact with each other in both types of tablets, which could be attributed to the difference in hardness of excipient particles and the core of the polymer-coated microgranules. Copyright © 2015 Elsevier B.V. All rights reserved.

  19. Coupling in-situ X-ray micro- and nano-tomography and discrete element method for investigating high temperature sintering of metal and ceramic powders

    Directory of Open Access Journals (Sweden)

    Yan Zilin

    2017-01-01

    Full Text Available The behaviour of various powder systems during high temperature sintering has been investigated by coupling X-ray microtomography and discrete element method (DEM. Both methods are particularly relevant to analyse particle interactions and porosity changes occurring during sintering. Two examples are presented. The first one deals with a copper powder including artificially created pores which sintering has been observed in situ at the European synchrotron and simulated by DEM. 3D images with a resolution of 1.5 μm have been taken at various times of the sintering cycle. The comparison of the real displacement of particle centers with the displacement derived from the mean field assumption demonstrates significant particle rearrangement in some regions of the sample. Although DEM simulation showed less rearrangement, it has been able to accurately predict the densification kinetics. The second example concerns multilayer ceramic capacitors (MLCCs composed of hundreds of alternated metal electrode and ceramic dielectric layers. The observation of Ni-based MLCCs by synchrotron nanotomography at Argon National Laboratory with a spatial resolution between 10 and 50 nm allowed understanding the origin of heterogeneities formed in Ni layers during sintering. DEM simulations confirmed this analysis and provided clues for reducing these defects.

  20. Wavelength dispersive X-ray absorption fine structure imaging by parametric X-ray radiation

    International Nuclear Information System (INIS)

    Inagaki, Manabu; Sakai, Takeshi; Sato, Isamu; Hayakawa, Yasushi; Nogami, Kyoko; Tanaka, Toshinari; Hayakawa, Ken; Nakao, Keisuke

    2008-01-01

    The parametric X-ray radiation (PXR) generator system at Laboratory for Electron Beam Research and Application (LEBRA) in Nihon University is a monochromatic and coherent X-ray source with horizontal wavelength dispersion. The energy definition of the X-rays, which depends on the horizontal size of the incident electron beam on the generator target crystal, has been investigated experimentally by measuring the X-ray absorption near edge structure (XANES) spectra on Cu and CuO associated with conventional X-ray absorption imaging technique. The result demonstrated the controllability of the spectrum resolution of XANES by adjusting of the horizontal electron beam size on the target crystal. The XANES spectra were obtained with energy resolution of several eV at the narrowest case, which is in qualitative agreement with the energy definition of the PXR X-rays evaluated from geometrical consideration. The result also suggested that the wavelength dispersive X-ray absorption fine structure measurement associated with imaging technique is one of the promising applications of PXR. (author)

  1. In situ x-ray photoelectron spectroscopy and capacitance voltage characterization of plasma treatments for Al{sub 2}O{sub 3}/AlGaN/GaN stacks

    Energy Technology Data Exchange (ETDEWEB)

    Qin, Xiaoye; Lucero, Antonio; Azcatl, Angelica; Kim, Jiyoung; Wallace, Robert M. [Department of Materials Science and Engineering, University of Texas at Dallas, Richardson, Texas 75080 (United States)

    2014-07-07

    We investigate the Al{sub 2}O{sub 3}/AlGaN/GaN metal-oxide-semiconductor structure pretreated by O{sub 2} anneals, N{sub 2} remote plasma, and forming gas remote plasma prior to atomic layer deposition of Al{sub 2}O{sub 3} using in situ X-ray photoelectron spectroscopy, low energy electron diffraction, and capacitance- voltage measurements. Plasma pretreatments reduce the Ga-oxide/oxynitride formation and the interface state density, while inducing a threshold voltage instability.

  2. 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

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

    International Nuclear Information System (INIS)

    Susini, J.

    2004-01-01

    Soon after the discovery of X-rays in 1895 by W. Roentgen, it became rapidly clear that the methods traditionally used in the visible light regime, namely refraction, diffraction and reflection were difficult to apply for X-ray optics. The physical origins of these difficulties are closely linked to the very nature of interaction of X-rays with matter. The small deviation δ of the refractive index of condensed matter from unity makes it difficult to extend refraction-based optics from the optical spectral region to the X-ray region because the refraction angle is proportional to δ. Similarly it is very challenging to extend diffraction-based focusing techniques to X-rays because the diffraction angle scales inversely with wavelength. Finally, the use of reflection-based optics is also limited by the very small critical angle for total reflection. All those fundamental limitations prevented for almost one century, the development of X-ray microscopy whereas electron microscopy became a standard tool. In the past twenty years, interests for X-ray microscopy revived, mainly because of several major advances in X-ray sources and X-ray optics. X-ray microscopy techniques are now emerging as powerful and complementary tools for submicron investigations. Soft X-ray microscopes offer traditionally the possibility to form direct images of thick hydrated biological material in near-native environment, at a spatial resolution well beyond that achievable with visible light microscopy. Natural contrast is available in the soft X-ray region, in the so-called ''water-window'', due to the presence of absorption edges of the major constituents (C,N,O). Recent advances in manufacturing techniques have enlarged the accessible energy range of micro-focussing optics and offer new applications in a broad range of disciplines. X-ray microscopy in the 1 - 30 keV energy range is better suited for fluorescence to map trace elements, tomography for 3D imaging and micro-diffraction. The

  4. 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.

  5. Application of X-rays and Synchrotron X Rays to Residual Stress Evaluation Near Surfaces

    International Nuclear Information System (INIS)

    Pyzalla, Anke

    1999-01-01

    A nondestructive residual stress analysis can be performed using diffraction methods. The easiest accessible radiation is characteristic X radiation that has a penetration depth of ∼10 microm suitable for the determination of the residual stresses in near-surface layers. Special techniques have been developed, e.g., with respect to in situ analyses of the stress state in oxide layers and the residual stress analysis in coarse grained zones of steel welds or annealed Ni-base alloys. Depending on the size of the gauge volume, neutron diffraction can provide information at depths of tens of millimetres of steel and many tens of millimetres of Al. An alternative to the use of the characteristic synchrotron radiation is the use of a high-energy polychromatic beam in an energy dispersive arrangement, which gives access to higher penetration depths at still gauge volumes as small as 100 microm x 100 microm x 1 mm in steel rods of 15-mm diameter. The combination of neutrons with conventional X rays and monochromatic and polychromatic synchrotron radiation allows for a comprehensive investigation of the phase composition, the texture, and the residual stresses

  6. X-ray diffraction investigation of spin reorientation in SmFe2

    International Nuclear Information System (INIS)

    Gaviko, V.S.; Korolyov, A.V.; Mushnikov, N.V.

    1996-01-01

    Spontaneous magnetoelastic crystal lattice distortions in the spin reorientation region of high magnetostrictive SmFe 2 have been investigated by X-ray diffraction in the temperature range 80-300 K. Comparison of experimental shapes of X-ray diffraction lines with calculated shapes shows that, in the region of the spin reorientation transition, a mixture of left angle 110 right angle and left angle 111 right angle phases rather than the angular left angle uuw right angle -type phase is realized. The temperature dependence of the relative volume content of left angle 110 right angle and left angle 111 right angle phases is determined using least-squares fitting. (orig.)

  7. Investigation of L X-ray intensity ratios in Pt induced by proton collisions

    International Nuclear Information System (INIS)

    Kaur, Manpuneet; Kaur, Mandeep; Mohan, Harsh; Jain, Arvind Kumar; Singh, Parjit S.; Vohra, Neelam; Sharma, Sunita

    2015-01-01

    A survey of literature on L X-ray parameters inspires us for taking up the present investigation. These parameters are useful to study atomic properties. In view of this, we report L X-ray intensity ratios for Pt, namely, L ℓ / L α , L β / L α and L γ / L α with proton collisions over the energy range 260 - 400 keV with an interval of 20 keV. The intention of research presented in this paper is to explore their energy dependence and comparison with theoretical calculations. These analyses will yield a data in the low energy region which assist in better clarity of proton induced X-ray emission phenomenon

  8. X-ray electromagnetic application technology

    International Nuclear Information System (INIS)

    2011-01-01

    The investigating committee aimed at research on electromagnetic fields in functional devices and X-ray fibers for efficient coherent X-ray generation and their material science, high-precision manufacturing, particularly for X-ray electromagnetic application technology from January 2006 to December 2008. In this report, we describe our research results, in particular, on the topics of synchrotron radiation and free-electron laser, Saga Synchrotron Project, X-ray waveguides and waveguide-based lens-less hard-X-ray imaging, X-ray nanofocusing for capillaries and zone plates, dispersion characteristics in photonics crystal consisting of periodic atoms for nanometer waveguides, electromagnetic characteristics of grid structures for scattering fields of nano-meter electromagnetic waves and X-rays, FDTD parallel computing of fundamental scattering and attenuation characteristics of X-ray for medical imaging diagnosis, orthogonal relations of electromagnetic fields including evanescent field in dispersive medium. (author)

  9. Multilayer X-ray imaging systems

    Science.gov (United States)

    Shealy, D. L.; Hoover, R. B.; Gabardi, D. R.

    1986-01-01

    An assessment of the imaging properties of multilayer X-ray imaging systems with spherical surfaces has been made. A ray trace analysis was performed to investigate the effects of using spherical substrates (rather than the conventional paraboloidal/hyperboloidal contours) for doubly reflecting Cassegrain telescopes. These investigations were carried out for mirrors designed to operate at selected soft X-ray/XUV wavelengths that are of significance for studies of the solar corona/transition region from the Stanford/MSFC Rocket X-Ray Telescope. The effects of changes in separation of the primary and secondary elements were also investigated. These theoretical results are presented as well as the results of ray trace studies to establish the resolution and vignetting effects as a function of field angle and system parameters.

  10. 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.

  11. X-ray investigation of fatigued nickel monocrystals by an analysis of diffraction line profiles

    International Nuclear Information System (INIS)

    Schmidt, G.K.

    1988-01-01

    Using a statistics of the inhomogeneous plastic deformation of a fatigued FCC monocrystal it may be possible to analyse the intensity distributions of the X-ray reflections of this crystal with regard to the fatigue phenomena. The results of an X-ray investigation of a fatigued nickel monocrystal are desribed. 3 refs.; 1 figure; 1 table

  12. Chandra and the VLT Jointly Investigate the Cosmic X-Ray Background

    Science.gov (United States)

    2001-03-01

    Summary Important scientific advances often happen when complementary investigational techniques are brought together . In the present case, X-ray and optical/infrared observations with some of the world's foremost telescopes have provided the crucial information needed to solve a 40-year old cosmological riddle. Very detailed observations of a small field in the southern sky have recently been carried out, with the space-based NASA Chandra X-Ray Observatory as well as with several ground-based ESO telescopes, including the Very Large Telescope (VLT) at the Paranal Observatory (Chile). Together, they have provided the "deepest" combined view at X-ray and visual/infrared wavelengths ever obtained into the distant Universe. The concerted observational effort has already yielded significant scientific results. This is primarily due to the possibility to 'identify' most of the X-ray emitting objects detected by the Chandra X-ray Observatory on ground-based optical/infrared images and then to determine their nature and distance by means of detailed (spectral) observations with the VLT . In particular, there is now little doubt that the so-called 'X-ray background' , a seemingly diffuse short-wave radiation first detected in 1962, in fact originates in a vast number of powerful black holes residing in active nuclei of distant galaxies . Moreover, the present investigation has permitted to identify and study in some detail a prime example of a hitherto little known type of object, a distant, so-called 'Type II Quasar' , in which the central black hole is deeply embedded in surrounding gas and dust. These achievements are just the beginning of a most fruitful collaboration between "space" and "ground". It is yet another impressive demonstration of the rapid progress of modern astrophysics, due to the recent emergence of a new generation of extremely powerful instruments. PR Photo 09a/01 : Images of a small part of the Chandra Deep Field South , obtained with ESO telescopes

  13. 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.

  14. 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

  15. 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.

  16. 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

  17. X-ray interferometric Fourier holography

    International Nuclear Information System (INIS)

    Balyan, M.K.

    2016-01-01

    The X-ray interferometric Fourier holography is proposed and theoretically investigated. Fourier The X-ray interferometric Young fringes and object image reconstruction are investigated. It is shown that the interference pattern of two slits formed on the exit surface of the crystal-analyzer (the third plate of the interferometer) is the X-ray interferometric Young fringes. An expression for X-ray interferometric Young fringes period is obtained. The subsequent reconstruction of the slit image as an object is performed by means of Fourier transform of the intensity distribution on the hologram. Three methods of reconstruction of the amplitude transmission complex function of the object are presented: analytical - approximate method, method of iteration and step by step method. As an example the X-ray Fourier interferometric hologram recording and the complex amplitude transmission function reconstruction for a beryllium circular wire are considered

  18. 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.)

  19. 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

  20. 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.

  1. 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

  2. Ion backscattering and X-ray investigations of violin varnish and wood

    International Nuclear Information System (INIS)

    Sigurd, D.; Tove, P.A.; Petersson, S.

    1980-01-01

    The use of Rutherford backscattering (RBS) of ions (i.e. α-particles) and excitation of characteristic X-rays by protons, for determining the elemental composition of the top layers of violin varnish and wood is described. The amount of elements such as C, O, Si, S, Ca, Cu, Fe, Ni, Zn, Pb has been measured, on the varnished and unvarnished sides of wood samples from old instrument makers such as A. Stradivari, G. Guarneri del Gesu, Santo Serafin, C. Tononi etc. Differences in both the shape of the RBS spectra and in the presence of different elements are found and discussed. The use of X-ray excitation by ions (i.e. protons) helps in assessing the presence of the different elements. X-ray investigations can be done with instruments in air while RBS (at least in the presently used form) has to be performed in a vacuum chamber. Apart from offering an aid in determining the materials and procedures which were used in fabricating acoustically excellent instruments, the method could be of value for identifying their authenticity. (orig.)

  3. Ion backscattering and x-ray investigations of violin varnish and wood

    Science.gov (United States)

    Arne Tove, Per; Sigurd, Dag; Petersson, Sture

    1980-01-01

    The use of Rutherford backscattering (RBS) of ions (i.e. α-particles) and excitation of characteristic X-rays by protons, for determining the elemental composition of the top layers of violin varnish and wood is described. The amount of elements such as C, O, Si, S, Ca, Cu, Fe, Ni, Zn, Pb has been measured, on the varnished and unvarnished sides of wood samples from old instrument makers such as A. Stradivari, G. Guarneri del Gesu, Santo Serafin, C. Tononi etc. Differences in both the shape of the RBS spectra and in the presence of different elements are found and discussed. The use of X-ray excitation by ions (i.e. protons) helps in assessing the presence of the different elements. X-ray investigations can be done with instruments in air while RBS (at least in the presently used form) has to be performed in a vacuum chamber. Apart from offering an aid in determining the materials and procedures which were used in fabricating acoustically excellent instruments, the method could be of value for identifying their authenticity.

  4. Applications of phase-contrast x-ray imaging to medicine using an x-ray interferometer

    Science.gov (United States)

    Momose, Atsushi; Yoneyama, Akio; Takeda, Tohoru; Itai, Yuji; Tu, Jinhong; Hirano, Keiichi

    1999-10-01

    We are investigating possible medical applications of phase- contrast X-ray imaging using an X-ray interferometer. This paper introduces the strategy of the research project and the present status. The main subject is to broaden the observation area to enable in vivo observation. For this purpose, large X-ray interferometers were developed, and 2.5 cm X 1.5 cm interference patterns were generated using synchrotron X-rays. An improvement of the spatial resolution is also included in the project, and an X-ray interferometer designed for high-resolution phase-contrast X-ray imaging was fabricated and tested. In parallel with the instrumental developments, various soft tissues are observed by phase- contrast X-ray CT to find correspondence between the generated contrast and our histological knowledge. The observation done so far suggests that cancerous tissues are differentiated from normal tissues and that blood can produce phase contrast. Furthermore, this project includes exploring materials that modulate phase contrast for selective imaging.

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

    International Nuclear Information System (INIS)

    Mainz, R.; Klenk, R.

    2011-01-01

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

  6. Investigation of elemental distribution in lung samples by X-ray fluorescence microtomography

    International Nuclear Information System (INIS)

    Pereira, Gabriela R.; Rocha, Henrique S.; Lopes, Ricardo T.

    2007-01-01

    X-Ray Fluorescence Microtomography (XRFCT) is a suitable technique to find elemental distributions in heterogeneous samples. While x-ray transmission microtomography provides information about the linear attenuation coefficient distribution, XRFCT allows one to map the most important elements in the sample. The x-ray fluorescence tomography is based on the use of the X-ray fluorescence emitted from the elements contained in a sample so as to give additional information to characterize the object under study. In this work a rat lung and two human lung tissue samples have been investigated in order to verify the efficiency of the system in determination of the internal distribution of detected elements in these kinds of samples and to compare the elemental distribution in the lung tissue of an old human and a fetus. The experiments were performed at the X-Ray Fluorescence beamline (XRF) of the Brazilian Synchrotron Light Source (LNLS), Campinas, Brazil. A white beam was used for the excitation of the elements and the fluorescence photons have been detected by a HPGe detector. All the tomographies have been reconstructed using a filtered-back projection algorithm. It was possible to visualize the distribution of high atomic number elements on both, artificial and tissues samples. It was compared the quantity of Zn, Cu and Fe for the lung human tissue samples and verify that these elements have a higher concentration on the fetus tissue sample than the adult tissue sample. (author)

  7. In situ liquid water visualization in polymer electrolyte membrane fuel cells with high resolution synchrotron x-ray radiography

    Energy Technology Data Exchange (ETDEWEB)

    Chevalier, S.; Banerjee, R.; Lee, J.; Ge, N.; Lee, C.; Bazylak, A., E-mail: abazylak@mie.utoronto.ca [Dept. of Mechanical & Industrial Engineering, Faculty of Applied Science & Engineering, University of Toronto, Toronto, Ontario (Canada); Wysokinski, T. W.; Belev, G.; Webb, A.; Miller, D.; Zhu, N. [Canadian Light Source, Saskatoon, Saskatchewan (Canada); Tabuchi, Y.; Kotaka, T. [EV System Laboratory, Research Division 2, Nissan Motor Co., Ltd., Yokosuka, Kanagawa (Japan)

    2016-07-27

    In this work, we investigated the dominating properties of the porous materials that impact water dynamics in a polymer electrolyte membrane fuel cell (PEMFC). Visualizations of liquid water in an operating PEMFC were performed at the Canadian Light Source. A miniature fuel cell was specifically designed for X-ray imaging investigations, and an in-house image processing algorithm based on the Beer-Lambert law was developed to extract quantities of liquid water thicknesses (cm) from raw X-ray radiographs. The X-ray attenuation coefficient of water at 24 keV was measured with a calibration device to ensure accurate measurements of the liquid water thicknesses. From this experiment, the through plane distribution of the liquid water in the fuel cell was obtained.

  8. In situ liquid water visualization in polymer electrolyte membrane fuel cells with high resolution synchrotron x-ray radiography

    International Nuclear Information System (INIS)

    Chevalier, S.; Banerjee, R.; Lee, J.; Ge, N.; Lee, C.; Bazylak, A.; Wysokinski, T. W.; Belev, G.; Webb, A.; Miller, D.; Zhu, N.; Tabuchi, Y.; Kotaka, T.

    2016-01-01

    In this work, we investigated the dominating properties of the porous materials that impact water dynamics in a polymer electrolyte membrane fuel cell (PEMFC). Visualizations of liquid water in an operating PEMFC were performed at the Canadian Light Source. A miniature fuel cell was specifically designed for X-ray imaging investigations, and an in-house image processing algorithm based on the Beer-Lambert law was developed to extract quantities of liquid water thicknesses (cm) from raw X-ray radiographs. The X-ray attenuation coefficient of water at 24 keV was measured with a calibration device to ensure accurate measurements of the liquid water thicknesses. From this experiment, the through plane distribution of the liquid water in the fuel cell was obtained.

  9. Effective X-ray elastic constant measurement for in situ stress measurement of biaxially strained AA5754-O

    International Nuclear Information System (INIS)

    Iadicola, Mark A.; Gnäupel-Herold, Thomas H.

    2012-01-01

    Accurate measurement of stresses by X-ray diffraction requires accurate X-ray elastic constants. Calibration experiments are one method to determine these for a specific material in a specific condition. In this paper, uniaxial tension experiments are used to investigate the variation of these constants after uniaxial and equal-biaxial plastic deformation for an aluminum alloy (AA5754-O) of interest to the automotive industry. These data are critical for accurate measurement of the biaxial mechanical properties of the material using a recent experimental method combining specialized sheet metal forming equipment with portable X-ray diffraction equipment. The measured effective X-ray elastic constants show some minor variation with increased plastic deformation, and this behavior was found to be consistent for both uniaxially and equal-biaxially strained samples. The use of two average values for effective X-ray elastic constants, one in the rolling direction and one transverse to the rolling direction of the sheet material, is shown to be of sufficient accuracy for the combined tests of interest. Comparison of uniaxial data measured using X-ray diffraction and standard methods show good agreement, and biaxial stress–strain results show good repeatability. Additionally, the calibration data show some non-linear behavior, which is analyzed in regards to crystallographic texture and intergranular stress effects. The non-linear behavior is found to be the result of intergranular stresses based on comparison with additional measurements using other X-ray diffraction equipment and neutron diffraction.

  10. 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...

  11. 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.

  12. 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.

  13. 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.

  14. Determination of existing exposure level of population during X ray investigations

    International Nuclear Information System (INIS)

    Tselinov, N.V.; Kudritskij, Yu.K.

    1978-01-01

    The distribution of X ray procedures among 500 inhabitants of the city of Vorkuta in 1975 is studied. Data on the distribution of the subjects by age group and type of X ray procedure are presented. The results obtained broaden the existing concepts on hygienic importance of radiation received by the population of the country during X ray studies. It is proposed that these results be used in developing methods for standardizing X ray procedures

  15. 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

  16. 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.

  17. In Situ Techniques for the Investigation of the Kinetics of Austenitization of Supermartensitic Stainless Steel

    DEFF Research Database (Denmark)

    Nießen, Frank; Villa, Matteo; Apel, Daniel

    2016-01-01

    The austenitization and inter-critical annealing of X4CrNiMo16-5-1 (1.4418) supermartensitic stainless steel were investigated in-situ with synchrotron X-ray diffraction (XRD), dilatometry and differential scanning calorimetry (DSC) under isochronal heating conditions. Austenitization occurred...... of surface martensite formation on the XRD measurement. The applicable temperature range for DSC as well as the close proximity of the Ac1- and the Curietemperature limited the usage of the technique in the present case....

  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. Probing molecular orientations in thin films by x-ray photoelectron spectroscopy

    Science.gov (United States)

    Li, Y.; Li, P.; Lu, Z.-H.

    2018-03-01

    A great number of functional organic molecules in active thin-film layers of optoelectronic devices have highly asymmetric structures, such as plate-like, rod-like, etc. This makes molecular orientation an important aspect in thin-films as it can significantly affect both the optical and electrical performance of optoelectronic devices. With a combination of in-situ ultra violet photoelectron spectroscopy (UPS) and x-ray photoelectron spectroscopy (XPS) investigations for organic molecules having a broad range of structural properties, we discovered a rigid connection of core levels and frontier highest occupied molecular orbital levels at organic interfaces. This finding opens up opportunities of using X-ray photoemission spectroscopy as an alternative tool to UPS for providing an easy and unambiguous data interpretation in probing molecular orientations.

  20. Trends in hard X-ray fluorescence mapping: environmental applications in the age of fast detectors

    Energy Technology Data Exchange (ETDEWEB)

    Lombi, E.; Donner, E. [University of South Australia, Centre for Environmental Risk Assessment and Remediation, Mawson Lakes, South Australia (Australia); CRC CARE, PO Box 486, Salisbury, South Australia (Australia); Jonge, M.D. de; Paterson, D. [Australian Synchrotron, X-ray Fluorescence Microscopy, 800 Blackburn Road, Clayton, Victoria (Australia); Ryan, C.G. [CSIRO Earth Science and Resource Engineering, Normanby Road, Clayton, Victoria (Australia)

    2011-06-15

    Environmental samples are extremely diverse but share a tendency for heterogeneity and complexity. This heterogeneity poses methodological challenges when investigating biogeochemical processes. In recent years, the development of analytical tools capable of probing element distribution and speciation at the microscale have allowed this challenge to be addressed. Of these available tools, laterally resolved synchrotron techniques such as X-ray fluorescence mapping are key methods for the in situ investigation of micronutrients and inorganic contaminants in environmental samples. This article demonstrates how recent advances in X-ray fluorescence detector technology are bringing new possibilities to environmental research. Fast detectors are helping to circumvent major issues such as X-ray beam damage of hydrated samples, as dwell times during scanning are reduced. They are also helping to reduce temporal beamtime requirements, making particularly time-consuming techniques such as micro X-ray fluorescence ({mu}XRF) tomography increasingly feasible. This article focuses on {mu}XRF mapping of nutrients and metalloids in environmental samples, and suggests that the current divide between mapping and speciation techniques will be increasingly blurred by the development of combined approaches. (orig.)

  1. Small angle X ray diffraction investigation of twinned opal_like structures

    NARCIS (Netherlands)

    Samusev, A.K.; Sinev, I.S.; Samusev, K.B.; Rybin, M.V.; Mistonov, A.A.; Grigoryeva, N.A.; Grigoriev, S.V.; Petukhov, A.V.; Byelov, D.; Trofimova, E.Y.; Kurdyukov, D.A.; Golubev, V.G.; Limonov, M.F.

    2012-01-01

    Small angle X ray diffraction from synthetic opal films has been investigated as a function of the orientation of the sample. All the observed (hkl) diffraction reflections have been interpreted. The reconstruct tion of the reciprocal lattice of the studied opal films has been carried out. The

  2. 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.

  3. Nanoscale characterization of local structures and defects in photonic crystals using synchrotron-based transmission soft X-ray microscopy

    Science.gov (United States)

    Nho, Hyun Woo; Kalegowda, Yogesh; Shin, Hyun-Joon; Yoon, Tae Hyun

    2016-01-01

    For the structural characterization of the polystyrene (PS)-based photonic crystals (PCs), fast and direct imaging capabilities of full field transmission X-ray microscopy (TXM) were demonstrated at soft X-ray energy. PS-based PCs were prepared on an O2-plasma treated Si3N4 window and their local structures and defects were investigated using this label-free TXM technique with an image acquisition speed of ~10 sec/frame and marginal radiation damage. Micro-domains of face-centered cubic (FCC (111)) and hexagonal close-packed (HCP (0001)) structures were dominantly found in PS-based PCs, while point and line defects, FCC (100), and 12-fold symmetry structures were also identified as minor components. Additionally, in situ observation capability for hydrated samples and 3D tomographic reconstruction of TXM images were also demonstrated. This soft X-ray full field TXM technique with faster image acquisition speed, in situ observation, and 3D tomography capability can be complementally used with the other X-ray microscopic techniques (i.e., scanning transmission X-ray microscopy, STXM) as well as conventional characterization methods (e.g., electron microscopic and optical/fluorescence microscopic techniques) for clearer structure identification of self-assembled PCs and better understanding of the relationship between their structures and resultant optical properties. PMID:27087141

  4. Evaluation of an in-situ x-ray fluorescence analyzer for inorganic pollutants in sediments and water columns

    International Nuclear Information System (INIS)

    Wogman, N.A.

    1979-09-01

    The applicability of an energy dispersive x-ray fluorescence spectrometer for measurement of trace elements in sediments and in water columns from Coast Guard vessels has been investigated. This investigation was conducted in both freshwater and saltwater areas and included Puget Sound, Lake Washington, Lake Union, and the ship canal in the State of Washington. The spectrometer system consisted of a solid cryogen-cooled Si(Li) detector and a 109 Cd excitation source. Sediments and water columns were viewed through a 0.2 mm Be window. This study showed the feasibility of measuring trace elements at concentrations ranging from 20 to about 100 ppM. Measurements of this sensitivity with a 100 mCi 109 Cd source are possible for time intervals as short as 5 minutes. This in-situ measurement capability permits the on-site mapping of pollution and avoids the problem of sediment disturbance which is inherent in the collection of grab samples of the sediment surface. Recommendations for an improved analyzer system included a detector assembly which could be towed, or allow continuous sediment surface analysis thereby recording the average composition of a large area

  5. Radiobiological investigations of soft X-rays near carbon, nitrogen, oxygen K-shell edges on Aspergillus oryzae spores

    International Nuclear Information System (INIS)

    Chen, L.; Jiang, S. P.; Wan, L. B.; Ma, X. D.; Li, M. F.

    2008-01-01

    Soft X-rays at carbon, nitrogen, oxygen K-shell edges have special radiobiological effects. Using Aspergillus oryzae spores as sample, the radiation effects of soft X-rays near the K-shell edges of C, N and O elements from synchrotron radiation were investigated. Also the dose depositions of different X-ray energies in spore were discussed. At the same time, the spores were irradiated by gamma rays from 60 Co and relative biological effects were compared with those produced by soft X-rays. The results showed that soft X-rays near K-shell edges of O element had higher ability of radiation damage than that of X-rays near K-shell edges of C and N elements as compared with one another. But they all had higher killing abilities per unit dose than that of gamma rays from 60 Co. The relative biological effects (RBEs), the comparison of dose to gamma rays at 10% survival level, of the three soft X-rays were 1.65, 1.73 and 1.91, respectively. (authors)

  6. 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.

  7. 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

  8. Phase-contrast X-ray CT

    Energy Technology Data Exchange (ETDEWEB)

    Momose, Atsushi [Hitachi Ltd., Saitama (Japan). Advanced Research Laboratory; Takeda, Tohoru; Itai, Yuji

    1995-12-01

    Phase-contrast X-ray computed tomography (CT) enabling the observation of biological soft tissues without contrast enhancement has been developed. The X-ray phase shift caused by an object is measured and input to a standard CT reconstruction algorithm. A thousand times increase in the image sensitivity to soft tissues is achieved compared with the conventional CT using absorption contrast. This is because the X-ray phase shift cross section of light elements is about a thousand times larger than the absorption cross section. The phase shift is detected using an X-ray interferometer and computer analyses of interference patterns. Experiments were performed using a synchrotron X-ray source. Excellent image sensitivity is demonstrated in the observation of cancerous rabbit liver. The CT images distinguish cancer lesion from normal liver tissue and, moreover, visualize the pathological condition in the lesion. Although the X-ray energy employed and the present observation area size are not suitable for medical applications as they are, phase-contrast X-ray CT is promising for investigating the internal structure of soft tissue which is almost transparent for X-rays. The high sensitivity also provides the advantage of reducing X-ray doses. (author).

  9. 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....

  10. 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

  11. 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

  12. Investigation of optimal scanning protocol for X-ray computed tomography polymer gel dosimetry

    Energy Technology Data Exchange (ETDEWEB)

    Sellakumar, P. [Bangalore Institute of Oncology, 44-45/2, II Cross, RRMR Extension, Bangalore 560 027 (India)], E-mail: psellakumar@rediffmail.com; James Jebaseelan Samuel, E. [School of Science and Humanities, VIT University, Vellore 632 014 (India); Supe, Sanjay S. [Department of Radiation Physics, Kidwai Memorial Institute of Oncology, Hosur Road, Bangalore 560 027 (India)

    2007-11-15

    X-ray computed tomography is one of the potential tool used to evaluate the polymer gel dosimeters in three dimensions. The purpose of this study is to investigate the factors which affect the image noise for X-ray CT polymer gel dosimetry. A cylindrical water filled phantom was imaged with single slice Siemens Somatom Emotion CT scanner. The imaging parameters like tube voltage, tube current, slice scan time, slice thickness and reconstruction algorithm were varied independently to study the dependence of noise on each other. Reductions of noise with number of images to be averaged and spatial uniformity of the image were also investigated. Normoxic polymer gel PAGAT was manufactured and irradiated using Siemens Primus linear accelerator. The radiation induced change in CT number was evaluated using X-ray CT scanner. From this study it is clear that image noise is reduced with increase in tube voltage, tube current, slice scan time, slice thickness and also reduced with increasing the number of images averaged. However to reduce the tube load and total scan time, it was concluded that tube voltage of 130 kV, tube current of 200 mA, scan time of 1.5 s, slice thickness of 3 mm for high dose gradient and 5 mm for low dose gradient were optimal scanning protocols for this scanner. Optimum number of images to be averaged was concluded to be 25 for X-ray CT polymer gel dosimetry. Choice of reconstruction algorithm was also critical. From the study it is also clear that CT number increase with imaging tube voltage and shows the energy dependency of polymer gel dosimeter. Hence for evaluation of polymer gel dosimeters with X-ray CT scanner needs the optimization of scanning protocols to reduce the image noise.

  13. 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)

  14. A multiple CCD X-ray detector and its first operation with synchrotron radiation X-ray beam

    CERN Document Server

    Suzuki, M; Kumasaka, T; Sato, K; Toyokawa, H; Aries, I F; Jerram, P A; Ueki, T

    1999-01-01

    A 4x4 array structure of 16 identical CCD X-ray detector modules, called the multiple CCD X-ray detector system (MCCDX), was submitted to its first synchrotron radiation experiment at the protein crystallography station of the RIKEN beamline (BL45XU) at the SPring-8 facility. An X-ray diffraction pattern of cholesterol powder was specifically taken in order to investigate the overall system performance.

  15. 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.

  16. 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....

  17. X-ray generation by femtosecond laser pulses and its application to soft X-ray imaging microscope

    International Nuclear Information System (INIS)

    Ikeda, Kenichi; Kotaki, Hideyuki; Nakajima, Kazuhisa

    2002-01-01

    We have developed laser-produced plasma X-ray sources using femtosecond laser pulses at 10Hz repetition rate in a table-top size in order to investigate basic mechanism of X-ray emission from laser-matter interactions and its application to a X-ray microscope. In a soft X-ray region over 5 nm wavelength, laser-plasma X-ray emission from a solid target achieved an intense flux of photons of the order of 1011 photons/rad per pulse with duration of a few 100 ps, which is intense enough to make a clear imaging in a short time exposure. As an application of laser-produced plasma X-ray source, we have developed a soft X-ray imaging microscope operating in the wavelength range around 14 nm. The microscope consists of a cylindrically ellipsoidal condenser mirror and a Schwarzshird objective mirror with highly-reflective multilayers. We report preliminary results of performance tests of the soft X-ray imaging microscope with a compact laser-produced plasma X-ray source

  18. 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

  19. 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...

  20. Probing molecular orientations in thin films by x-ray photoelectron spectroscopy

    Directory of Open Access Journals (Sweden)

    Y. Li

    2018-03-01

    Full Text Available A great number of functional organic molecules in active thin-film layers of optoelectronic devices have highly asymmetric structures, such as plate-like, rod-like, etc. This makes molecular orientation an important aspect in thin-films as it can significantly affect both the optical and electrical performance of optoelectronic devices. With a combination of in-situ ultra violet photoelectron spectroscopy (UPS and x-ray photoelectron spectroscopy (XPS investigations for organic molecules having a broad range of structural properties, we discovered a rigid connection of core levels and frontier highest occupied molecular orbital levels at organic interfaces. This finding opens up opportunities of using X-ray photoemission spectroscopy as an alternative tool to UPS for providing an easy and unambiguous data interpretation in probing molecular orientations.

  1. Investigation of the human spleen by X-ray microanalysis

    International Nuclear Information System (INIS)

    Kopani, M.; Jakubovsky, J.; Polak, S.

    2001-01-01

    Qualitative and quantitative topographic analysis using X-ray fluorescence (XRF), X-ray powder diffraction (XRD) and scanning electron microscopy was performed in tissue samples of rat and human spleens. The presence of silico-aluminium and silico-calcareous particles of various sizes could be seen. The presence of the inorganic substances mentioned in the human red pulp cords is assumed to be a consequence of the purifying function of the spleen. (Authors)

  2. 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

  3. 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

  4. Application of synchrotron radiation X-ray computed tomography to investigate the agglomerating behavior of TiB2 particles in aluminum

    International Nuclear Information System (INIS)

    Chen, Fei; Mao, Feng; Chen, Zongning; Han, Jingyu; Yan, Guangyuan; Wang, Tongmin; Cao, Zhiqiang

    2015-01-01

    Highlights: • SR-CT was a powerful tool to investigate the TiB 2 distribution in Al-TiB 2 in situ composites. • Three kinds of agglomerations frequently present in the composites. • Agglomerations formed via the diffused atoms reacting with intermediate products. • The composites containing agglomerations show a much reduced ductility. - Abstract: Agglomeration of reinforcing particles has a number of deleterious effects on the properties of in situ metal matrix composites (MMCs). In order to better understand this phenomenon, the agglomerating behavior of TiB 2 particles in aluminum based in situ MMCs was investigated using synchrotron radiation X-ray computed tomography (SR-CT) and field emission scanning electron microscope (FESEM). SR-CT was shown to be a powerful tool for visualizing and quantifying the three-dimensional (3D) features within the composites. Based on the SR-CT and FESEM results, a formation mechanism of the flaky agglomerates, flocculent agglomerates and clusters of coarse TiB 2 particles, which are most frequently presented in the in situ Al/TiB 2 composite, has been proposed. The mechanism shows that the formation of these three kinds of agglomerates can be attributed to three parallel processes, i.e. diffusing titanium atoms reacting with AlB 2 , aluminum melt directly reacting with emulsified salt, diffusing boron atoms reacting with TiAl 3 , respectively. Moreover, the mechanism may shed some light on how to design better processing techniques for obtaining homogenous particle distribution in in situ Al/TiB 2 composites in the future

  5. Detector calibration for in-situ gamma ray spectrometry

    CERN Document Server

    Balea, G

    2002-01-01

    The power in the technique of in-situ spectrometry lies in the fact that a detector placed on ground measures gamma radiation from sources situated over an area of several hundred square meters. The 'field of view' for the detector would be larger for high energy radiation sources and for sources closer to the soil surface. In contrast, a soil sample would represent an area of a few tens of hundreds of square centimeters. In practice, an effective characterization of a site would involve in-situ gamma ray spectrometry in conjunction with soil sampling. As part of an overall program, in-situ gamma ray spectrometry provides a means to assess the degree of contamination in areas during the course of operations in the field, thus guiding the investigator on where to collect samples. It can also substantially reduce the number of samples need to be collected and subsequently analyzed. (author)

  6. 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.

  7. Investigation of multilayered nanocomposites as low energy X-Rays attenuators

    Energy Technology Data Exchange (ETDEWEB)

    Silva, Liliane; Batista, Adriana S.M.; Nascimento, Jefferson P.; Furtado, Clascídia A.; Faria, Luiz O., E-mail: asfisica@gmail.com, E-mail: adriananuclear@yahoo.com.br, E-mail: farialo@cdtn.br, E-mail: nascimentopatricio@yahoo.com.br, E-mail: clas@cdtn.br [Universidade Federal de Minas Gerais (UFMG), Belo Horizonte, MG (Brazil); Centro de Desenvolvimento da Tecnologia Nuclear (CDTN/CNEN-MG), Belo Horizonte, MG (Brazil)

    2017-11-01

    The development of radiation attenuating materials has application in radioprotection and conditioning of short-lived waste. Polymeric materials can serve as a matrix for the dispersion of nanomaterials with good attenuation features, resulting in lightweight, conformable, flexible and easy-to-process materials. Thus, some well-known shielding materials could be used in low proportion for the formation of new materials. On the other hand, nanostructured carbon materials, such as graphene oxide (GO) and carbon nanotubes (NTCs), have been reported recently to show enhanced attenuation properties. In this sense, polymeric matrixes provide the necessary flexibility for use in various applications that require molding. For the present work, poly(vinylidene fluoride) [PVDF] homopolymers and its fluorinated copolymers were filled with nanosized metallic and graphene oxides in order to produce nanocomposites with increased low energy X-ray attenuation efficiency. Film samples of PVDF/reduced Graphene Oxide [PVDF/rGO] and Poly(vinylidene fluoride – tryfluorethylene)/Barium Oxide [P(VDF-TrFE)/BaO] were synthesized. In a second step, the samples were then sandwiched between Kapton® layers and exposed to X-rays source (8.5 keV). The samples were characterized with Scanning Electron Microscopy (SEM) and Energy Dispersive Spectroscopy (EDS). The attenuation coefficient was evaluated and compared with the attenuation of the individual constituents. It was observed an increase in the linear attenuation coefficient of the layered materials, justifying further investigation of these nanostructured composites as X-ray or gamma radiation attenuators. (author)

  8. Investigation of multilayered nanocomposites as low energy X-Rays attenuators

    International Nuclear Information System (INIS)

    Silva, Liliane; Batista, Adriana S.M.; Nascimento, Jefferson P.; Furtado, Clascídia A.; Faria, Luiz O.

    2017-01-01

    The development of radiation attenuating materials has application in radioprotection and conditioning of short-lived waste. Polymeric materials can serve as a matrix for the dispersion of nanomaterials with good attenuation features, resulting in lightweight, conformable, flexible and easy-to-process materials. Thus, some well-known shielding materials could be used in low proportion for the formation of new materials. On the other hand, nanostructured carbon materials, such as graphene oxide (GO) and carbon nanotubes (NTCs), have been reported recently to show enhanced attenuation properties. In this sense, polymeric matrixes provide the necessary flexibility for use in various applications that require molding. For the present work, poly(vinylidene fluoride) [PVDF] homopolymers and its fluorinated copolymers were filled with nanosized metallic and graphene oxides in order to produce nanocomposites with increased low energy X-ray attenuation efficiency. Film samples of PVDF/reduced Graphene Oxide [PVDF/rGO] and Poly(vinylidene fluoride – tryfluorethylene)/Barium Oxide [P(VDF-TrFE)/BaO] were synthesized. In a second step, the samples were then sandwiched between Kapton® layers and exposed to X-rays source (8.5 keV). The samples were characterized with Scanning Electron Microscopy (SEM) and Energy Dispersive Spectroscopy (EDS). The attenuation coefficient was evaluated and compared with the attenuation of the individual constituents. It was observed an increase in the linear attenuation coefficient of the layered materials, justifying further investigation of these nanostructured composites as X-ray or gamma radiation attenuators. (author)

  9. A new cell for temperature-dependent X-ray absorption spectroscopy of liquid solutions: application to PbBr2 solutions in diethylene glycol.

    Science.gov (United States)

    Lützenkirchen-Hecht, D; Oldag, T; Keil, P; Keller, H L; Frahm, R

    2005-03-01

    An in situ cell has been constructed for temperature-dependent X-ray absorption experiments (EXAFS and XANES) of lead bromine (PbBr2) solutions in diethylene glycol in the temperature range from room temperature up to about 433 K. The solution is kept in a thermostated container made of carbon-reinforced teflon between two thin chemically inert quartz glass windows with a high transmission for hard X-rays. The construction of the cell ensures that these X-ray windows are thermalized so that any possible precipitation of solid products from the solution is inhibited. The cell consists mainly of two hermetically sealed teflon containers for the thermostating fluid (silicon oil) that were fitted together in such a way that a small and variable volume (approximately 2-4 cm3) for the liquid under investigation was achieved. A small thermocouple in a glass enclosure was placed in the solution to maintain temperature control and feedback to the thermostat. The cell design and its performance for temperature-dependent in situ investigations with X-rays are reported. Some preliminary results obtained for PbBr2 solutions in diethylene glycol are given.

  10. Development of quantitative x-ray microtomography

    International Nuclear Information System (INIS)

    Deckman, H.W.; Dunsmuir, J.A.; D'Amico, K.L.; Ferguson, S.R.; Flannery, B.P.

    1990-01-01

    The authors have developed several x-ray microtomography systems which function as quantitative three dimensional x-ray microscopes. In this paper the authors describe the evolutionary path followed from making the first high resolution experimental microscopes to later generations which can be routinely used for investigating materials. Developing the instrumentation for reliable quantitative x-ray microscopy using synchrotron and laboratory based x-ray sources has led to other imaging modalities for obtaining temporal and spatial two dimensional information

  11. 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

  12. 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.)

  13. X-Ray-induced Deuterium Enrichment of N-rich Organics in Protoplanetary Disks: An Experimental Investigation Using Synchrotron Light

    Energy Technology Data Exchange (ETDEWEB)

    Gavilan, Lisseth; Carrasco, Nathalie [LATMOS, Université Versailles St Quentin, UPMC Université Paris 06, CNRS, 11 blvd d’Alembert, F-78280 Guyancourt (France); Remusat, Laurent; Roskosz, Mathieu [IMPMC, CNRS UMR 7590, Sorbonne Universités, UPMC Université Paris 06, IRD, Muséum National d’Histoire Naturelle, CP 52, 57 rue Cuvier, Paris F-75231 (France); Popescu, Horia; Jaouen, Nicolas [SEXTANTS beamline, SOLEIL synchrotron, L’Orme des Merisiers, F-91190 Saint-Aubin (France); Sandt, Christophe [SMIS beamline, SOLEIL synchrotron, L’Orme des Merisiers, F-91190 Saint-Aubin (France); Jäger, Cornelia [Laboratory Astrophysics and Cluster Physics Group of the Max Planck Institute for Astronomy at the Friedrich Schiller University and Institute of Solid State Physics, Helmholtzweg 3, D-07743 Jena (Germany); Henning, Thomas [Max-Planck Institute for Astronomy Königstuhl 17, D-69117 Heidelberg (Germany); Simionovici, Alexandre [Institut des Sciences de la Terre, Observatoire des Sciences de l’Univers de Grenoble, BP 53, F-38041 Grenoble (France); Lemaire, Jean Louis [Institut des Sciences Moléculaires d’Orsay (ISMO), CNRS, Univ. Paris Sud, Université Paris-Saclay, F-91405 Orsay (France); Mangin, Denis, E-mail: lisseth.gavilan@latmos.ipsl.fr [Institut Jean Lamour, CNRS, Université de Lorraine, F-54011 Nancy (France)

    2017-05-01

    The deuterium enrichment of organics in the interstellar medium, protoplanetary disks, and meteorites has been proposed to be the result of ionizing radiation. The goal of this study is to simulate and quantify the effects of soft X-rays (0.1–2 keV), an important component of stellar radiation fields illuminating protoplanetary disks, on the refractory organics present in the disks. We prepared tholins, nitrogen-rich organic analogs to solids found in several astrophysical environments, e.g., Titan’s atmosphere, cometary surfaces, and protoplanetary disks, via plasma deposition. Controlled irradiation experiments with soft X-rays at 0.5 and 1.3 keV were performed at the SEXTANTS beamline of the SOLEIL synchrotron, and were immediately followed by ex-situ infrared, Raman, and isotopic diagnostics. Infrared spectroscopy revealed the preferential loss of singly bonded groups (N–H, C–H, and R–N≡C) and the formation of sp{sup 3} carbon defects with signatures at ∼1250–1300 cm{sup −1}. Raman analysis revealed that, while the length of polyaromatic units is only slightly modified, the introduction of defects leads to structural amorphization. Finally, tholins were measured via secondary ion mass spectrometry to quantify the D, H, and C elemental abundances in the irradiated versus non-irradiated areas. Isotopic analysis revealed that significant D-enrichment is induced by X-ray irradiation. Our results are compared to previous experimental studies involving the thermal degradation and electron irradiation of organics. The penetration depth of soft X-rays in μ m-sized tholins leads to volume rather than surface modifications: lower-energy X-rays (0.5 keV) induce a larger D-enrichment than 1.3 keV X-rays, reaching a plateau for doses larger than 5 × 10{sup 27} eV cm{sup −3}. Synchrotron fluences fall within the expected soft X-ray fluences in protoplanetary disks, and thus provide evidence of a new non-thermal pathway to deuterium fractionation of

  14. X-Ray-induced Deuterium Enrichment of N-rich Organics in Protoplanetary Disks: An Experimental Investigation Using Synchrotron Light

    Science.gov (United States)

    Gavilan, Lisseth; Remusat, Laurent; Roskosz, Mathieu; Popescu, Horia; Jaouen, Nicolas; Sandt, Christophe; Jäger, Cornelia; Henning, Thomas; Simionovici, Alexandre; Lemaire, Jean Louis; Mangin, Denis; Carrasco, Nathalie

    2017-05-01

    The deuterium enrichment of organics in the interstellar medium, protoplanetary disks, and meteorites has been proposed to be the result of ionizing radiation. The goal of this study is to simulate and quantify the effects of soft X-rays (0.1-2 keV), an important component of stellar radiation fields illuminating protoplanetary disks, on the refractory organics present in the disks. We prepared tholins, nitrogen-rich organic analogs to solids found in several astrophysical environments, e.g., Titan’s atmosphere, cometary surfaces, and protoplanetary disks, via plasma deposition. Controlled irradiation experiments with soft X-rays at 0.5 and 1.3 keV were performed at the SEXTANTS beamline of the SOLEIL synchrotron, and were immediately followed by ex-situ infrared, Raman, and isotopic diagnostics. Infrared spectroscopy revealed the preferential loss of singly bonded groups (N-H, C-H, and R-N≡C) and the formation of sp3 carbon defects with signatures at ˜1250-1300 cm-1. Raman analysis revealed that, while the length of polyaromatic units is only slightly modified, the introduction of defects leads to structural amorphization. Finally, tholins were measured via secondary ion mass spectrometry to quantify the D, H, and C elemental abundances in the irradiated versus non-irradiated areas. Isotopic analysis revealed that significant D-enrichment is induced by X-ray irradiation. Our results are compared to previous experimental studies involving the thermal degradation and electron irradiation of organics. The penetration depth of soft X-rays in μm-sized tholins leads to volume rather than surface modifications: lower-energy X-rays (0.5 keV) induce a larger D-enrichment than 1.3 keV X-rays, reaching a plateau for doses larger than 5 × 1027 eV cm-3. Synchrotron fluences fall within the expected soft X-ray fluences in protoplanetary disks, and thus provide evidence of a new non-thermal pathway to deuterium fractionation of organic matter.

  15. 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.

  16. 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

  17. 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

  18. 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...

  19. 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.)

  20. The X-ray Astronomy Recovery Mission

    Science.gov (United States)

    Tashiro, M.; Kelley, R.

    2017-10-01

    On 25 March 2016, the Japanese 6th X-ray astronomical satellite ASTRO-H (Hitomi), launched on February 17, lost communication after a series of mishap in its attitude control system. In response to the mishap the X-ray astronomy community and JAXA analyzed the direct and root cause of the mishap and investigated possibility of a recovery mission with the international collaborator NASA and ESA. Thanks to great effort of scientists, agencies, and governments, the X-ray Astronomy Recovery Mission (XARM) are proposed. The recovery mission is planned to resume high resolution X-ray spectroscopy with imaging realized by Hitomi under the international collaboration in the shortest time possible, simply by focusing one of the main science goals of Hitomi Resolving astrophysical problems by precise high-resolution X-ray spectroscopy'. XARM will carry a 6 x 6 pixelized X-ray micro-calorimeter on the focal plane of an X-ray mirror assembly, and an aligned X-ray CCD camera covering the same energy band and wider field of view, but no hard X-ray or soft gamma-ray instruments are onboard. In this paper, we introduce the science objectives, mission concept, and schedule of XARM.

  1. 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.)

  2. Synchronization of x-ray pulses to the pump laser in an ultrafast x-ray facility

    International Nuclear Information System (INIS)

    Corlett, J.N.; Barry, W.; Byrd, J.M.; Schoenlein, R.; Zholents, A.

    2002-01-01

    Accurate timing of ultrafast x-ray probe pulses emitted from a synchrotron radiation source with respect to a pump laser exciting processes in the sample under study is critical for the investigation of structural dynamics in the femtosecond regime. We describe a scheme for synchronizing femtosecond x-ray pulses relative to a pump laser. X-ray pulses of <100 fs duration are generated from a proposed source based on a recirculating superconducting linac [1,2,3]. Short x-ray pulses are obtained by a process of electron pulse compression, followed by transverse temporal correlation of the electrons, and ultimately x-ray pulse compression. Timing of the arrival of the x-ray pulse with respect to the pump laser is found to be dominated by the operation of the deflecting cavities which provide the transverse temporal correlation of the electrons. The deflecting cavities are driven from a highly stable RF signal derived from a modelocked laser oscillator which is also the origin of the pump l aser pulses

  3. 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.

  4. 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.

  5. Extended X-ray absorption fine structure investigation of nitrogen stabilized expanded austenite

    DEFF Research Database (Denmark)

    Oddershede, Jette; Christiansen, Thomas; Ståhl, Kenny

    2010-01-01

    As-delivered austenitic stainless steel and nitrogen stabilized expanded austenite, both fully nitrided and denitrided (in H2), were investigated with Cr, Fe and Ni extended X-ray absorption fine structure. The data shows pronounced short-range ordering of Cr and N. For the denitrided specimen...

  6. 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 ...

  7. 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

  8. 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

  9. 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

  10. Non-destructive investigations of Swiss museums objects with neutron and x-ray imaging methods

    International Nuclear Information System (INIS)

    Lehmann, E.H.; Deschler, E.; Pernet, L.; Vontobel, P.

    2004-01-01

    Many objects of archaeological relevance found in Switzerland are from the Celtic and Roman era. Because of their uniqueness in most cases it is demanded to perform any investigation with such samples non-destructively. Depending on the structure and size of the objects a transmission experiment performed either with X-ray or neutron can alight inner structures, composition, defects or the principles of the manufacturing procedures. Furthermore, the treatment by conservators and restaurateurs becomes visible in many cases. This report describes some examples of such investigations. In the case of neutron investigations, beside the transmission imaging as a radiograph the three-dimensional structure was observed with a tomography technique. For X-ray radiography, the images were obtained in the same digital format because the similar experimental method (imaging plates) was applied. It becomes evident in the described examples that the combination and complementary use of both methods (neutrons and X-ray) brings insights in different aspects of the samples properties and treatment. This approach to study museums objects stored and exhibit in Switzerland can be extrapolated to other countries where these techniques are also simultaneously available in order to investigate other objects of relevance. The European network COST-G8 entitled 'Non-destructive analysis and testing of museum objects' can help to support initiatives in this direction. (author)

  11. 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

  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. 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.

  15. 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

  16. 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.

  17. 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

  18. 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)

  19. X-ray investigation of intermetallides and their hydrides under hydrogen pressure in H2-LaNi5 system

    International Nuclear Information System (INIS)

    Karonik, V.V.; Tsypin, M.I.; Prokof'ev, M.V.; Kazakov, D.N.

    1983-01-01

    X-ray phase analysis has been used to investigate phase composition of LaNi 5 -H 2 system; comparison of X-ray diffraction data with the results of plotting absorption and desorption isotherms is conducted. Technique of the X-ray diffraction study of intermetallide-hydrogen system using special X-ray chamber to diffractometer DRON-1.5 (GUR-5) is worked out. The parameters of elementary cell of the LaNisub(5)Hsub(6.2) hydride are determined: a=0.541(2) pm, c=0.430(2) nm, c/a=0.795, V=0.109 nm 3 (hexagonal syngony)

  20. 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.

  1. 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)

  2. 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.

  3. In situ X-ray near-edge absorption spectroscopy investigation of the state of charge of all-vanadium redox flow batteries.

    Science.gov (United States)

    Jia, Chuankun; Liu, Qi; Sun, Cheng-Jun; Yang, Fan; Ren, Yang; Heald, Steve M; Liu, Yadong; Li, Zhe-Fei; Lu, Wenquan; Xie, Jian

    2014-10-22

    Synchrotron-based in situ X-ray near-edge absorption spectroscopy (XANES) has been used to study the valence state evolution of the vanadium ion for both the catholyte and anolyte in all-vanadium redox flow batteries (VRB) under realistic cycling conditions. The results indicate that, when using the widely used charge-discharge profile during the first charge process (charging the VRB cell to 1.65 V under a constant current mode), the vanadium ion valence did not reach V(V) in the catholyte and did not reach V(II) in the anolyte. Consequently, the state of charge (SOC) for the VRB cell was only 82%, far below the desired 100% SOC. Thus, such incompletely charged mix electrolytes results in not only wasting the electrolytes but also decreasing the cell performance in the following cycles. On the basis of our study, we proposed a new charge-discharge profile (first charged at a constant current mode up to 1.65 V and then continuously charged at a constant voltage mode until the capacity was close to the theoretical value) for the first charge process that achieved 100% SOC after the initial charge process. Utilizing this new charge-discharge profile, the theoretical charge capacity and the full utilization of electrolytes has been achieved, thus having a significant impact on the cost reduction of the electrolytes in VRB.

  4. 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)

  5. 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)

  6. Structural investigation of semi-conductor nanostructures by x-ray diffraction

    International Nuclear Information System (INIS)

    Stangl, J.

    2003-01-01

    Full text: Semiconductor nanostructures present a topic of increasing interest due to their potential for new device concepts, as well as from a scientific point of view. In structures with dimensions smaller than the DeBroglie wavelength of electrons or holes, quantum confinement effects determine the electronic and optical properties. For the understanding of such structures, their structural investigation, i.e., the determination of size, shape, chemical composition and strain state is mandatory. X-ray diffraction is a powerful technique for this purpose. In particular, the strain fields within nanostructures as well as in the surrounding matrix can be determined with high precision. Using synchrotron radiation sources, also the distribution of chemical composition within objects with typically several nm height and 10 to 100 nm width can be established. With x-ray diffraction, the non-destructive investigation of uncapped and buried structures is possible. The latter is important, as for applications buried structures are needed, and during capping the structural properties may change considerably. Here, we will focus on so-called self-assembled nanostructures, which form during the deposition of different semiconductors on top of each other. In contrast to structures etched after growth of planar layers, self organized islands or wires are virtually defect-free and hence promising for applications. Different scattering techniques sensitive to shape and/or composition and strain will be discussed. (author)

  7. X-ray topographic method of investigation of phase objects

    International Nuclear Information System (INIS)

    Levonyan, L.V.

    2001-01-01

    The intensity distribution of the monochromatized synchrotron radiation transmitting through the phase object and crystal-analyzer in Laue geometry is considered. It is shown that the local angular deviation of the incident radiation caused by the refraction on structural inhomogeneities of the object under investigation is directly transferred to the X-ray topographic image. In the absence of the phase object the latter consists of parallel straight fringes with a slowly decreasing period. The presence of the phase object changes the shape and period of fringes. The influence of the spatial and temporal coherence on the image is discussed. 5 refs

  8. 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 ...

  9. 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 ...

  10. 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)

  11. X-ray investigation of Nb/O interfaces

    International Nuclear Information System (INIS)

    Delheusy, Melissa

    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 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 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.)

  12. 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.

  13. 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

  14. Investigation of chemical vapour deposition diamond detectors by X-ray micro-beam induced current and X-ray micro-beam induced luminescence techniques

    International Nuclear Information System (INIS)

    Olivero, P.; Manfredotti, C.; Vittone, E.; Fizzotti, F.; Paolini, C.; Lo Giudice, A.; Barrett, R.; Tucoulou, R.

    2004-01-01

    Tracking detectors have become an important ingredient in high-energy physics experiments. In order to survive the harsh detection environment of the large hadron collider (LHC), trackers need to have special properties. They must be radiation hard, provide fast collection of charge, be as thin as possible and remove heat from readout electronics. The unique properties of diamond allow it to fulfill these requirements. In this work we present an investigation of the charge transport and luminescence properties of 'detector grade' artificial chemical vapour deposition (CVD) diamond devices developed within the CERN RD42 collaboration, performed by means of X-ray micro-beam induced current collection (XBICC) and X-ray micro-beam induced luminescence (XBIL) techniques. XBICC technique allows quantitative estimates of the transport parameters of the material to be evaluated and mapped with micrometric spatial resolution. In particular, the high resolution and sensitivity of the technique has allowed a quantitative study of the inhomogeneity of the charge transport parameter defined as the product of mobility and lifetime for both electron and holes. XBIL represents a technique complementary to ion beam induced luminescence (IBIL), which has already been used by our group, since X-ray energy loss profile in the material is different from that of MeV ions. X-ray induced luminescence maps have been performed simultaneously with induced photocurrent maps, to correlate charge transport and induced luminescence properties of diamond. Simultaneous XBICC and XBIL maps exhibit features of partial complementarity that have been interpreted on the basis of considerations on radiative and non-radiative recombination processes which compete with charge transport efficiency

  15. In situ chemical state analysis of buried polymer/metal adhesive interface by hard X-ray photoelectron spectroscopy

    International Nuclear Information System (INIS)

    Ozawa, Kenichi; Kakubo, Takashi; Shimizu, Katsunori; Amino, Naoya; Mase, Kazuhiko; Ikenaga, Eiji; Nakamura, Tetsuya; Kinoshita, Toyohiko; Oji, Hiroshi

    2014-01-01

    Highlights: • Chemical state analysis of the buried rubber/brass interface is conducted by HAXPES. • Ultrathin rubber films are prepared on the brass surface by two methods. • A high density of Cu 2 S is found on the rubber side of the buried adhesive layer. • The chemical states of the buried and exposed interfaces are compared. - Abstract: Chemical state analysis of adhesive interfaces is important to understand an adhesion mechanism between two different materials. Although photoelectron spectroscopy (PES) is an ideal tool for such an analysis, the adhesive interfaces must be exposed to the surface because PES is essentially a surface sensitive technique. However, an in situ observation is possible by hard X-ray PES (HAXPES) owing to its large probing depth. In the present study, HAXPES is applied to investigate the adhesive interface between rubber and brass without exposing the interface. It is demonstrated that copper sulfides formed at the buried rubber/brass interface are distinguished from S-containing species in the rubber overlayer. The chemical state of the buried interface is compared with that of the “exposed” interface prepared by so-called a filter-paper method

  16. 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

  17. An investigation of infection control for x-ray cassettes in a diagnostic imaging department

    International Nuclear Information System (INIS)

    Fox, Matthew; Harvey, Jane M.

    2008-01-01

    Introduction: This research was conducted to investigate if X-ray cassettes could be a possible source of pathogens capable of causing nosocomial infections, and if they could be a possible vector for cross infection within the hospital environment. Method: The research involved the swabbing of X-ray cassettes in a Diagnostic Imaging Department of a large hospital in the east of England. Two areas of the Diagnostic Imaging Department were included in the study. Research concentrated on X-ray cassettes used for mobile radiography, accident and emergency and inpatient use. Forty cassettes were swabbed in total specifically for general levels of bacterial contamination, also for the presence or absence of methicillin-resistant Staphylococcus aureus (MRSA). A mapping exercise was completed following the location of an X-ray cassette typically used in mobile radiography. The exercise noted the level of direct contact with patient's skin and other possible routes of infection. Results: The results demonstrated that there were large levels of growth of samples taken from cassettes and developed in the Microbiology Department. Coagulase-negative Staphylococcus, Micrococci, Diptheroids and species of Bacillus were all identified. The mapping exercise in which the journey of a 35/43 cm cassette used for mobile radiography was tracked found that contact with patient's skin and potential pathogens or routes of cross infection was a common occurrence whilst undertaking mobile radiography. Conclusion: The research has identified the presence of bacterial contamination on cassettes. The research established that X-ray cassettes/imaging plates are often exposed to pathogens and possible routes of cross infection; also that patient's skin often comes directly in contact with the X-ray cassette/imaging plate. The research also shows that as cassettes/imaging plates are a potential source of cross infection, the Diagnostic Imaging Department may be partly responsible for adding to

  18. 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)

  19. Effect of particle size, filler loadings and x-ray tube voltage on the transmitted x-ray transmission in tungsten oxide—epoxy composites

    International Nuclear Information System (INIS)

    Noor Azman, N.Z.; Siddiqui, S.A.; Hart, R.; Low, I.M.

    2013-01-01

    The effect of particle size, filler loadings and x-ray tube voltage on the x-ray transmission in WO 3 -epoxy composites has been investigated using the mammography unit and a general radiography unit. Results indicate that nano-sized WO 3 has a better ability to attenuate the x-ray beam generated by lower tube voltages (25–35 kV) when compared to micro-sized WO 3 of the same filler loading. However, the effect of particle size on x-ray transmission was negligible at the higher x-ray tube voltages (40–120 kV). - Highlights: ► Investigated the effect of particle size of WO 3 on the x-ray attenuation ability. ► Nano-sized WO 3 has a better ability to attenuate lower x-ray energies (22–49 kV p ). ► Particle size has negligible effect at the higher x-ray energy range (40–120 kV p ).

  20. Interface Energy Alignment of Atomic-Layer-Deposited VOx on Pentacene: an in Situ Photoelectron Spectroscopy Investigation.

    Science.gov (United States)

    Zhao, Ran; Gao, Yuanhong; Guo, Zheng; Su, Yantao; Wang, Xinwei

    2017-01-18

    Ultrathin atomic-layer-deposited (ALD) vanadium oxide (VO x ) interlayer has recently been demonstrated for remarkably reducing the contact resistance in organic electronic devices (Adv. Funct. Mater. 2016, 26, 4456). Herein, we present an in situ photoelectron spectroscopy investigation (including X-ray and ultraviolet photoelectron spectroscopies) of ALD VO x grown on pentacene to understand the role of the ALD VO x interlayer for the improved contact resistance. The in situ photoelectron spectroscopy characterizations allow us to monitor the ALD growth process of VO x and trace the evolutions of the work function, pentacene HOMO level, and VO x defect states during the growth. The initial VO x growth is found to be partially delayed on pentacene in the first ∼20 ALD cycles. The underneath pentacene layer is largely intact after ALD. The ALD VO x is found to contain a high density of defect states starting from 0.67 eV below the Fermi level, and the energy level of these defect states is in excellent alignment with the HOMO level of pentacene, which therefore allows these VO x defect states to provide an efficient hole-injection pathway at the contact interface.

  1. Investigation of water seepage through porous media using X-ray imaging technique

    Science.gov (United States)

    Jung, Sung Yong; Lim, Seungmin; Lee, Sang Joon

    2012-07-01

    SummaryDynamic movement of wetting front and variation of water contents through three different porous media were investigated using X-ray radiography. Water and natural sand particles were used as liquid and porous media in this study. To minimize the effects of minor X-ray attenuation and uneven illumination, the flat field correction (FFC) was applied before determining the position of wetting front. In addition, the thickness-averaged (in the direction of the X-ray penetration) water content was obtained by employing the Beer-Lambert law. The initial inertia of water droplet influences more strongly on the vertical migration, compared to the horizontal migration. The effect of initial inertia on the horizontal migration is enhanced as sand size decreases. The pattern of water transport is observed to be significantly affected by the initial water contents. As the initial water contents increases, the bulb-type transport pattern is shifted to a trapezoidal shape. With increasing surface temperature, water droplets are easily broken on the sand surface. This consequently decreases the length of the initial inertia region. Different from the wetting front migration, the water contents at the initial stage clearly exhibit a preferential flow along the vertical direction. The water transport becomes nearly uniform in all directions beyond the saturation state.

  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. 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.)

  4. 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.

  5. Fluid adsorption in ordered mesoporous solids determined by in situ small-angle X-ray scattering.

    Science.gov (United States)

    Findenegg, Gerhard H; Jähnert, Susanne; Müter, Dirk; Prass, Johannes; Paris, Oskar

    2010-07-14

    The adsorption of two organic fluids (n-pentane and perfluoropentane) in a periodic mesoporous silica material (SBA-15) is investigated by in situ small-angle X-ray scattering (SAXS) using synchrotron radiation. Structural changes are monitored as the ordered and disordered pores in the silica matrix are gradually filled with the fluids. The experiments yield integrated peak intensities from up to ten Bragg reflections from the 2D hexagonal pore lattice, and additionally diffuse scattering contributions arising from disordered (mostly intrawall) porosity. The analysis of the scattering data is based on a separation of these two contributions. Bragg scattering is described by adopting a form factor model for ordered pores of cylindrical symmetry which accounts for the filling of the microporous corona, the formation of a fluid film at the pore walls, and condensation of the fluid in the core. The filling fraction of the disordered intrawall pores is extracted from the diffuse scattering intensity and its dependence on the fluid pressure is analyzed on the basis of a three-phase model. The data analysis introduced here provides an important generalisation of a formalism presented recently (J. Phys. Chem. C, 2009, 13, 15201), which was applicable to contrast-matching fluids only. In this way, the adsorption behaviour of fluids into ordered and disordered pores in periodic mesoporous materials can be analyzed quantitatively irrespective of the fluid density.

  6. 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.

  7. Soft X-ray spectroscopic investigations in experiments on Z-pinch stabilization

    International Nuclear Information System (INIS)

    Pikuz, S.A.; Skobelev, I.Yu.

    1996-01-01

    X-ray spectroscopic methods were used to investigate the spatial distribution of Z-pinch plasma parameters. Experiments were carried out on the GAEL pulse line generator in Ecole Polytechnique (France) with different types of load. Obtained results for the concentration of electrons and plasma temperature showed that higher plasma homogeneity was obtained in experiments with complex load. Spectrograms demonstrate the stabilization effect of the A1-jet. (orig.)

  8. Soft X-ray spectroscopic investigations in experiments on Z-pinch stabilization

    Energy Technology Data Exchange (ETDEWEB)

    Pikuz, S.A. [Rossijskaya Akademiya Nauk, Moscow (Russian Federation). Fizicheskij Inst.; Shelkovenko, T.A. [Rossijskaya Akademiya Nauk, Moscow (Russian Federation). Fizicheskij Inst.; Romanova, V.M. [Rossijskaya Akademiya Nauk, Moscow (Russian Federation). Fizicheskij Inst.; Etlicher, B. [Ecole Polytechnique, Palaseau (France). Lab. de Phys. des Mililux Ionises; Attelan, S. [Ecole Polytechnique, Palaseau (France). Lab. de Phys. des Mililux Ionises; Chuvatin, A.S. [Ecole Polytechnique, Palaseau (France). Lab. de Phys. des Mililux Ionises; Faenov, A.Ya. [MISDC VNIIFTRI, Moscow (Russian Federation); Skobelev, I.Yu. [MISDC VNIIFTRI, Moscow (Russian Federation)

    1996-04-01

    X-ray spectroscopic methods were used to investigate the spatial distribution of Z-pinch plasma parameters. Experiments were carried out on the GAEL pulse line generator in Ecole Polytechnique (France) with different types of load. Obtained results for the concentration of electrons and plasma temperature showed that higher plasma homogeneity was obtained in experiments with complex load. Spectrograms demonstrate the stabilization effect of the A1-jet. (orig.).

  9. 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).

  10. 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).

  11. Glass sample preparation and performance investigations. [solar x-ray imager

    Science.gov (United States)

    Johnson, R. Barry

    1992-01-01

    This final report details the work performed under this delivery order from April 1991 through April 1992. The currently available capabilities for integrated optical performance modeling at MSFC for large and complex systems such as AXAF were investigated. The Integrated Structural Modeling (ISM) program developed by Boeing for the U.S. Air Force was obtained and installed on two DECstations 5000 at MSFC. The structural, thermal and optical analysis programs available in ISM were evaluated. As part of the optomechanical engineering activities, technical support was provided in the design of support structure, mirror assembly, filter wheel assembly and material selection for the Solar X-ray Imager (SXI) program. As part of the fabrication activities, a large number of zerodur glass samples were prepared in different sizes and shapes for acid etching, coating and polishing experiments to characterize the subsurface damage and stresses produced by the grinding and polishing operations. Various optical components for AXAF video microscope and the x-ray test facility were also fabricated. A number of glass fabrication and test instruments such as a scatter plate interferometer, a gravity feed saw and some phenolic cutting blades were fabricated, integrated and tested.

  12. Elucidating oxygen electrocatalysis with synchrotron X-rays: PEM fuel cells and electrolyzers

    DEFF Research Database (Denmark)

    Pedersen, Anders Filsøe

    In this thesis electrocatalysts for the oxygen reduction reaction (ORR) and the oxygen evolution reaction (OER) have been investigated using synchrotron based X-ray diffraction and X-ray absorption spectroscopy methods. The catalysts are based on Pt alloys and RuO2 for ORR and OER, respectively...... stability measurements showed that the in-plane compression relaxes during the first 2000-3000 cycles, explaining the loss of activity primarily in this range of cycling. For OER mass-selected nanoparticles of metallic Ru and thermally oxidized RuO2 were fabricated. Both materials are highly active for OER......, although the metallic Ru nanoparticles exceptionally so. However this comes as a trade-off in stability, as the metallic particles dissolves rapidly at OER conditions. In an in-situ XAS experiment the oxidation state of the nanoparticles were tracked as a function of potential. It was found...

  13. Soft X-ray radiation damage in EM-CCDs used for Resonant Inelastic X-ray Scattering

    Science.gov (United States)

    Gopinath, D.; Soman, M.; Holland, A.; Keelan, J.; Hall, D.; Holland, K.; Colebrook, D.

    2018-02-01

    Advancement in synchrotron and free electron laser facilities means that X-ray beams with higher intensity than ever before are being created. The high brilliance of the X-ray beam, as well as the ability to use a range of X-ray energies, means that they can be used in a wide range of applications. One such application is Resonant Inelastic X-ray Scattering (RIXS). RIXS uses the intense and tuneable X-ray beams in order to investigate the electronic structure of materials. The photons are focused onto a sample material and the scattered X-ray beam is diffracted off a high resolution grating to disperse the X-ray energies onto a position sensitive detector. Whilst several factors affect the total system energy resolution, the performance of RIXS experiments can be limited by the spatial resolution of the detector used. Electron-Multiplying CCDs (EM-CCDs) at high gain in combination with centroiding of the photon charge cloud across several detector pixels can lead to sub-pixel spatial resolution of 2-3 μm. X-ray radiation can cause damage to CCDs through ionisation damage resulting in increases in dark current and/or a shift in flat band voltage. Understanding the effect of radiation damage on EM-CCDs is important in order to predict lifetime as well as the change in performance over time. Two CCD-97s were taken to PTB at BESSY II and irradiated with large doses of soft X-rays in order to probe the front and back surfaces of the device. The dark current was shown to decay over time with two different exponential components to it. This paper will discuss the use of EM-CCDs for readout of RIXS spectrometers, and limitations on spatial resolution, together with any limitations on instrument use which may arise from X-ray-induced radiation damage.

  14. 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 ...

  15. Time-resolved X-ray absorption spectroscopy for laser-ablated silicon particles in xenon gas

    International Nuclear Information System (INIS)

    Makimura, Tetsuya; Sakuramoto, Tamaki; Murakami, Kouichi

    1996-01-01

    We developed a laboratory-scale in situ apparatus for soft X-ray absorption spectroscopy with a time resolution of 10 ns and a space resolution of 100 μm. Utilizing this spectrometer, we have investigated the dynamics of silicon atoms formed by laser ablation in xenon gas. It was found that 4d-electrons in the xenon atoms are excited through collision with electrons in the laser-generated silicon plasma. (author)

  16. Is low-energy-ion bombardment generated X-ray emission a secondary mutational source to ion-beam-induced genetic mutation?

    Energy Technology Data Exchange (ETDEWEB)

    Thongkumkoon, P. [Plasma and Beam Physics Research Facility, Department of Physics and Materials Science, Faculty of Science, Chiang Mai University, Chiang Mai 50200 (Thailand); Thailand Center of Excellence in Physics, Commission on Higher Education, 328 Si Ayutthaya Road, Bangkok 10400 (Thailand); Prakrajang, K. [Plasma and Beam Physics Research Facility, Department of Physics and Materials Science, Faculty of Science, Chiang Mai University, Chiang Mai 50200 (Thailand); Faculty of Science, Maejo University, Chiang Mai 50290 (Thailand); Thopan, P.; Yaopromsiri, C. [Plasma and Beam Physics Research Facility, Department of Physics and Materials Science, Faculty of Science, Chiang Mai University, Chiang Mai 50200 (Thailand); Suwannakachorn, D. [Plasma and Beam Physics Research Facility, Department of Physics and Materials Science, Faculty of Science, Chiang Mai University, Chiang Mai 50200 (Thailand); Thailand Center of Excellence in Physics, Commission on Higher Education, 328 Si Ayutthaya Road, Bangkok 10400 (Thailand); Yu, L.D., E-mail: yuld@fnrf.science.cmu.ac.th [Plasma and Beam Physics Research Facility, Department of Physics and Materials Science, Faculty of Science, Chiang Mai University, Chiang Mai 50200 (Thailand); Thailand Center of Excellence in Physics, Commission on Higher Education, 328 Si Ayutthaya Road, Bangkok 10400 (Thailand)

    2013-07-15

    Highlights: ► Detected X-ray emission from metal, plastic and biological samples. ► Characteristic X-ray emission was detected from metal but not from non-metals. ► Low-energy ion bombarded bacteria held in different sample holders. ► Bacteria held in metal holder had higher mutation rate than in plastic holder. ► Ion-beam-induced X-ray from biological sample is not a basic mutation source. -- Abstract: Low-energy ion beam biotechnology has achieved tremendous successes in inducing crop mutation and gene transfer. However, mechanisms involved in the related processes are not yet well understood. In ion-beam-induced mutation, ion-bombardment-produced X-ray has been proposed to be one of the secondary mutation sources, but the speculation has not yet been experimentally tested. We carried out this investigation to test whether the low-energy ion-beam-produced X-ray was a source of ion-beam-induced mutation. In the investigation, X-ray emission from 29-keV nitrogen- or argon- ion beam bombarded bacterial Escherichia coli (E. coli) cells held in a metal or plastic sample holder was in situ detected using a highly sensitive X-ray detector. The ion beam bombarded bacterial cells held in different material holders were observed for mutation induction. The results led to a conclusion that secondary X-ray emitted from ion-beam-bombarded biological living materials themselves was not a, or at least a negligible, mutational source, but the ion-beam-induced X-ray emission from the metal that made the sample holder could be a source of mutation.

  17. Is low-energy-ion bombardment generated X-ray emission a secondary mutational source to ion-beam-induced genetic mutation?

    International Nuclear Information System (INIS)

    Thongkumkoon, P.; Prakrajang, K.; Thopan, P.; Yaopromsiri, C.; Suwannakachorn, D.; Yu, L.D.

    2013-01-01

    Highlights: ► Detected X-ray emission from metal, plastic and biological samples. ► Characteristic X-ray emission was detected from metal but not from non-metals. ► Low-energy ion bombarded bacteria held in different sample holders. ► Bacteria held in metal holder had higher mutation rate than in plastic holder. ► Ion-beam-induced X-ray from biological sample is not a basic mutation source. -- Abstract: Low-energy ion beam biotechnology has achieved tremendous successes in inducing crop mutation and gene transfer. However, mechanisms involved in the related processes are not yet well understood. In ion-beam-induced mutation, ion-bombardment-produced X-ray has been proposed to be one of the secondary mutation sources, but the speculation has not yet been experimentally tested. We carried out this investigation to test whether the low-energy ion-beam-produced X-ray was a source of ion-beam-induced mutation. In the investigation, X-ray emission from 29-keV nitrogen- or argon- ion beam bombarded bacterial Escherichia coli (E. coli) cells held in a metal or plastic sample holder was in situ detected using a highly sensitive X-ray detector. The ion beam bombarded bacterial cells held in different material holders were observed for mutation induction. The results led to a conclusion that secondary X-ray emitted from ion-beam-bombarded biological living materials themselves was not a, or at least a negligible, mutational source, but the ion-beam-induced X-ray emission from the metal that made the sample holder could be a source of mutation

  18. 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.

  19. 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

  20. 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.

  1. Flash X-Ray (FXR) Accelerator Optimization Electronic Time-Resolved Measurement of X-Ray Source Size

    International Nuclear Information System (INIS)

    Jacob, J; Ong, M; Wargo, P

    2005-01-01

    Lawrence Livermore National Laboratory (LLNL) is currently investigating various approaches to minimize the x-ray source size on the Flash X-Ray (FXR) linear induction accelerator in order to improve x-ray flux and increase resolution for hydrodynamic radiography experiments. In order to effectively gauge improvements to final x-ray source size, a fast, robust, and accurate system for measuring the spot size is required. Timely feedback on x-ray source size allows new and improved accelerator tunes to be deployed and optimized within the limited run-time constraints of a production facility with a busy experimental schedule; in addition, time-resolved measurement capability allows the investigation of not only the time-averaged source size, but also the evolution of the source size, centroid position, and x-ray dose throughout the 70 ns beam pulse. Combined with time-resolved measurements of electron beam parameters such as emittance, energy, and current, key limiting factors can be identified, modeled, and optimized for the best possible spot size. Roll-bar techniques are a widely used method for x-ray source size measurement, and have been the method of choice at FXR for many years. A thick bar of tungsten or other dense metal with a sharp edge is inserted into the path of the x-ray beam so as to heavily attenuate the lower half of the beam, resulting in a half-light, half-dark image as seen downstream of the roll-bar; by measuring the width of the transition from light to dark across the edge of the roll-bar, the source size can be deduced. For many years, film has been the imaging medium of choice for roll-bar measurements thanks to its high resolution, linear response, and excellent contrast ratio. Film measurements, however, are fairly cumbersome and require considerable setup and analysis time; moreover, with the continuing trend towards all-electronic measurement systems, film is becoming increasingly difficult and expensive to procure. Here, we shall

  2. 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)

  3. Sulfur X-ray absorption fine structure in porous Li–S cathode films measured under argon atmospheric conditions

    International Nuclear Information System (INIS)

    Müller, Matthias; Choudhury, Soumyadip; Gruber, Katharina; Cruz, Valene B.; Fuchsbichler, Bernd; Jacob, Timo; Koller, Stefan; Stamm, Manfred; Ionov, Leonid; Beckhoff, Burkhard

    2014-01-01

    In this paper we present the first results for the characterization of highly porous cathode materials with pore sizes below 1 μm for Lithium Sulfur (Li–S) batteries by Near Edge X-ray Absorption Fine Structure (NEXAFS) spectroscopy. A novel cathode material of porous carbon films fabricated with colloidal array templates has been investigated. In addition, an electrochemical characterization has been performed aiming on an improved correlation of physical and chemical parameters with the electrochemical performance. The performed NEXAFS measurements of cathode materials allowed for a chemical speciation of the sulfur content inside the cathode material. The aim of the presented investigation was to evaluate the potential of the NEXAFS technique to characterize sulfur in novel battery material. The long term goal for the characterization of the battery materials is the sensitive identification of undesired side reactions, such as the polysulfide shuttle, which takes place during charging and discharging of the battery. The main drawback associated with the investigation of these materials is the fact that NEXAFS measurements can usually only be performed ex situ due to the limited in situ instrumentation being available. For Li–S batteries this problem is more pronounced because of the low photon energies needed to study the sulfur K absorption edge at 2472 eV. We employed 1 μm thick Si 3 N 4 windows to construct sealed argon cells for NEXAFS measurements under ultra high vacuum (UHV) conditions as a first step towards in situ measurements. The cells keep the sample under argon atmosphere at any time and the X-ray beam passes mainly through vacuum which enables the detection of the low energy X-ray emission of sulfur. Using these argon cells we found indications for the presence of lithium polysulfides in the cathode films whereas the correlations to the offline electrochemical results remain somewhat ambiguous. As a consequence of these findings one may

  4. The X-ray imager on AXO

    DEFF Research Database (Denmark)

    Budtz-Jørgensen, Carl; Kuvvetli, Irfan; Westergaard, Niels Jørgen Stenfeldt

    2001-01-01

    DSRI has initiated a development program of CZT X-ray and gamma-ray detectors employing strip readout techniques. A dramatic improvement of the energy response was found operating the detectors as the so-called drift detectors. For the electronic readout, modern ASIC chips were investigated....... Modular design and the low-power electronics will make large area detectors using the drift strip method feasible. The performance of a prototype CZT system will be presented and discussed. One such detector system has been proposed for future space missions: the X-Ray Imager (XRI) on the Atmospheric X-ray...... Observatory (AXO), which is a mission proposed to the Danish Small Satellite Program and is dedicated to observations of X-ray generating processes in the Earth's atmosphere. Of special interest will be simultaneous optical and X-ray observations of sprites that are flashes appearing directly above an active...

  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. Electrochemical kinetics and X-ray absorption spectroscopy investigations of select chalcogenide electrocatalysts for oxygen reduction reaction applications

    International Nuclear Information System (INIS)

    Ziegelbauer, Joseph M.; Murthi, Vivek S.; O'Laoire, Cormac; Gulla, Andrea F.; Mukerjee, Sanjeev

    2008-01-01

    Transition metal-based chalcogenide electrocatalysts exhibit a promising level of performance for oxygen reduction reaction applications while offering significant economic benefits over the state of the art Pt/C systems. The most active materials are based on Ru x Se y clusters, but the toxicity of selenium will most likely limit their embrace by the marketplace. Sulfur-based analogues do not suffer from toxicity issues, but suffer from substantially less activity and stability than their selenium brethren. The structure/property relationships that result in these properties are not understood due to ambiguities regarding the specific morphologies of Ru x S y -based chalcogenides. To clarify these properties, an electrochemical kinetics study was interpreted in light of extensive X-ray diffraction, scanning electron microscopy, and in situ X-ray absorption spectroscopy evaluations. The performance characteristics of ternary M x Ru y S z /C (M = Mo, Rh, or Re) chalcogenide electrocatalysts synthesized by the now-standard low-temperature nonaqueous (NA) route are compared to commercially available (De Nora) Rh- and Ru-based systems. Interpretation of performance differences is made in regards to bulk and surface properties of these systems. In particular, the overall trends of the measured activation energies in respect to increasing overpotential and the gross energy values can be explained in regards to these differences

  7. 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.

  8. Investigation of radiation absorption and X-ray fluorescence properties of medical imaging scintillators by Monte Carlo methods

    International Nuclear Information System (INIS)

    Nikolopoulos, D.; Kandarakis, I.; Cavouras, D.; Valais, I.; Linardatos, D.; Michail, C.; David, S.; Gaitanis, A.; Nomicos, C.; Louizi, A.

    2006-01-01

    X-ray absorption and X-ray fluorescence properties of medical imaging scintillating screens were studied by Monte Carlo methods as a function of the incident photon energy and screen-coating thickness. The scintillating materials examined were Gd 2 O 2 S (GOS) Gd 2 SiO 5 (GSO) YAlO 3 (YAP), Y 3 Al 5 O 12 (YAG), LuSiO 5 (LSO), LuAlO 3 (LuAP) and ZnS. Monoenergetic photon exposures were modeled in the range from 10 to 100 keV. The corresponding ranges of coating thicknesses of the investigated scintillating screens ranged up to 200 mg cm -2 . Results indicated that X-ray absorption and X-ray fluorescence are affected by the incident photon energy and the screen's coating thickness. Regarding incident photon energy, this X-ray absorption and fluorescence was found to exhibit very intense changes near the corresponding K edge of the heaviest element in the screen's scintillating material. Regarding coating thickness, thicker screens exhibited higher X-ray absorption and X-ray fluorescence. Results also indicated that a significant fraction of the generated X-ray fluorescent quanta escape from the scintillating screen. This fraction was found to increase with screen's coating thickness. At the energy range studied, most of the incident photons were found to be absorbed via one-hit photoelectric effect. As a result, the reabsorption of scattered radiation was found to be of rather minor importance; nevertheless this was found to increase with the screen's coating thickness. Differences in X-ray absorption and X-ray fluorescence were found among the various scintillators studied. LSO scintillator was found to be the most attractive material for use in many X-ray imaging applications, exhibiting the best absorption properties in the largest part of the energy range studied. Y-based scintillators were also found to be of significant absorption performance within the low energy ranges

  9. Simultaneous investigation of parent electrons and bremsstrahlung x rays by rocket-borne detectors

    International Nuclear Information System (INIS)

    Vij, K.K.; Venkatesan, D.; Sheldon, W.R.; Kern, J.W.; Benbrook, J.R.; Whalen, B.A.

    1975-01-01

    Simultaneous measurements of the energy spectrum of precipitating electrons and the resulting bremsstrahlung X ray spectrum were carried out during an auroral event on March 3, 1971, at the Churchill Research Range, Manitoba, Canada. The electron data were obtained with detectors on a Black Brant VB sounding rocket (275-km apogee), while the X ray flux was measured by an instrument package that was boosted to 60 km on an Arcas rocket. The X ray package was deployed on a parachute at apogee to provide a slow descent through the atmosphere. Thick target bremsstrahlung theory is used to calculate the X ray flux produced by the incident electrons, and a Monte Carlo method is used to predict the X ray spectrum at various altitudes appropriate for comparison with the measured X ray data. Satisfactory agreement between theory and experiment is obtained, and the value of the constant in the thick target theory has been estimated to be (2plus-or-minus0.5) times10 -5

  10. Simultaneous investigation of parent electrons and bremsstrahlung x rays by Rocket--Borne detectors

    International Nuclear Information System (INIS)

    Vij, K.K.; Venkatesan, D.; Sheldon, W.R.; Kern, J.W.; Benbrook, J.R.; Whalen, B.A.

    1975-01-01

    Simultaneous measurements of the energy spectrum of precipitating electrons and the resulting bremsstrahlung X ray spectrum were carried out during an auroral event on March 3, 1971, at the Churchill Research Range, Manitoba, Canada. The electron data were obtained with detectors on a Black Brant VB sounding rocket (275-km apogee), while the X ray flux was measured by an instrument package that was boosted to 60 km on an Arcas rocket. The X ray package was deployed on a parachute apogee to provide a slow descent through the atmosphere. Thick target bremsstrahlung theory is used to calculate the X ray flux produced by the incident electrons, and a Monte Carlo method is used to predict the X ray spectrum at various altitudes appropriate for comparison with the measured X ray data. Satisfactory agreement between theory and experiment is obtained, and the value of the constant in the thick target theory has been estimated to be (2plus-or-minus0.5) times10 -5 . (auth)

  11. Bone age assessment by dual-energy X-ray absorptiometry in children: an alternative for X-ray?

    Science.gov (United States)

    Heppe, D H M; Taal, H R; Ernst, G D S; Van Den Akker, E L T; Lequin, M M H; Hokken-Koelega, A C S; Geelhoed, J J M; Jaddoe, V W V

    2012-02-01

    The aim of the study was to validate dual-energy X-ray absorptiometry (DXA) as a method to assess bone age in children. Paired dual-energy X-ray absorptiometry (DXA) scans and X-rays of the left hand were performed in 95 children who attended the paediatric endocrinology outpatient clinic of University Hospital Rotterdam, the Netherlands. We compared bone age assessments by DXA scan with those performed by X-ray. Bone age assessment was performed by two blinded observers according to the reference method of Greulich and Pyle. Intra-observer and interobserver reproducibility were investigated using the intraclass correlation coefficient (ICC), and agreement was tested using Bland and Altman plots. The intra-observer ICCs for both observers were 0.997 and 0.991 for X-ray and 0.993 and 0.987 for DXA assessments. The interobserver ICC was 0.993 and 0.991 for X-ray and DXA assessments, respectively. The mean difference between bone age assessed by X-ray and DXA was 0.11 years. The limits of agreement ranged from -0.82 to 1.05 years, which means that 95% of all differences between the methods were covered by this range. Results of bone age assessment by DXA scan are similar to those obtained by X-ray. The DXA method seems to be an alternative for assessing bone age in a paediatric hospital-based population.

  12. 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

  13. Techniques for synchronization of X-Ray pulses to the pump laser in an ultrafast X-Ray facility

    International Nuclear Information System (INIS)

    Corlett, J.N.; Doolittle, L.; Schoenlein, R.; Staples, J.; Wilcox, R.; Zholents, A.

    2003-01-01

    Accurate timing of ultrafast x-ray probe pulses emitted from a synchrotron radiation source with respect to the signal initiating a process in the sample under study is critical for the investigation of structural dynamics in the femtosecond regime. We describe schemes for achieving accurate timing of femtosecond x-ray synchrotron radiation pulses relative to a pump laser, where x-rays pulses of <100 fs duration are generated from the proposed LUX source based on a recirculating superconducting linac. We present a description of the timing signal generation and distribution systems to minimize timing jitter of the x-rays relative to the experimental lasers

  14. 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....

  15. In situ X-ray and neutron diffraction of the Ruddlesden–Popper compounds (RE2−xSrx)0.98(Fe0.8Co0.2)1−yMgyO4−δ (RE=La, Pr): Structure and CO2 stability

    International Nuclear Information System (INIS)

    Chatzichristodoulou, C.; Hauback, B.C.; Hendriksen, P.V.

    2013-01-01

    The crystal structure of the Ruddlesden–Popper compounds (La 1.0 Sr 1.0 ) 0.98 Fe 0.8 Co 0.2 O 4−δ and (La 1.2 Sr 0.8 ) 0.98 (Fe 0.8 Co 0.2 ) 0.8 Mg 0.2 O 4−δ was investigated at 1000 °C in N 2 (a O2 =1×10 −4 ) by in-situ powder neutron diffraction. In-situ powder X-ray diffraction (PXD) was also employed to investigate the temperature dependence of the lattice parameters of the compounds in air and the oxygen activity dependence of the lattice parameters at 800 °C and 1000 °C. The thermal and chemical expansion coefficients, determined along the two crystallographic directions of the tetragonal unit cell, are highly anisotropic. The equivalent pseudo-cubic thermal and chemical expansion coefficients are in agreement with values determined by dilatometry. The chemical stability in CO 2 containing environments of various Ruddlesden–Popper compounds with chemical formula (RE 2−x Sr x ) 0.98 (Fe 0.8 Co 0.2 ) 1−y Mg y O 4−δ (RE=La, Pr), as well as their stability limit in H 2 /H 2 O=4.5 were also determined by in-situ PXD for x=0.9, 1.0 and y=0, 0.2. - Graphical abstract: Influence of electronic configuration on bond length, lattice parameters and anisotropic thermal and chemical expansion. Highlights: ► The thermal and chemical expansion coefficients are largely anisotropic. ► The expansion of the perovskite layers is constrained along the a direction. ► The studied compositions show remarkable thermodynamic stability upon reduction. ► The thermal and chemical expansion coefficients are lower than related perovskites. ► The investigated materials decompose in CO 2 containing atmospheres

  16. 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.

  17. A reference sample for investigating the stability of the imaging system of x-ray computed tomography

    International Nuclear Information System (INIS)

    Sun, Wenjuan; Brown, Stephen; Flay, Nadia; McCarthy, Michael; McBride, John

    2016-01-01

    The use of x-ray computed tomography for dimensional measurements associated with engineering applications has flourished in recent years. However, error sources associated with the technology are not well understood. In this paper, a novel two-sphere reference sample has been developed and used to investigate the stability of the imaging system that consists of an x-ray tube and a detector. In contrast with other research work reported, this work considered relative positional variation along the x -, y - and z -axes. This sample is a significant improvement over the one sphere sample proposed previously, which can only be used to observe the stability of the imaging system along x - and y -axes. Temperature variations of different parts of the system have been monitored and the relationship between temperature variations and x-ray image stability has been studied. Other effects that may also influence the stability of the imaging system have been discussed. The proposed reference sample and testing method are transferable to other types of x-ray computed tomography systems, for example, systems with transmission targets and systems with sub-micrometre focal spots. (paper)

  18. 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.

  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. 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 ...

  2. 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 ...

  3. 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 ...

  4. 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 ...

  5. AN X-RAY INVESTIGATION OF THREE SUPERNOVA REMNANTS IN THE LARGE MAGELLANIC CLOUD

    International Nuclear Information System (INIS)

    Klimek, Matthew D.; Points, S. D.; Smith, R. C.; Shelton, R. L.; Williams, R.

    2010-01-01

    We have investigated three supernova remnants (SNRs) in the LMC using multi-wavelength data. These SNRs are generally fainter than the known sample (see Section 4) and may represent a previously missed population. One of our SNRs is the second LMC remnant analyzed which is larger than any Galactic remnant for which a definite size has been established. The analysis of such a large remnant contributes to the understanding of the population of highly evolved SNRs. We have obtained X-ray images and spectra of three of these recently identified SNRs using the XMM-Newton observatory. These data, in conjunction with pre-existing optical emission-line images and spectra, were used to determine the physical conditions of the optical- and X-ray-emitting gas in the SNRs. We have compared the morphologies of the SNRs in the different wavebands. The physical properties of the warm ionized shell were determined from the Hα surface brightness and the SNR expansion velocity. The X-ray spectra were fit with a thermal plasma model and the physical conditions of the hot gas were derived from the model fits. Finally, we have compared our observations with simulations of SNR evolution.

  6. 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)

  7. Investigation of surface residual stress profile on martensitic stainless steel weldment with X-ray diffraction

    Directory of Open Access Journals (Sweden)

    I.I. Ahmed

    2018-04-01

    Full Text Available The development of residual stresses during fabrication is inevitable and often neglected with dire consequences during the service life of the fabricated components. In this work, the surface residual stress profile following the martensitic stainless steel (MSS pipe welding was investigated with X-ray diffraction technique. The results revealed the presence of residual stresses equilibrated across the weldment zones. Tensile residual stress observed in weld metal was balanced by compressive residual stresses in the parent material on the opposing sides of weld metal. Keywords: Residual stress, Weld, Stainless steel, X-ray, HAZ

  8. Investigations concerning the applicability of X-ray flash interference and laser technology to shock-induced solidification of organic liquids

    International Nuclear Information System (INIS)

    Krehl, Peter; Schaaffs, Werner

    By a dielectric discharge through a thin layer of liquid a hot plasma is created, which expands very fast and builds up around a compression ring of very highly compressed matter. X-ray flash interferences and laser light are applied to investigate the structure of the compression rings. To perform investigation of the fine structure, an X-ray flash machine was developed which permits to obtain with a single flash in less than 1μs Laue patterns of monocrystals, and Debye-Scherrer patterns of polycrystalline substances. The investigation of the compression rings in diverse substances by laser light resulted that the optical transparency and solidification is different in different regions of the compression ring. Therefore important hints for experiments with X-ray flash interferences were obtained

  9. 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 ...

  10. 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

  11. 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 ...

  12. 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)

  13. 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)

  14. 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

  15. Automated microfluidic sample-preparation platform for high-throughput structural investigation of proteins by small-angle X-ray scattering

    DEFF Research Database (Denmark)

    Lafleur, Josiane P.; Snakenborg, Detlef; Nielsen, Søren Skou

    2011-01-01

    A new microfluidic sample-preparation system is presented for the structural investigation of proteins using small-angle X-ray scattering (SAXS) at synchrotrons. The system includes hardware and software features for precise fluidic control, sample mixing by diffusion, automated X-ray exposure...... control, UV absorbance measurements and automated data analysis. As little as 15 l of sample is required to perform a complete analysis cycle, including sample mixing, SAXS measurement, continuous UV absorbance measurements, and cleaning of the channels and X-ray cell with buffer. The complete analysis...

  16. 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.

  17. 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

  18. An investigation of dose changes for therapeutic kilovoltage x-ray beams with underlying lead shielding

    International Nuclear Information System (INIS)

    Hill, Robin; Healy, Brendan; Holloway, Lois; Baldock, Clive

    2007-01-01

    Kilovoltage x-ray beams are used to treat cancer on or close to the skin surface. Many clinical cases use high atomic number materials as shielding to reduce dose to underlying healthy tissues. In this work, we have investigated the effect on both the surface dose and depth doses in a water phantom with lead shielding at depth in the phantom. The EGSnrc Monte Carlo code was used to simulate the water phantom and to calculate the surface doses and depth doses using primary x-ray beam spectra derived from an analytical model. The x-ray beams were in the energy range of 75-135 kVp with field sizes of 2, 5 and 8 cm diameter. The lead sheet was located beneath the water surface at depths ranging from 0.5-7.5 cm. The surface dose decreased as the lead was positioned closer to the water surface and as the field size was increased. The variation in surface dose as a function of x-ray beam energy was only small but the maximum reduction occurred for the 100 kVp x-ray beam. For the 8 cm diameter field with the lead at 1 cm depth and using the 100 kVp x-ray beam, the surface dose was reduced to 0.898 of the surface dose in the water phantom only. Measured surface dose changes, using a Farmer-type ionization chamber, agreed with the Monte Carlo calculated doses. Calculated depth doses in water with a lead sheet positioned below the surface showed that the dose fall-off increased as the lead was positioned closer to the water surface as compared to the depth dose in the water phantom only. Monte Carlo calculations of the total x-ray beam spectrum at the water surface showed that the total fluence decreased due to a reduction in backscatter from within the water and very little backscatter from the lead. The mean energy of the x-ray spectrum varied less than 1 keV, with the lead at 1 cm beneath the water phantom surface. As the Monte Carlo calculations showed good agreement with the measured results, this method can be used to verify surface dose changes in clinical situations

  19. 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

  20. 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.)

  1. 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

  2. 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.)

  3. Investigation of Co nanoparticle formation using time-dependent and spatially-resolved X-ray absorption spectroscopy

    Energy Technology Data Exchange (ETDEWEB)

    Zinoveva, S

    2008-04-15

    A crucial step towards controlled synthesis of nanoparticles is the detailed understanding of the various chemical processes that take place during the synthesis. X-ray Absorption Spectroscopy (XAS) is especially suitable for elucidating the type and structure of the intermediate metal species. It is applicable to materials that have no long range order and provides information on both electronic and geometric structures. Here a comparative study is reported of the formation of cobalt nanoparticles via thermolysis of two organometallic precursors dicobalt octacarbonyl (DCO) and alkyne-bridged dicobalt hexacarbonyl (ADH) in the presence of aluminum organics. Using time-dependent XAS a reaction pathway different from both the atom based La Mer model and the Watzky and Finsky autocatalytic surface growth model is observed. Where prior to the nucleation several intermediates are formed and the initial nucleus is composed of Co atoms coordinated with ligands Co{sub n}(CO){sub m} with n=2-3, m=3-5. The formation of Co nanoparticles was also investigated using a reaction different from thermolysis of cobalt carbonyls, namely reduction of Co (II) acetate by sodium borohydrate. Here the combination of microreactor system and spatially resolved XAS allowed ''in situ'' monitoring of the wet chemical synthesis. Several steps of the reaction were spatially resolved in the microreactor. The vertical size of the X-ray beam (50 {mu}m) focused with Kirkpatrick-Baez mirror system, determines the time resolution (better than 2 ms). The results provide direct insight into rapid process of nanoparticles formation and demonstrate the potential of this new technique for the fundamental studies of such type of processes where miniaturization and timeresolution are important. Like in the carbonyls thermolysis no evidence for the reduction of the starting complex to isolated Co{sup 0} atoms followed by nucleation of Co{sup 0} atoms was observed. (orig.)

  4. Investigation of Co nanoparticle formation using time-dependent and spatially-resolved X-ray absorption spectroscopy

    Energy Technology Data Exchange (ETDEWEB)

    Zinoveva, S.

    2008-04-15

    A crucial step towards controlled synthesis of nanoparticles is the detailed understanding of the various chemical processes that take place during the synthesis. X-ray Absorption Spectroscopy (XAS) is especially suitable for elucidating the type and structure of the intermediate metal species. It is applicable to materials that have no long range order and provides information on both electronic and geometric structures. Here a comparative study is reported of the formation of cobalt nanoparticles via thermolysis of two organometallic precursors dicobalt octacarbonyl (DCO) and alkyne-bridged dicobalt hexacarbonyl (ADH) in the presence of aluminum organics. Using time-dependent XAS a reaction pathway different from both the atom based La Mer model and the Watzky and Finsky autocatalytic surface growth model is observed. Where prior to the nucleation several intermediates are formed and the initial nucleus is composed of Co atoms coordinated with ligands Co{sub n}(CO){sub m} with n=2-3, m=3-5. The formation of Co nanoparticles was also investigated using a reaction different from thermolysis of cobalt carbonyls, namely reduction of Co (II) acetate by sodium borohydrate. Here the combination of microreactor system and spatially resolved XAS allowed ''in situ'' monitoring of the wet chemical synthesis. Several steps of the reaction were spatially resolved in the microreactor. The vertical size of the X-ray beam (50 {mu}m) focused with Kirkpatrick-Baez mirror system, determines the time resolution (better than 2 ms). The results provide direct insight into rapid process of nanoparticles formation and demonstrate the potential of this new technique for the fundamental studies of such type of processes where miniaturization and timeresolution are important. Like in the carbonyls thermolysis no evidence for the reduction of the starting complex to isolated Co{sup 0} atoms followed by nucleation of Co{sup 0} atoms was observed. (orig.)

  5. Electrochemical activation of Li2MnO3 at elevated temperature investigated by in situ Raman microscopy

    International Nuclear Information System (INIS)

    Lanz, Patrick; Villevieille, Claire; Novák, Petr

    2013-01-01

    Layered-layered oxides of the type xLi 2 MnO 3 ·(1 − x)LiMO 2 (M = Mn, Ni, Co) have been postulated to contain Li 2 MnO 3 domains which, upon electrochemical activation, give rise to a characteristic potential plateau at 4.5 V vs. Li + /Li. To improve our understanding of the complex reaction mechanisms at play, we applied in situ Raman microscopy to investigate the constituent Li 2 MnO 3 . Li 2 MnO 3 synthesised via a two-step solid-state reaction was characterised by scanning electron microscopy and X-ray diffraction. Preliminary electrochemical tests and ex situ Raman microscopy showed the need for elevated temperatures to achieve activation. For the first time, in situ Raman microscopy (at 50 °C) confirmed the activation of Li 2 MnO 3 . The main signal at 615 cm −1 shifted to higher wavenumbers upon charging. After reaching 4.4 V vs. Li + /Li, this shift grew significantly, which is in good agreement with the onset of the potential plateau in both Li 2 MnO 3 and xLi 2 MnO 3 ·(1 − x)LiMO 2 , and is assigned to the partial formation of a spinel-like phase

  6. 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.

  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. Time-resolved X-ray PIV technique for diagnosing opaque biofluid flow with insufficient X-ray fluxes.

    Science.gov (United States)

    Jung, Sung Yong; Park, Han Wook; Kim, Bo Heum; Lee, Sang Joon

    2013-05-01

    X-ray imaging is used to visualize the biofluid flow phenomena in a nondestructive manner. A technique currently used for quantitative visualization is X-ray particle image velocimetry (PIV). Although this technique provides a high spatial resolution (less than 10 µm), significant hemodynamic parameters are difficult to obtain under actual physiological conditions because of the limited temporal resolution of the technique, which in turn is due to the relatively long exposure time (~10 ms) involved in X-ray imaging. This study combines an image intensifier with a high-speed camera to reduce exposure time, thereby improving temporal resolution. The image intensifier amplifies light flux by emitting secondary electrons in the micro-channel plate. The increased incident light flux greatly reduces the exposure time (below 200 µs). The proposed X-ray PIV system was applied to high-speed blood flows in a tube, and the velocity field information was successfully obtained. The time-resolved X-ray PIV system can be employed to investigate blood flows at beamlines with insufficient X-ray fluxes under specific physiological conditions. This method facilitates understanding of the basic hemodynamic characteristics and pathological mechanism of cardiovascular diseases.

  9. In Situ Local Contact Angle Measurement in a CO2-Brine-Sand System Using Microfocused X-ray CT.

    Science.gov (United States)

    Lv, Pengfei; Liu, Yu; Wang, Zhe; Liu, Shuyang; Jiang, Lanlan; Chen, Junlin; Song, Yongchen

    2017-04-11

    The wettability of porous media is of major interest in a broad range of natural and engineering applications. The wettability of a fluid on a solid surface is usually evaluated by the contact angle between them. While in situ local contact angle measurements are complicated by the topology of porous media, which can make it difficult to use traditional methods, recent advances in microfocused X-ray computed tomography (micro-CT) and image processing techniques have made it possible to measure contact angles on the scale of the pore sizes in such media. However, the effects of ionic strength, CO 2 phase, and flow pattern (drainage or imbibition) on pore-scale contact angle distribution are still not clear and have not been reported in detail in previous studies. In this study, we employed a micro-CT scanner for in situ investigation of local contact angles in a CO 2 -brine-sand system under various conditions. The effects of ionic strength, CO 2 phase, and flow pattern on the local contact-angle distribution were examined in detail. The results showed that the local contact angles vary over a wide range as a result of the interaction of surface contaminants, roughness, pore topology, and capillarity. The wettability of a porous surface could thus slowly weaken with increasing ionic strength, and the average contact angle could significantly increase when gaseous CO 2 (gCO 2 ) turns into supercritical CO 2 (scCO 2 ). Contact angle hysteresis also occurred between drainage and imbibition procedures, and the hysteresis was more significant under gCO 2 condition.

  10. An investigation of infection control for x-ray cassettes in a diagnostic imaging department

    Energy Technology Data Exchange (ETDEWEB)

    Fox, Matthew [School of Allied Health Professions and Science, Faculty of Health, Wellbeing and Science, University Campus Suffolk, Rope Walk, Ipswich, Suffolk, IP4 1LT (United Kingdom); Harvey, Jane M. [School of Allied Health Professions and Science, Faculty of Health, Wellbeing and Science, University Campus Suffolk, Rope Walk, Ipswich, Suffolk, IP4 1LT (United Kingdom)], E-mail: j.harvey@ucs.ac.uk

    2008-11-15

    Introduction: This research was conducted to investigate if X-ray cassettes could be a possible source of pathogens capable of causing nosocomial infections, and if they could be a possible vector for cross infection within the hospital environment. Method: The research involved the swabbing of X-ray cassettes in a Diagnostic Imaging Department of a large hospital in the east of England. Two areas of the Diagnostic Imaging Department were included in the study. Research concentrated on X-ray cassettes used for mobile radiography, accident and emergency and inpatient use. Forty cassettes were swabbed in total specifically for general levels of bacterial contamination, also for the presence or absence of methicillin-resistant Staphylococcus aureus (MRSA). A mapping exercise was completed following the location of an X-ray cassette typically used in mobile radiography. The exercise noted the level of direct contact with patient's skin and other possible routes of infection. Results: The results demonstrated that there were large levels of growth of samples taken from cassettes and developed in the Microbiology Department. Coagulase-negative Staphylococcus, Micrococci, Diptheroids and species of Bacillus were all identified. The mapping exercise in which the journey of a 35/43 cm cassette used for mobile radiography was tracked found that contact with patient's skin and potential pathogens or routes of cross infection was a common occurrence whilst undertaking mobile radiography. Conclusion: The research has identified the presence of bacterial contamination on cassettes. The research established that X-ray cassettes/imaging plates are often exposed to pathogens and possible routes of cross infection; also that patient's skin often comes directly in contact with the X-ray cassette/imaging plate. The research also shows that as cassettes/imaging plates are a potential source of cross infection, the Diagnostic Imaging Department may be partly responsible

  11. In-situ investigation of the icosahedral Al-Cu-Fe phase formation in thin films

    Energy Technology Data Exchange (ETDEWEB)

    Haidara, F., E-mail: fanta.haidara@im2np.fr [IM2NP, UMR 6242 CNRS - Universite Aix-Marseille, Av. Escadrille Normandie-Niemen, Case 142, 13397 Marseille Cedex 20 (France); Duployer, B. [Universite Paul Sabatier CIRIMAT-LCMIE 2R1, 118, Route de Narbonne, 31062 Toulouse Cedex 09 (France); Mangelinck, D.; Record, M.-C. [IM2NP, UMR 6242 CNRS - Universite Aix-Marseille, Av. Escadrille Normandie-Niemen, Case 142, 13397 Marseille Cedex 20 (France)

    2012-09-05

    Highlights: Black-Right-Pointing-Pointer We investigated the phase formation of i-Al{sub 62.5}Cu{sub 25}Fe{sub 12.5} in thin films. Black-Right-Pointing-Pointer We characterized the samples by DSC and in-situ XRD and resistance measurements. Black-Right-Pointing-Pointer The resistivity value for i-Al{sub 62.5}Cu{sub 25}Fe{sub 12.5} was determined. - Abstract: This work is an investigation of the formation by reactive diffusion at high temperatures of the icosahedral phase, i-Al{sub 62.5}Cu{sub 25}Fe{sub 12.5}, in thin films. The samples were prepared by sputtering at room temperature. The elements Al, Cu and Fe were sequentially deposited onto oxidized silicon substrates. The two following stacking sequences, Al/Cu/Fe and Al/Fe/Cu, were investigated. The phase formation was studied using in situ resistivity, in situ X-ray Diffraction and Differential Scanning Calorimetry measurements. Whatever the stacking sequence, the sequences of phase formation evidenced during the heating treatment are similar. However the temperatures of formation for the first phases that are formed are different; they are higher in the case of the Al/Fe/Cu stacking sequence.

  12. 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 ...

  13. 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)

  14. [Experimental investigation of laser plasma soft X-ray source with gas target].

    Science.gov (United States)

    Ni, Qi-liang; Gong, Yan; Lin, Jing-quan; Chen, Bo; Cao, Jian-lin

    2003-02-01

    This paper describes a debris-free laser plasma soft X-ray source with a gas target, which has high operating frequency and can produce strong soft X-ray radiation. The valve of this light source is drived by a piezoelectrical ceramic whose operating frequency is up to 400 Hz. In comparison with laser plasma soft X-ray sources using metal target, the light source is debris-free. And it has higher operating frequency than gas target soft X-ray sources whose nozzle is controlled by a solenoid valve. A channel electron multiplier (CEM) operating in analog mode is used to detect the soft X-ray generated by the laser plasma source, and the CEM's output is fed to to a charge-sensitive preamplifier for further amplification purpose. Output charges from the CEM are proportional to the amplitude of the preamplifier's output voltage. Spectra of CO2, Xe and Kr at 8-14 nm wavelength which can be used for soft X-ray projection lithography are measured. The spectrum for CO2 consists of separate spectral lines originate mainly from the transitions in Li-like and Be-like ions. The Xe spectrum originating mainly from 4d-5f, 4d-4f, 4d-6p and 4d-5p transitions in multiply charged xenon ions. The spectrum for Kr consists of separate spectral lines and continuous broad spectra originating mainly from the transitions in Cu-, Ni-, Co- and Fe-like ions.

  15. 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)

  16. 3-D Cellular Ultrastructure Can Be Resolved by X-ray Microscopy | Center for Cancer Research

    Science.gov (United States)

    X-ray microscopy (XRM) is more rapid than cryoelectron tomography or super-resolution fluorescence microscopy and could fill an important gap in current technologies used to investigate in situ three-dimensional structure of cells. New XRM methods developed by first author Gerd Schneider, Ph.D., working with James McNally. Ph.D., and a team of colleagues, is capable of revealing full cellular ultrastructure without requiring fixation, staining, or sectioning.

  17. Investigation of liquid water in gas diffusion layers of polymer electrolyte fuel cells using X-ray tomographic microscopy

    Energy Technology Data Exchange (ETDEWEB)

    Flueckiger, Reto [Electrochemistry Laboratory, Paul Scherrer Institut, CH-5232 Villigen PSI (Switzerland); Marone, Federica [Swiss Light Source, Paul Scherrer Institut, CH-5232 Villigen PSI (Switzerland); Stampanoni, Marco [Swiss Light Source, Paul Scherrer Institut, CH-5232 Villigen PSI (Switzerland); Institute for Biomedical Engineering, University and ETH Zurich, Gloriastrasse 35, CH-8092 Zurich (Switzerland); Wokaun, Alexander [Electrochemistry Laboratory, Paul Scherrer Institut, CH-5232 Villigen PSI (Switzerland); Buechi, Felix N., E-mail: felix.buechi@psi.c [Electrochemistry Laboratory, Paul Scherrer Institut, CH-5232 Villigen PSI (Switzerland)

    2011-02-01

    In polymer electrolyte fuel cells (PEFCs), condensation of water within the pore network of the gas diffusion layers (GDL) can influence the gas transport properties and thus reduce the electrochemical conversion rates. The use of X-ray tomographic microscopy (XTM), which allows for a resolution in the order of one micrometer is investigated for studying ex situ the local saturation in GDL's. The strength of XTM is the high spatial resolution with simultaneous contrast for water and carbon, allowing for non-destructive 3D-imaging of the solid and the contained water. The application of this method for imaging the ex situ water intrusion into the porous network of GDLs is explored using absorption and phase contrast methods. It is shown that the inhomogeneous filling behavior of GDL materials can indeed be visualized with sufficient resolution. For Toray paper TGP-H-060 the local saturation was measured as function of the water pressure. The results, evaluated in 1D, 2D and 3D show a liquid water retention effect at the denser layers near the surface. A comparison with established capillary pressure functions is presented. Altogether, the results show the potential of the XTM-method as a tool for studying the liquid water behavior in PEFC on a microscopic scale.

  18. Investigation of liquid water in gas diffusion layers of polymer electrolyte fuel cells using X-ray tomographic microscopy

    International Nuclear Information System (INIS)

    Flueckiger, Reto; Marone, Federica; Stampanoni, Marco; Wokaun, Alexander; Buechi, Felix N.

    2011-01-01

    In polymer electrolyte fuel cells (PEFCs), condensation of water within the pore network of the gas diffusion layers (GDL) can influence the gas transport properties and thus reduce the electrochemical conversion rates. The use of X-ray tomographic microscopy (XTM), which allows for a resolution in the order of one micrometer is investigated for studying ex situ the local saturation in GDL's. The strength of XTM is the high spatial resolution with simultaneous contrast for water and carbon, allowing for non-destructive 3D-imaging of the solid and the contained water. The application of this method for imaging the ex situ water intrusion into the porous network of GDLs is explored using absorption and phase contrast methods. It is shown that the inhomogeneous filling behavior of GDL materials can indeed be visualized with sufficient resolution. For Toray paper TGP-H-060 the local saturation was measured as function of the water pressure. The results, evaluated in 1D, 2D and 3D show a liquid water retention effect at the denser layers near the surface. A comparison with established capillary pressure functions is presented. Altogether, the results show the potential of the XTM-method as a tool for studying the liquid water behavior in PEFC on a microscopic scale.

  19. Phase transformation in δ-Pu alloys at low temperature: An in situ microstructural characterization using X-ray diffraction

    International Nuclear Information System (INIS)

    Ravat, B.; Platteau, C.; Texier, G.; Oudot, B.; Delaunay, F.

    2009-01-01

    In order to investigate the martensitic transformation, an isothermal hold at -130 deg. C for 48 h was performed on a highly homogenized PuGa alloy. The modifications of the microstructure were characterized in situ thanks to a specific tool. This device was developed at the CEA-Valduc to analyze the crystalline structure of plutonium alloys as a function of temperature and more especially at low temperature using X-ray diffraction. The analysis of the recorded diffraction patterns highlighted that the martensitic transformation for this alloy is the result of a direct δ → α' + δ phase transformation. Moreover, a significant Bragg's peaks broadening corresponding to the δ-phase was observed. A microstructural analysis was made to characterize anisotropic microstrain resulting from the stress induced by the unit cell volume difference between the δ and α' phases. The amount of α'-phase evolved was analyzed within the framework of the Avrami theory in order to characterize the nucleation process. The results suggested that the growth mechanism corresponded to a general mechanism where the nucleation sites were in the δ-grain edges and the α'-phase had a plate-like morphology.

  20. Phase transformation in δ-Pu alloys at low temperature: An in situ microstructural characterization using X-ray diffraction

    Science.gov (United States)

    Ravat, B.; Platteau, C.; Texier, G.; Oudot, B.; Delaunay, F.

    2009-09-01

    In order to investigate the martensitic transformation, an isothermal hold at -130 °C for 48 h was performed on a highly homogenized PuGa alloy. The modifications of the microstructure were characterized in situ thanks to a specific tool. This device was developed at the CEA-Valduc to analyze the crystalline structure of plutonium alloys as a function of temperature and more especially at low temperature using X-ray diffraction. The analysis of the recorded diffraction patterns highlighted that the martensitic transformation for this alloy is the result of a direct δ → α' + δ phase transformation. Moreover, a significant Bragg's peaks broadening corresponding to the δ-phase was observed. A microstructural analysis was made to characterize anisotropic microstrain resulting from the stress induced by the unit cell volume difference between the δ and α' phases. The amount of α'-phase evolved was analyzed within the framework of the Avrami theory in order to characterize the nucleation process. The results suggested that the growth mechanism corresponded to a general mechanism where the nucleation sites were in the δ-grain edges and the α'-phase had a plate-like morphology.

  1. Phase transformation in delta-Pu alloys at low temperature: An in situ microstructural characterization using X-ray diffraction

    Energy Technology Data Exchange (ETDEWEB)

    Ravat, B., E-mail: brice.ravat@cea.f [CEA, Valduc, F-21120 Is-sur-Tille (France); Platteau, C.; Texier, G.; Oudot, B.; Delaunay, F. [CEA, Valduc, F-21120 Is-sur-Tille (France)

    2009-09-15

    In order to investigate the martensitic transformation, an isothermal hold at -130 deg. C for 48 h was performed on a highly homogenized PuGa alloy. The modifications of the microstructure were characterized in situ thanks to a specific tool. This device was developed at the CEA-Valduc to analyze the crystalline structure of plutonium alloys as a function of temperature and more especially at low temperature using X-ray diffraction. The analysis of the recorded diffraction patterns highlighted that the martensitic transformation for this alloy is the result of a direct delta -> alpha' + delta phase transformation. Moreover, a significant Bragg's peaks broadening corresponding to the delta-phase was observed. A microstructural analysis was made to characterize anisotropic microstrain resulting from the stress induced by the unit cell volume difference between the delta and alpha' phases. The amount of alpha'-phase evolved was analyzed within the framework of the Avrami theory in order to characterize the nucleation process. The results suggested that the growth mechanism corresponded to a general mechanism where the nucleation sites were in the delta-grain edges and the alpha'-phase had a plate-like morphology.

  2. 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 ...

  3. 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)

  4. 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

  5. X-ray structural investigation into complexes of p-aminobenzoic acid and metals

    International Nuclear Information System (INIS)

    Amiraslanov, I.R.; Musaev, F.N.; Mamedov, Kh.S.

    1982-01-01

    X-ray structural investigation of p-aminobenzoatodiaqua-strontium Sr(H 2 NC 6 H 4 COO) 2 x2H 2 o' was carried out. Crystals were rhombic: a=6.86(1), b=13.39(2), c=18.58(2) A, V=1705 A, Z=4, space group P2 1 2 1 2 1 . The basis of the structure was formed by infinite along the axis a chains of strontium atom octavertices articulated with common oxygen vertices. Sr-O bond lengths were 2.46-2.74 A; the distance between strontium neighbour - ring atom 4.07(1) A. Bond angles were presented

  6. Time-resolved X-ray diffraction with accelerator- and laser-plasma-based X-ray sources

    International Nuclear Information System (INIS)

    Nicoul, Matthieu

    2010-01-01

    Femtosecond X-ray pulses are a powerful tool to investigate atomic motions triggered by femtosecond pump pulses. This thesis is dedicated to the production of such pulses and their use in optical pump - X-ray probe measurement. This thesis describes the laser-plasma-based sources available at the University of Duisburg-Essen. Part of it consists of the description of the design, built-up and characterization of a new ''modular'' X-ray source dedicated to optimize the X-ray flux onto the sample under investigation. The acoustic wave generation in femtosecond optically excited semiconductor (gallium arsenide) and metal (gold) was performed using the sources of the University of Duisburg-Essen. The physical answer of the material was modeled by a simple strain model for the semiconductor, pressure model for the metal, in order to gain information on the interplay of the electronic and thermal pressures rising after excitation. Whereas no reliable information could be obtain in gallium arsenide (principally due to the use of a bulk), the model for gold achieved very good agreement, providing useful information. The relaxation time of the electron to lattice energy was found to be (5.0±0.3) ps, and the ratio of the Grueneisen parameters was found to be γ e / γ i = (0.5±0.1). This thesis also describes the Sub-Picosecond Pulse Source (SPPS) which existed at the (formally) Stanford Linear Accelerator Center, an accelerator-based X-ray source, and two measurements performed with it. The first one is the detailed investigation of the phonon softening of the A 1g mode launch in bismuth upon fluence excitation. Detailed information concerning the new equilibrium position and phonon frequency were obtained over extended laser pump fluences. The second measurement concerned the study of the liquid phase dynamics in a newly formed liquid phase following ultrafast melting in indium antimonide. The formation of the liquid phase and its development for excitations close to the

  7. Time-resolved X-ray diffraction with accelerator- and laser-plasma-based X-ray sources

    Energy Technology Data Exchange (ETDEWEB)

    Nicoul, Matthieu

    2010-09-01

    Femtosecond X-ray pulses are a powerful tool to investigate atomic motions triggered by femtosecond pump pulses. This thesis is dedicated to the production of such pulses and their use in optical pump - X-ray probe measurement. This thesis describes the laser-plasma-based sources available at the University of Duisburg-Essen. Part of it consists of the description of the design, built-up and characterization of a new ''modular'' X-ray source dedicated to optimize the X-ray flux onto the sample under investigation. The acoustic wave generation in femtosecond optically excited semiconductor (gallium arsenide) and metal (gold) was performed using the sources of the University of Duisburg-Essen. The physical answer of the material was modeled by a simple strain model for the semiconductor, pressure model for the metal, in order to gain information on the interplay of the electronic and thermal pressures rising after excitation. Whereas no reliable information could be obtain in gallium arsenide (principally due to the use of a bulk), the model for gold achieved very good agreement, providing useful information. The relaxation time of the electron to lattice energy was found to be (5.0{+-}0.3) ps, and the ratio of the Grueneisen parameters was found to be {gamma}{sub e} / {gamma}{sub i} = (0.5{+-}0.1). This thesis also describes the Sub-Picosecond Pulse Source (SPPS) which existed at the (formally) Stanford Linear Accelerator Center, an accelerator-based X-ray source, and two measurements performed with it. The first one is the detailed investigation of the phonon softening of the A{sub 1g} mode launch in bismuth upon fluence excitation. Detailed information concerning the new equilibrium position and phonon frequency were obtained over extended laser pump fluences. The second measurement concerned the study of the liquid phase dynamics in a newly formed liquid phase following ultrafast melting in indium antimonide. The formation of the liquid phase

  8. Structural Investigations of Nanowires Using X-Ray Diffraction

    DEFF Research Database (Denmark)

    Stankevic, Tomas

    Advancements in growth of the nanowire-based devices opened another dimension of possible structures and material combinations, which nd their applications in a wide variety of elds, including everyday life. Characterization of such devices brings its own challenges and here we show that X-rays oer...

  9. 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.

  10. 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

  11. 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 ...

  12. Improving x-ray fluorescence signal for benchtop polychromatic cone-beam x-ray fluorescence computed tomography by incident x-ray spectrum optimization: a Monte Carlo study.

    Science.gov (United States)

    Manohar, Nivedh; Jones, Bernard L; Cho, Sang Hyun

    2014-10-01

    To develop an accurate and comprehensive Monte Carlo (MC) model of an experimental benchtop polychromatic cone-beam x-ray fluorescence computed tomography (XFCT) setup and apply this MC model to optimize incident x-ray spectrum for improving production/detection of x-ray fluorescence photons from gold nanoparticles (GNPs). A detailed MC model, based on an experimental XFCT system, was created using the Monte Carlo N-Particle (MCNP) transport code. The model was validated by comparing MC results including x-ray fluorescence (XRF) and scatter photon spectra with measured data obtained under identical conditions using 105 kVp cone-beam x-rays filtered by either 1 mm of lead (Pb) or 0.9 mm of tin (Sn). After validation, the model was used to investigate the effects of additional filtration of the incident beam with Pb and Sn. Supplementary incident x-ray spectra, representing heavier filtration (Pb: 2 and 3 mm; Sn: 1, 2, and 3 mm) were computationally generated and used with the model to obtain XRF/scatter spectra. Quasimonochromatic incident x-ray spectra (81, 85, 90, 95, and 100 keV with 10 keV full width at half maximum) were also investigated to determine the ideal energy for distinguishing gold XRF signal from the scatter background. Fluorescence signal-to-dose ratio (FSDR) and fluorescence-normalized scan time (FNST) were used as metrics to assess results. Calculated XRF/scatter spectra for 1-mm Pb and 0.9-mm Sn filters matched (r ≥ 0.996) experimental measurements. Calculated spectra representing additional filtration for both filter materials showed that the spectral hardening improved the FSDR at the expense of requiring a much longer FNST. In general, using Sn instead of Pb, at a given filter thickness, allowed an increase of up to 20% in FSDR, more prominent gold XRF peaks, and up to an order of magnitude decrease in FNST. Simulations using quasimonochromatic spectra suggested that increasing source x-ray energy, in the investigated range of 81-100 ke

  13. 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...

  14. 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

  15. 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.

  16. 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 ...

  17. Laboratory micro- and nanoscale X-ray tomographic investigation of Al–7 at.%Cu solidification structures

    International Nuclear Information System (INIS)

    Patterson, B.M.; Henderson, K.C.; Gibbs, P.J.; Imhoff, S.D.; Clarke, A.J.

    2014-01-01

    X-ray computed tomography across multiple length scales provides an opportunity to non-destructively visualize and quantify the micro- to nano-scale microstructural features of solidification structures in three dimensions. Aluminum–7 at.%copper samples were directionally solidified at three cooling rates (0.44, 0.67, and 1.33 °C/s), resulting in systematic changes in the as-solidified microstructure, which are difficult to quantify using traditional microscopic techniques. The cooling rate of a material affects its ultimate microstructure, and characterizing that microstructure is key to predicting and understanding its bulk properties. Here, two different laboratory X-ray computed tomography instruments were used to characterize as-solidified microstructures, including micro-scale computed tomography with approximately 1 mm field-of-view, ∼ 1.7 μm resolution, and nano-scale X-ray computed tomography ∼ 65 μm FOV, 150 nm resolution. Micro-scale X-ray radiography and computed tomography enabled a quantitative investigation of changes in the primary dendritic solidification structure with increasing cooling rate. Nano-scale absorption contrast X-ray computed tomography resolved the distinct phases of the lamellar eutectic structure and three dimensional measurements of the ∼ 1 μm interlamellar spacing. It is found that the lamella eutectic structure thickness is inversely proportional to the cooling rate. Nano-scale Zernike phase contrast was also used to image voids at eutectic colony boundaries. The application and resolution of these two instruments are discussed with respect to the resolvable features of the solidification structures. - Highlights: • Al–Cu eutectic is a model system for studying solidification microstructure. • X-ray computed tomography provides a 3D picture of these complex structures. • Micro-scale tomography images the primary and secondary dendritic structures. • Nano-scale tomography images the eutectic lamella and

  18. Laboratory micro- and nanoscale X-ray tomographic investigation of Al–7 at.%Cu solidification structures

    Energy Technology Data Exchange (ETDEWEB)

    Patterson, B.M., E-mail: bpatterson@lanl.gov; Henderson, K.C.; Gibbs, P.J.; Imhoff, S.D.; Clarke, A.J.

    2014-09-15

    X-ray computed tomography across multiple length scales provides an opportunity to non-destructively visualize and quantify the micro- to nano-scale microstructural features of solidification structures in three dimensions. Aluminum–7 at.%copper samples were directionally solidified at three cooling rates (0.44, 0.67, and 1.33 °C/s), resulting in systematic changes in the as-solidified microstructure, which are difficult to quantify using traditional microscopic techniques. The cooling rate of a material affects its ultimate microstructure, and characterizing that microstructure is key to predicting and understanding its bulk properties. Here, two different laboratory X-ray computed tomography instruments were used to characterize as-solidified microstructures, including micro-scale computed tomography with approximately 1 mm field-of-view, ∼ 1.7 μm resolution, and nano-scale X-ray computed tomography ∼ 65 μm FOV, 150 nm resolution. Micro-scale X-ray radiography and computed tomography enabled a quantitative investigation of changes in the primary dendritic solidification structure with increasing cooling rate. Nano-scale absorption contrast X-ray computed tomography resolved the distinct phases of the lamellar eutectic structure and three dimensional measurements of the ∼ 1 μm interlamellar spacing. It is found that the lamella eutectic structure thickness is inversely proportional to the cooling rate. Nano-scale Zernike phase contrast was also used to image voids at eutectic colony boundaries. The application and resolution of these two instruments are discussed with respect to the resolvable features of the solidification structures. - Highlights: • Al–Cu eutectic is a model system for studying solidification microstructure. • X-ray computed tomography provides a 3D picture of these complex structures. • Micro-scale tomography images the primary and secondary dendritic structures. • Nano-scale tomography images the eutectic lamella and

  19. Ultra high-speed x-ray imaging of laser-driven shock compression using synchrotron light

    Science.gov (United States)

    Olbinado, Margie P.; Cantelli, Valentina; Mathon, Olivier; Pascarelli, Sakura; Grenzer, Joerg; Pelka, Alexander; Roedel, Melanie; Prencipe, Irene; Laso Garcia, Alejandro; Helbig, Uwe; Kraus, Dominik; Schramm, Ulrich; Cowan, Tom; Scheel, Mario; Pradel, Pierre; De Resseguier, Thibaut; Rack, Alexander

    2018-02-01

    A high-power, nanosecond pulsed laser impacting the surface of a material can generate an ablation plasma that drives a shock wave into it; while in situ x-ray imaging can provide a time-resolved probe of the shock-induced material behaviour on macroscopic length scales. Here, we report on an investigation into laser-driven shock compression of a polyurethane foam and a graphite rod by means of single-pulse synchrotron x-ray phase-contrast imaging with MHz frame rate. A 6 J, 10 ns pulsed laser was used to generate shock compression. Physical processes governing the laser-induced dynamic response such as elastic compression, compaction, pore collapse, fracture, and fragmentation have been imaged; and the advantage of exploiting the partial spatial coherence of a synchrotron source for studying low-density, carbon-based materials is emphasized. The successful combination of a high-energy laser and ultra high-speed x-ray imaging using synchrotron light demonstrates the potentiality of accessing complementary information from scientific studies of laser-driven shock compression.

  20. Investigations of some regional river systems by INAA and X-ray fluorescence

    International Nuclear Information System (INIS)

    Drazhkovich, R.J.; Kukoch, A.

    1985-01-01

    Distribution of Zn, Hg, Sb, Cr, Fe, Sc and Co has been investigated in materials dissolved and suspended in the rivers Ibar, Zapadna Morava and Kamenica by means of INAA and X-ray fluorescence. Irradiation was made in VKG-channels of RA-nuclear reactor Vincha. Distribution coefficients were calculated, as well as contamination factors for investigated river regional systems in comparison to the uncontaminated water system. Data obtained indicate the possibility of utilization of these two analytical methods for investigation and control of biogeochemical and contamination processes in small regional water systems, especially important for modern studies in life sciences

  1. 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.

  2. 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.

  3. 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

  4. 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 ...

  5. In situ investigation of SnAgCu solder alloy microstructure

    International Nuclear Information System (INIS)

    Pietrikova, Alena; Bednarcik, Jozef; Durisin, Juraj

    2011-01-01

    Research highlights: → In situ X-ray diffraction investigation enabled detailed analysis of the melting and solidification process of the SAC305 alloy. → It was found that the SAC305 solder melts at 230 deg. C. When cooling from 240 deg. C the SAC305 alloy solidifies at the temperature of 214 deg. C. During solidification β-Sn and Cu 6 Sn 5 is also formed. Formation of Ag 3 Sn occurs at 206 deg. C and the remaining amount of alloy crystallizes approximately at 160 deg. C. → Furthermore, observation of the thermal expansion behaviour of the β-Sn tetragonal unit cell revealed linear dependence of the unit cell volume on temperature. The unit cell parameters a and c also increase linearly with the temperature. Despite the fact that the c parameter is substantially smaller than parameter a, it exhibits a significantly higher linear thermal expansion coefficient. Comparison between data obtained during heating and cooling indicates that the thermal expansion coefficient is slightly greater in the case of cooling. - Abstract: In situ X-ray diffraction experiments, using synchrotron radiation, were employed to analyze microstructure evolution of the 96.5Sn3Ag0.5Cu (wt.%)-SAC305 lead-free solder alloy during heating (30-240 deg. C), isothermal dwell (240 deg. C) and cooling (240-30 deg. C). The special emphasis was placed on the study of the melting and solidification processes, explaining formation, distribution and the order of crystallization of the crystal phases (β-Sn, intermetallic compounds) in the solder alloy. Furthermore, thermal expansion behaviour of the main constituent phase β-Sn was analyzed prior to melting and after the consequent solidification.

  6. X-ray and Moessbauer investigations of isotropic barium ferrites

    International Nuclear Information System (INIS)

    Kirichok, P.P.; Pashchenko, V.A.; Dem'yaniv, T.O.; Ryabova, G.N.; Lisovskij, A.M.

    1984-01-01

    Using the methods of X-ray and γ-resonance spectroscopy the crystal chemical and magnetic structure of isotropic barium hexaferrites is studied. compacting pressure the lattice parameter c of ferrite of the BaOx5.7Fe 2 O 3 is decreased and the diffraction line width on its X-ray p attern is increased. Due to increasing the isoststical compacting pressure quadrupole splitting of the γ-resonance absorption spectrum of 57 Fe nuclei in tetrahedral positions 4f 1 and in positions 2a decreases. The sintering temperature growth leads to increasing the lattice parameter c and diffraction line widths and decreasing the effeutive field values and isomeric s hifts on 57 Fe nuclei. Isostatical compacting pressure does not affect the electron configuration of iron ions

  7. 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.)

  8. 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)

  9. Exposure of nitrous oxide to X-rays

    International Nuclear Information System (INIS)

    Yanagida, H.

    1980-01-01

    A study was performed to determine how much NO and NO 2 is produced when nitrous oxide is exposed to X-radiation. Polyethylene bottles filled with either nitrous oxide alone or with nitrous oxide and 30% oxygen were placed 30 cm from the X-ray tube at a standard X-ray beam setting for chest fluoroscopy for 0 to 5 minutes. In the bottles filled with nitrous oxide alone, the production of NO was not affected by the duration of X-ray exposure, but the longer duration of X-ray exposure produced a larger amount of NO 2 . In the bottles filled with nitrous oxide and 30% oxygen, the longer duration of X-ray exposure produced larger amounts of both NO and NO 2 . These findings confirmed a previous investigation in which nitrous oxide was not inert under X-ray exposure. As the presence of oxygen plays an important role in the oxidation of nitrous oxide under X-ray exposure, this study suggests another potentially hazardous interaction that may occur secondary to the administration of an anaesthetic in the presence of X-irradiation as in pulmonary angiography, cardiac catheterisation, and fluoroscopic bronchoscopy or biopsy. (author)

  10. 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.

  11. X-ray instrumentation in astronomy

    International Nuclear Information System (INIS)

    Cuhlane, J.L.

    1985-01-01

    This book presents the proceedings of a conference devoted to x-ray instrumentation in astronomy. Special sections are: AXAF X-Ray Optical Systems; Specialized X-Ray Systems; X-Ray Optical Systems I; X-Ray Optical Systems II; Gas Filled X-Ray Detectors II; The NASA Advanced X-Ray Astrophysics Facility; X-Ray and EUV Spectrometers; Microchannel Plates; and Solid State Detectors

  12. X-ray dosimetry of TlGaSe2 single crystals

    International Nuclear Information System (INIS)

    Kerimova, E.M.; Mustafaeva, S.N.; Mamedbeili, S.D.; Jabarov, J.N.; Iskenderova, P.M.; Kazimov, S.B.

    2002-01-01

    TlGaSe 2 compound belongs to group of layered semiconductors of A 3 B 3 C 2 6 -type. Photoelectric and optical properties of TlGaSe 2 single crystals were investigated in detail. Influence of gamma-, electron and neutron radiation on photoelectric properties of TlGaSe 2 single crystals is investigated too. The present work deals with experimental results relative to X-ray dosimetric characteristics of TlGaSe 2 crystals at 300 K. X-ray conductivity and X-ray dosimetric characteristic measurements are carried out in low load resistance regime. The source of X-ray radiation is the installation of X-ray diffraction analysis (URS-55a) with the BCV-2(Cu). Intensity of X-ray radiation (E) is regulated by measurement with current variation in tube at each given value of X-ray radiation dose E (R/min) are measured by crystal dosimeter DRGZ-02. X-ray conductivity coefficients K σ characterising X-ray sensitivity of investigated crystals are determined as the relative change of conductivity under X-ray radiation a per dose. There have been determined values of characteristic coefficients of TlGaSe 2 single crystal X-ray conductivity at different values of accelerating voltage (V a ) on the tube and corresponding doses of X-ray radiation. Analysis of obtained data showed that X-ray conductivity coefficients K σ in studied crystals are regularly decreased (from 0.276 to 0.033) as with the rise of dose (E=0.75-78.0 R/min) as with the increase of values of V a on X-ray tube (V a =254-50 keV). One of the possible reasons of observed regularities is that X-ray conductivity in investigated crystals, especially at comparatively low V a is due predominantly to radiation of thin layer of crystal. In this case with the rise of radiation intensity there have been started to prevail the mechanism of surface quadratic recombination which leads to observed decrease of X-ray conductivity. With the rise of accelerating potential 'effective hardness' is increased, as a result of which there

  13. Electronic structure of nanoscale Cu/Pt alloys: A combined X-ray diffraction and X-ray absorption investigations

    International Nuclear Information System (INIS)

    Chen Xing; Chu Wangsheng; Cai Quan; Xia Dingguo; Wu Zhonghua; Wu Ziyu

    2006-01-01

    PVP-protected Cu/Pt clusters were prepared by glycol/water reduction method and characterized with transmission electron microscopy (TEM), X-ray diffraction (XRD) and absorption spectra. TEM and XRD analysis show that the Cu/Pt clusters with different molar ratio have fcc structure with particle size of about 4 nm, while the lattice parameters in these clusters reduce with increasing Cu concentration. From the X-ray absorption near edge structure (XANES) at Cu-K edge and Pt-L 2,3 edge, we demonstrate that the d-electronic states of Cu and Pt are affected by the local environment as a function of Cu/Pt molar ratio. With increasing Cu concentration, Pt loses a fraction of 5d electrons and the hybridization between p- and d-states at Cu sites is enhanced

  14. Electronic structure of nanoscale Cu/Pt alloys: A combined X-ray diffraction and X-ray absorption investigations

    Energy Technology Data Exchange (ETDEWEB)

    Chen Xing [Beijing Synchrotron Radiation Facility, Institute of High Energy Physics, CAS, Beijing (China); Graduate School of the Chinese Academy of Sciences, 100864 Beijing (China); Chu Wangsheng [Beijing Synchrotron Radiation Facility, Institute of High Energy Physics, CAS, Beijing (China); University of Science and Technology of China, Hefei, 230036 (China); Cai Quan [Beijing Synchrotron Radiation Facility, Institute of High Energy Physics, CAS, Beijing (China); Graduate School of the Chinese Academy of Sciences, 100864 Beijing (China); Xia Dingguo [College of Environmental and Energy Engineering, Beijing University of Technology, 100022 Beijing (China); Wu Zhonghua [Beijing Synchrotron Radiation Facility, Institute of High Energy Physics, CAS, Beijing (China); Wu Ziyu [Beijing Synchrotron Radiation Facility, Institute of High Energy Physics, CAS, Beijing (China) and National Center for Nanoscience and Technology (China)]. E-mail: wuzy@ihep.ac.cn

    2006-11-15

    PVP-protected Cu/Pt clusters were prepared by glycol/water reduction method and characterized with transmission electron microscopy (TEM), X-ray diffraction (XRD) and absorption spectra. TEM and XRD analysis show that the Cu/Pt clusters with different molar ratio have fcc structure with particle size of about 4 nm, while the lattice parameters in these clusters reduce with increasing Cu concentration. From the X-ray absorption near edge structure (XANES) at Cu-K edge and Pt-L{sub 2,3} edge, we demonstrate that the d-electronic states of Cu and Pt are affected by the local environment as a function of Cu/Pt molar ratio. With increasing Cu concentration, Pt loses a fraction of 5d electrons and the hybridization between p- and d-states at Cu sites is enhanced.

  15. A mirror for lab-based quasi-monochromatic parallel x-rays.

    Science.gov (United States)

    Nguyen, Thanhhai; Lu, Xun; Lee, Chang Jun; Jung, Jin-Ho; Jin, Gye-Hwan; Kim, Sung Youb; Jeon, Insu

    2014-09-01

    A multilayered parabolic mirror with six W/Al bilayers was designed and fabricated to generate monochromatic parallel x-rays using a lab-based x-ray source. Using this mirror, curved bright bands were obtained in x-ray images as reflected x-rays. The parallelism of the reflected x-rays was investigated using the shape of the bands. The intensity and monochromatic characteristics of the reflected x-rays were evaluated through measurements of the x-ray spectra in the band. High intensity, nearly monochromatic, and parallel x-rays, which can be used for high resolution x-ray microscopes and local radiation therapy systems, were obtained.

  16. Adsorbate induced surface alloy formation investigated by near ambient pressure X-ray photoelectron spectroscopy

    DEFF Research Database (Denmark)

    Nierhoff, Anders Ulrik Fregerslev; Conradsen, Christian Nagstrup; McCarthy, David Norman

    2014-01-01

    for engineering of more active or selective catalyst materials. Dynamical surface changes on alloy surfaces due to the adsorption of reactants in high gas pressures are challenging to investigate using standard characterization tools. Here we apply synchrotron illuminated near ambient pressure X-ray photoelectron...

  17. Note: Loading method of molecular fluorine using x-ray induced chemistry

    International Nuclear Information System (INIS)

    Pravica, Michael; Sneed, Daniel; White, Melanie; Wang, Yonggang

    2014-01-01

    We have successfully loaded molecular fluorine into a diamond anvil cell at high pressure using the synchrotron x-ray induced decomposition of perfluorohexane (C 6 F 14 ). “White” x-ray radiation from the Advanced Photon Source was used to initiate the chemical decomposition of C 6 F 14 , which resulted in the in situ production of F 2 as verified via Raman spectroscopy. Due to the toxic nature of fluorine, this method will offer significant advantages in the ability to easily load a relatively nontoxic and inert substance into a chamber (such as a diamond anvil cell) that, when sealed with other reactants and irradiate with hard x-rays (>7 keV), releases highly reactive and toxic fluorine into the sample/reaction chamber to enable novel chemical synthesis under isolated and/or extreme conditions

  18. Characteristics of specifications of transportable inverter-type X-ray equipment

    CERN Document Server

    Yamamoto, K; Asano, H

    2003-01-01

    Our X-ray systems study group measured and examined the characteristics of four transportable inverter-type X-ray equipments. X-ray tube voltage and X-ray tube current were measured with the X-ray tube voltage and the X-ray tube current measurement terminals provided with the equipment. X-ray tube voltage, irradiation time, and dose were measured with a non-invasive X-ray tube voltage-measuring device, and X-ray output was measured by fluorescence meter. The items investigated were the reproducibility and linearity of X-ray output, error of pre-set X-ray tube voltage and X-ray tube current, and X-ray tube voltage ripple percentage. The waveforms of X-ray tube voltage, the X-ray tube current, and fluorescence intensity draw were analyzed using the oscilloscope gram and a personal computer. All of the equipment had a preset error of X-ray tube voltage and X-ray tube current that met Japanese Industrial Standards (JIS) standards. The X-ray tube voltage ripple percentage of each equipment conformed to the tendenc...

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

    Science.gov (United States)

    Godinho, jose; Gerke, kirill

    2016-04-01

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

  20. Image analysis in x-ray cinefluorography

    Energy Technology Data Exchange (ETDEWEB)

    Ikuse, J; Yasuhara, H; Sugimoto, H [Toshiba Corp., Kawasaki, Kanagawa (Japan)

    1979-02-01

    For the cinefluorographic image in the cardiovascular diagnostic system, the image quality is evaluated by means of MTF (Modulation Transfer Function), and object contrast by introducing the concept of x-ray spectrum analysis. On the basis of these results, further investigation is made of optimum X-ray exposure factors set for cinefluorography and the cardiovascular diagnostic system.

  1. Panoramic Dental X-Ray

    Science.gov (United States)

    ... Physician Resources Professions Site Index A-Z Panoramic Dental X-ray Panoramic dental x-ray uses a very small dose of ... x-ray , is a two-dimensional (2-D) dental x-ray examination that captures the entire mouth ...

  2. Proceedings of the workshop on X-ray computed microtomography

    Energy Technology Data Exchange (ETDEWEB)

    NONE

    1998-02-01

    This report consists of vugraphs from the nine presentations at the conference. Titles of the presentations are: CMT: Applications and Techniques; Computer Microtomography Using X-rays from Third Generation Synchrotron X-ray; Approaches to Soft-X-ray Nanotomography; Diffraction Enhanced Tomography; X-ray Computed Microtomography Applications at the NSLS; XCMT Applications in Forestry and Forest Products; 3DMA: Investigating Three Dimensional Pore Geometry from High Resolution Images; X-ray Computed Microtomography Studies of Volcanic Rock; and 3-D Visualization of Tomographic Volumes.

  3. Proceedings of the workshop on X-ray computed microtomography

    International Nuclear Information System (INIS)

    1998-02-01

    This report consists of vugraphs from the nine presentations at the conference. Titles of the presentations are: CMT: Applications and Techniques; Computer Microtomography Using X-rays from Third Generation Synchrotron X-ray; Approaches to Soft-X-ray Nanotomography; Diffraction Enhanced Tomography; X-ray Computed Microtomography Applications at the NSLS; XCMT Applications in Forestry and Forest Products; 3DMA: Investigating Three Dimensional Pore Geometry from High Resolution Images; X-ray Computed Microtomography Studies of Volcanic Rock; and 3-D Visualization of Tomographic Volumes

  4. Chest X-Ray

    Medline Plus

    Full Text Available ... I’d like to talk with you about chest radiography also known as chest x-rays. Chest x-rays are the most ... far outweighs any risk. For more information about chest x-rays, visit Radiology Info dot org. Thank you for your time! ...

  5. X-ray transport and radiation response assessment (XTRRA) experiments at the National Ignition Facility

    Energy Technology Data Exchange (ETDEWEB)

    Fournier, K. B., E-mail: fournier2@llnl.gov; Brown, C. G.; Yeoman, M. F.; Compton, S.; Holdener, F. R.; Kemp, G. E.; Blue, B. E. [Lawrence Livermore National Laboratory, 7000 East Avenue, Livermore, California 94551 (United States); Fisher, J. H.; Newlander, C. D.; Gilliam, R. P.; Froula, N. [Fifth Gait Technologies, Inc., 14040 Camden Circle, Huntsville, Alabama 35803 (United States); Seiler, S. W.; Davis, J. F.; Lerch, MAJ. A. [Defense Threat Reduction Agency, 8725 John J. Kingman Road, Fort Belvoir, Virginia 22060-6201 (United States); Hinshelwood, D. [Naval Research Laboratory, 4555 Overlook Ave. SW, Washington, DC 20375 (United States); Lilly, M. [Dynasen, Inc., 20 Arnold Pl., Goleta, California 93117 (United States)

    2016-11-15

    Our team has developed an experimental platform to evaluate the x-ray-generated stress and impulse in materials. Experimental activities include x-ray source development, design of the sample mounting hardware and sensors interfaced to the National Ignition Facility’s diagnostics insertion system, and system integration into the facility. This paper focuses on the X-ray Transport and Radiation Response Assessment (XTRRA) test cassettes built for these experiments. The test cassette is designed to position six samples at three predetermined distances from the source, each known to within ±1% accuracy. Built-in calorimeters give in situ measurements of the x-ray environment along the sample lines of sight. The measured accuracy of sample responses as well as planned modifications to the XTRRA cassette is discussed.

  6. Use of portable X-ray fluorescence instrument for bulk alloy analysis on low corroded indoor bronzes

    International Nuclear Information System (INIS)

    Šatović, D.; Desnica, V.; Fazinić, S.

    2013-01-01

    One of the most often used non-destructive methods for elemental analysis when performing field measurements on bronze sculptures is X-ray fluorescence (XRF) analysis based on portable instrumentation. However, when performing routine in-situ XRF analysis on corroded objects obtained results are sometimes considerably influenced by the corrosion surface products. In this work the suitability of portable XRF for bulk analysis of low corroded bronzes, which were initially precisely characterized using sophisticated and reliable laboratory methods, was investigated and some improvements in measuring technique and data processing were given. Artificially corroded bronze samples were analyzed by a portable XRF instrument using the same methodology and procedures as when performing in-situ analysis on real objects. The samples were first investigated using sophisticated complementary laboratory techniques: Scanning Electron Microscopy, Proton-Induced X-ray Emission Spectroscopy and Rutherford Backscattering Spectrometry, in order to gain precise information on the formation of the corrosion product layers and in-depth elemental profile of corrosion layers for different aging parameters. It has been shown that for corrosion layers of up to ca. 25 μm a portable XRF can yield very accurate quantification results. - Highlights: • XRF quantification is very accurate for bronze corrosion layers of up to ca. 25 μm. • Corrosion layer formation on bronze described in two phases. • Corrosion layers precisely characterized using PIXE, RBS and SEM. • Corrosion approximated as CuO for layer thickness calculations via X-ray attenuations • Increasingly lighter corrosion matrix may cause SnLα radiation intensity inversion

  7. Use of portable X-ray fluorescence instrument for bulk alloy analysis on low corroded indoor bronzes

    Energy Technology Data Exchange (ETDEWEB)

    Šatović, D., E-mail: dsatovic@alu.hr [Department of Conservation and Restoration, Academy of Fine Arts, Ilica 85, 10000 Zagreb (Croatia); Desnica, V. [Department of Conservation and Restoration, Academy of Fine Arts, Ilica 85, 10000 Zagreb (Croatia); Fazinić, S. [Laboratory for Ion Beam Interactions, Ruđer Bošković Institute, Bijenička 54, 10000 Zagreb (Croatia)

    2013-11-01

    One of the most often used non-destructive methods for elemental analysis when performing field measurements on bronze sculptures is X-ray fluorescence (XRF) analysis based on portable instrumentation. However, when performing routine in-situ XRF analysis on corroded objects obtained results are sometimes considerably influenced by the corrosion surface products. In this work the suitability of portable XRF for bulk analysis of low corroded bronzes, which were initially precisely characterized using sophisticated and reliable laboratory methods, was investigated and some improvements in measuring technique and data processing were given. Artificially corroded bronze samples were analyzed by a portable XRF instrument using the same methodology and procedures as when performing in-situ analysis on real objects. The samples were first investigated using sophisticated complementary laboratory techniques: Scanning Electron Microscopy, Proton-Induced X-ray Emission Spectroscopy and Rutherford Backscattering Spectrometry, in order to gain precise information on the formation of the corrosion product layers and in-depth elemental profile of corrosion layers for different aging parameters. It has been shown that for corrosion layers of up to ca. 25 μm a portable XRF can yield very accurate quantification results. - Highlights: • XRF quantification is very accurate for bronze corrosion layers of up to ca. 25 μm. • Corrosion layer formation on bronze described in two phases. • Corrosion layers precisely characterized using PIXE, RBS and SEM. • Corrosion approximated as CuO for layer thickness calculations via X-ray attenuations • Increasingly lighter corrosion matrix may cause SnLα radiation intensity inversion.

  8. Miniature x-ray point source for alignment and calibration of x-ray optics

    International Nuclear Information System (INIS)

    Price, R.H.; Boyle, M.J.; Glaros, S.S.

    1977-01-01

    A miniature x-ray point source of high brightness similar to that of Rovinsky, et al. is described. One version of the x-ray source is used to align the x-ray optics on the Argus and Shiva laser systems. A second version is used to determine the spatial and spectral transmission functions of the x-ray optics. The spatial and spectral characteristics of the x-ray emission from the x-ray point source are described. The physical constraints including size, intensity and thermal limitations, and useful lifetime are discussed. The alignment and calibration techniques for various x-ray optics and detector combinations are described

  9. X-rays and photocarcinogenesis in hairless mice.

    Science.gov (United States)

    Lerche, Catharina M; Philipsen, Peter A; Wulf, Hans Christian

    2013-08-01

    It is well known that excessive X-ray radiation can cause non-melanoma skin cancers. With the increased incidence of sun-related skin cancer there is a need to investigate the combination of sunlight and X-rays. Immunocompetent C3.Cg/TifBomTac mice (n = 298) were divided into 12 groups. Mice were irradiated with 12, 29 or 50 kV X-rays. The mice received a total dose of 45 Gy. They were irradiated with 3 SED simulated solar radiation (SSR) either before or after irradiation with X-rays. The groups irradiated with X-rays alone, 0, 3, 9 and 10 mice (0, 12, 29 and 50 kV, respectively) developed squamous cell carcinoma. In the groups irradiated with SSR after X-rays the development of tumours was significantly faster in the 50 kV group than in the corresponding control group (175 vs. 194 days, p X-ray radiation the development of tumours was significantly faster in the 29 and the 50 kV groups than in the corresponding control group (175 vs. 202 days, p X-ray radiation alone is a weak carcinogen in hairless mice. There is an added carcinogenic effect if X-ray radiation is given on prior sun-exposed skin or if the skin is sun-exposed after X-rays. We still believe that X-ray radiation is a safe and effective therapy for various dermatological diseases but caution should be observed if a patient has severely sun-damaged skin or has a high-risk sun behaviour.

  10. Portable and micro x-ray fluorescence investigations of the wall paintings belonging to different periods of anatolian history

    International Nuclear Information System (INIS)

    Zararsiz, A.; Ozen, L.; Kalayci, Y.

    2014-01-01

    Full text: In this study portable x-ray fluorescence spectrometer and micro x-ray fluorescence spectrometer were used for investigating the pigments on the Chatalhoyuk wall paintings from the neolithic period which are located in Museum of Anatolian Civilizations. Totally 15 artifacts were investigated in this study and the elemental compositions of the pigments were identified on this paintings. The communities which have lived in different periods of time have revealed different cultures during the 12 000 years old cultural heritage in our country

  11. Subluminous X-ray binaries

    NARCIS (Netherlands)

    Armas Padilla, M.

    2013-01-01

    The discovery of the first X-ray binary, Scorpius X-1, by Giacconi et al. (1962), marked the birth of X-ray astronomy. Following that discovery, many additional X-ray sources where found with the first generation of X-ray rockets and observatories (e.g., UHURU and Einstein). The short-timescale

  12. X-Ray Exam: Forearm

    Science.gov (United States)

    ... Staying Safe Videos for Educators Search English Español X-Ray Exam: Forearm KidsHealth / For Parents / X-Ray Exam: ... Muscles, and Joints Broken Bones Getting an X-ray (Video) X-Ray (Video) View more Partner Message About Us ...

  13. X-Ray Exam: Foot

    Science.gov (United States)

    ... Staying Safe Videos for Educators Search English Español X-Ray Exam: Foot KidsHealth / For Parents / X-Ray Exam: ... Muscles, and Joints Broken Bones Getting an X-ray (Video) X-Ray (Video) View more Partner Message About Us ...

  14. X-Ray Exam: Wrist

    Science.gov (United States)

    ... Staying Safe Videos for Educators Search English Español X-Ray Exam: Wrist KidsHealth / For Parents / X-Ray Exam: ... Muscles, and Joints Broken Bones Getting an X-ray (Video) X-Ray (Video) View more Partner Message About Us ...

  15. Thoracic spine x-ray

    Science.gov (United States)

    Vertebral radiography; X-ray - spine; Thoracic x-ray; Spine x-ray; Thoracic spine films; Back films ... 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 ...

  16. X-Ray Exam: Finger

    Science.gov (United States)

    ... Staying Safe Videos for Educators Search English Español X-Ray Exam: Finger KidsHealth / For Parents / X-Ray Exam: ... Muscles, and Joints Broken Bones Getting an X-ray (Video) X-Ray (Video) View more Partner Message About Us ...

  17. 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.

  18. 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.

  19. X-ray and scanning electron microscopic investigation of porous silicon and silicon epitaxial layers grown on porous silicon

    International Nuclear Information System (INIS)

    Wierzchowski, W.; Pawlowska, M.; Nossarzewska-Orlowska, E.; Brzozowski, A.; Wieteska, K.; Graeff, W.

    1998-01-01

    The 1 to 5 μm thick layers of porous silicon and epitaxial layers grown on porous silicon were studied by means of X-ray diffraction methods, realised with a wide use of synchrotron source and scanning microscopy. The results of x-ray investigation pointed the difference of lateral periodicity between the porous layer and the substrate. It was also found that the deposition of epitaxial layer considerably reduced the coherence of porous fragments. A number of interface phenomena was also observed in section and plane wave topographs. The scanning electron microscopic investigation of cleavage faces enabled direct evaluation of porous layer thickness and revealed some details of their morphology. The scanning observation of etched surfaces of epitaxial layers deposited on porous silicon revealed dislocations and other defects not reasonable in the X-ray topographs. (author)

  20. 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